CA1119793A

CA1119793A - Suspension of entrapped hydrolytic flavor oil in non-confined hydrophobic flavor oil

Info

Publication number: CA1119793A
Application number: CA000340608A
Authority: CA
Inventors: Don Marmo; Frank L. Rocco
Original assignee: International Flavors and Fragrances Inc
Current assignee: International Flavors and Fragrances Inc
Priority date: 1979-03-05
Filing date: 1979-11-26
Publication date: 1982-03-16

Abstract

ABSTRACT OF THE DISCLOSURE

Described are (A) smoking tobacco composition or substitute smoking tobacco compositions which, on fabrication into a smoking article, on smoking, yield a high flavor intensity release substantially evenly and uniformly over an extended period of time; the smoking tobacco composition or substitutes therefor containing a mixture of (i) a non confined flavor oil;
(ii) a flavor oil which is physically entrapped in solid particles; and (iii) a suspending agent such as hydroxpropyl cellulose; the non-confined flavor oil, the entrapped flavor oil and the suspension agent being premixed prior to addition to said smoking tobacco or said smoking tobacco substitute;
and (B) hot beverage mix compositions which, on admixing with a heated edible liquid, yield a high flavor intensity release substantially evenly and uniformly over an extended use period, the hot beverage mix containing a mixture of (i) a non-confined flavor oil; (ii) a flavor oil which is physically entrapped in solid particles; and (iii) a suspending agent such as hydroxy-propyl cellulose; the non-confined flavor oil, the entrapped flavor oil and the suspension agent being premixed prior to addition to said beverage mix or (C) other orally utilizable compositions which may be either chewing gum compositions, chewable medicinal tablets, chewing tobacco or toothpaste having an oral intake, a high flavor intensity release substan-tially evenly and uniformly, over an extended oral utilization time in the mouth cavity; the orally utilizable compositions containing a non-confined flavor oil, a flavor oil which is physically entrapped in solid particles and a suspending agent which is hydroxypropyl cellulose; the non-confined flavor oil, the entrapped flavor oil and the suspension agent being pre-mixed prior to addition to either of the chewing gum base, the chewing tobacco or the chewable medicinal tablet base, or to the toothpaste base.

Description

IFF-~615.5 ~7~3 cAna ,, . -1- .
,, Pield of the Invention:

This invention relates to specific flavor compositions useful in augmenting or enhancing the aroma or taste of "hot" beverage powder mixes or smoking tobaccos or substitute smoking tobaccos. The smoking tobacco compositions as well as the "hot" beverage powder mixes when consumed in their proper respective environments have flavors with good initial strengths which 1avors are controllably released (under the conditions of ad~ixing with a hot consumable liquid, e.g., ethanol or water or combinations thereof or under conditions of smoking tobacco pyrolysis during the smoking activity) -at a consistently high level over an extended period of time; and to processes for preparing such specially useful smoking tobacco and substitute smoking tobacco flavoring compositions as well as such specially useful hot beverage compositions and hot beverage flavoring compositions~ -..:
~his inVention also relates to other improved orallyutilizable compositions having a flavor with good initial strength and which flavor is controllably released (under the hydrolytic conditions of the human mouth cavity) at a consistently high level over an extended period of time; to processes for preparing such orally utilizable compositions; to flavor compositions useful in preparing same and to processes for preparing such specially useful flavoring compositions.
~., The term "orally utilizable compositions" includes such materials as chewing gum, chewable medicinal tablets such as chewable vitamin tablets, chewing tobacco and toothpaste.
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Descr1ption of the Prior Art:

There has been considerable work performed relating to smoking tobacco or substitute tobacco substances which have a flavor impact both initially and over an ; extended period of time during the smoking activity.
Problems have arisen in attempting to create such flavor compositions for use with smoking tobacco wherein part of the flavor is available for i~mediate results whereas another part provides the effect of such smoking tobacco fla~or or substitute smoking flavor gradually over extended periods of time. Such problems ` include the continuous distribution of "initial impactl' and "extended release" flavor over the entire mass of the smoking tobacco or substitute smoking tobacco as - well as commercial manufacture of same. - -Indeed, in using menthol in flavoring tobacco, the menthol is applied on tobacco by spraying an alcoholic solution of men-thol crystals thereon. The usual amount of menthol used is 0O3% by weight of the total spray compositionO When menthol is used in this manner, however/ the smoking articles insofar as their flavor value is concerned have unsatisfactory shelf lives.
.~ . ' - Furthermore, there has been considerable work performed relating to hot beverage substances which have a flavor impact both initially and over an extended period of time after addi-tion of the hot edible liquid (e.g., water, ethanol or a com-bination of water and ethanol) to the beverage flavor powder, for example problems have arisen in attempting to create such flavor compositions for use with beverage powders wherein part of the flavor is available for immediate results whereas another part provides the effect of such flavor gradually over extended periods of time. Such problems include the continuous distri-bution of "initial impact" and "extended release" flavor over c the entire length of time of drinking the hot beverage as well as commercial manufacture of same.
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97~3 There has also been considerable work performed relating to orally utilizable substances such as chewing gum, ¢hewable medicinal tablets, chewing tobacco and tooth-paste whereby su~h orally utilizable substances have a flavor impact both initially and over an extended period of time. Problems have arisen in attempting to create such orally utilizable compositions wherein par~ of the flavor is available for immediate results whereas another part provides the effect of such flavor gradually over extended periods of time. Such ~roblems include the continuous distribution of "initial impact" and "extended release" flavor over the entire mass of the orally utilizable composition as well as commercial manufacture of sameO
., ., United States Patents 4,001,438 and 3,920,849 have presented solutions to such problems where various consumable materials are concerned. Thus, described in - U.S. Patent 3,920,849 are orally utili~able compositions which may be either chewing gum compositions, chewable medicinal tablets, chewing tobacco or toothpaste having, on oral intake~ a high flavor intensity release, sub-stantially evenly and uniformly, over an extended oral utilization time in the mouth cavity; the orally utilizable compositions containing a non-confined flavor oil/ a flavox oil which is physically entrapped in solid particles and a suspending agent such as silica, xanthan gum and ethyl cellulose; the non-confined flavor oil, the entrapped flavor oil and the suspension agent being premixed prior to addition to either o~ the chewing gum base, the chewing tobacco or the chewable medicinal tablet base or to the toothpaste base. Neither U.S.
Patent 3,920,849 nor U.S. Patent 4,001,438 discloses the use of such materials for flavoring consumable materials which are consumed at temperatures significantly greater t than ambient temperatures, e.g., smoking tobacco and hot ~ea, hot coffee or alcoholic beverages which include hot aqueous tea extracts or hot aqueous coffee extracts.
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U.5. Patent No. 1,526,039 teaches that if an essential ~il or flavoring is comblned with a chewing gum base in a finely divided condition, and the particles of the flavoring or oil are encased in a suitable covering so as not to contact the gum directly during manufacture, the deleterious efect of the flavoring on the gum is prevented or largely reduced. It is further stated therein that:

"When the emulsion is added to the gum base, it is thoroughly mixed therewith by the usual means employed for mixing the flavoring material with such base.
'.
~ he production of the emulsion serves to break up the essential oil into fine particles and to encase these particles in the emulsifying material, so that when the emulsion is added to the gum mass, the essential oil to a large degree is prevented from coming into direct contact with the base, and from having deleterious action thereon. Il U.S~ Patent No. 2,886,440 teaches a method of preparing a chewing gum characterized by "extended flavor perception time, true flavor character, and high degree of flavor release com-prising the steps of forming a spray-dried emulsion of a vola-tile, water-immiscible flavoring agent encapsulated within finely divided particles of gelatin, and substantially uniformly distributing said gelatin encapsulated flavoring agent within an all-enveloping mass of a chewable gum base. n .

The use of separatc ~fixed~ and "unfixed~ flavor portions is also taught but there is ~ot disclo~ure therein of the prin-~ciple of this invention to wito mixing the fixed and unfixed ; flavor portions with a suspension agent prior to either (i) adding to a smoking tobacco or substitute smoking tobacco prior to incorporation thereof into a smoking tobacco or substitute smokikng tobacco article prior to smoking or (ii) adding to a dry beverage mix formulation prior to addition of hot edible liquid thereto immediately prior to ingestion~

U.S~ Patent No. 2,886,446 teaches a chewing gum comprising (i) smaller particles of gelatin characterized by faster lib-eration of flavor and (ii) larger particles of gelatin chara-cterized by slower liberation of flavor, each of the gelatin particles containing dispersed therewithin, in dried emulsion form, discrete micro-droplets of a volatile water-immiscible flavoring agent, and an all-enveloping mass of a chewable gum base within which the particles are substantially uniformly distri~uted whereby the flavor is released substantially evenly and uniformly over the extended chewing time.
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U.S. Patent ~o. 2~886,445 teaches that:
"It is now possible to obtain a flavoring composition, particularly adapted for use in chewing gum which permits attainment of a product characteri~ed by extended flavor per-ception time, true flavor character, and release o a large proportion of flavoring agent. This flavoring composition comprises finely divided particles of a dried hardened gelatin emulsion containing discrete micro-droplets of a volatile, water-immiscible flavoring agent. Preparation of the ; flavoring composition of this invention may be effected by encapsulating discrete micro-droplets of volatile, water immiscible flavoring agent within finely divided particles of a dried emulsion of hardened gelatin.~

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U.S. Patent No. 2,886,449 teaches:
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.~ "A chewing gum containing a flavoring composition - ~ characteri7ed by an extended flavor perception ~ s l! time, true flavor character, controlled release - ,i of a large portion of flavoring agent, and reduction in amount of flavor oil required ~which) may be prepared by the process comprising forming a gelatin-coacerYated flavor, and substantially uniformly distributing said gelatin-coacervated flavor within an all-enveloping mass of a - chewable gum base. The~ product chewing gum... com-prises..~finely divided particles of coacervated gelatin containing a water-immiscible flavoring ` 15 agent therewithin and an all-enveloping mass of a chewing gum base within which the particles are substantially distributed."
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; The utili2ation of sustained released flavor containing capsules in such materials as chewing gum and medicinal tablets is also taught in British Patent No. 1,205,764.
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The use of sustained release flavor capsules in conjunct~
ion with polyethylene glycols (which are taught to be employed to desolventize the capsules) is set forth in British Patent -~ No. 1,318,799.

The use of hydroxypropyl cellulose contained in microcap-sules especially for pressure sensitive copying paper is dis-closed in Japanese Patent J 7 9000 426 claiming a priority of United States Application 480,956 filed on June 19, 1974 and assigned to the Mead CorporationO In said Japanese Patent J7 9000 426 it is indicated that oil~containin~ microcapsules L
especially for pressure sensitive copying paper are prepared by ~a) preparing an aqueous solution of hydroxypropyl cellulose containing reactive hydroxyl groups and having a decreasing water solubility as the temperature increases; ~b) then preparing ' I' ' Z

Il i , _7~ 1 .
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a solution of an oil soluble cross-linking agent for the hydroxy-propyl cellulose in an oil; ~hen emulsifying the oil solution ~n the aqueous solution to form an emulsion containing droplets '' of the oil solutiQn; (c) then heating the emulsion to a temp-erature above the precipitation temperature of the hydroxypropyl i, cellulose :50 that hydroxypropyl cellulose precipitates over the drople~s to form solid microcapsule walls and (d) finally maintaining the emulsion at this temperature until the micro- j ' ~apsule walls-become insaluble in water and in the oil. Nothing in the Japanese Patent J7 9000 426 discloses the creation of a smoking tobacco composition or a powdered hot beverage com-position w~-e-rein the flavor thereof is controllably released ; during the-smoking activity or beverage ingestion activity (as the case may be) at a consistently high level over an extended period of time.- --- , In United States Patent 3,623,489 the formation of a shred-ded tobacco material having intimately admixed therewith a micro encapsulated,synthetic clove flavoring material (wherein ~he ~- 20 capsules are of such a size as to create an audible crackling sound when burned) and the incorporation thereof into smoking ` articles such as cigarettes and cigars is disclosed. It is further disclosed- that these capsules may also contain a tobacco ~lavor enhancer. ~ - -U.S. Patent 3,753,730 issued on August 21, 1973 discloses processes for altering the flavors of particulate grain products comprising applying a composition comprising a flavoring agent, an edible cold water insoluble film former and a vehicle to a particulate grain product; drying the distributed composition to form a flavor containing film on the grain product; and then optionally, distributing the coated flavored grain through a large mass of uncoated grain particles.
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I
. 1 -8-. , , German Offenlengungsschrift 2,826,042 published on January 4, 1979 discloses a condiment consistin~ of a lemon flavored sal~ prepared by mixing salt and a lemon oil powder and spray-ing the resulting mixture with lemon oilO More particularly, the salt is admixed with (a) from 0.1 up to 0~5 weight percent of salt of a terpene-free lemon oil bonded to a powdery carrier and (b) terpene-free liquid lemon oil. The condiment is pre-pared by mixing the dry salt with component a, spraying the mixtu~e with component b and mixing through a screw conveyorO
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.. ~0 Hydroxypropyl cellulose itself is described in particular . in three publications:
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. a. Hercules/Klucel ~/hydroxypropyl cellulose . published by Hercules Incorporated of ~ Wilmir.gton, Delaware;
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b. Klug, Vol. 24, No. 51, Food Technology, January, 1970, page 51 entitled: "Functional Helpmate to Development...Hydroxypropyl : Cellulose/a New Water Soluble Cellulose Polymer"; and . c. United States Patent 3,278,521, issued on October 11, 1966 entitled: "Hydroxypropyl .
Cellulose and Process"/Inventor: Klug~ :

However, the prior art does not set forth commercially feasible . :
. . .processes for creating a smoking tobacco composition of substi-.; tute smoking tobacco composition containing a flavoring compo-sition which provides instantaneous evenly distributed flavor release, extended continuous, non-interrupted flavor perception time periods and at the same time provides during the smoking : activity, extended constant flavor impact; wh~ch is provided by o~r invention; nor does the prior art teach the creation of a hot beverage mix composition which on admixing with a heated edible liquid yields a high flavor intensity re.l`ease substan- ~
tially evenly and uniformly over an extended use period. .
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g Furthermore nothing ln the prior art indicates the use of hydroxypropyl cellulose as defined in U.S. Patent

3,278,521 issued on October 11, 1966 for taking the place of the suspension agents of 3,920,849.
Brief Description of the Drawings:
Figure l sets forth a block diagram flow sheet indicating the preparation of the flavored beverage powder as well as the flavored smoking tobacco of our invention as more fully described in Examples A-Y and I-LXXXIV.
Figure 2 sets forth a block diagram flow sheet indicating the preparation of the flavored chewing gum of our invention as more fully described in the Examples 9 infra.
Figure 3 sets forth a graph indicating the Klucel brand of hydroxylpropyl cellulose solids concentration (weight percent) versus Brookfield viscosit~ at 25C in centipoises for types E, L, J, G, M and H Xlucel R hydroxypropyl cellulose materials. Thus, Figure 2 indicates the effect of concentration in Klucel R type on viscosity of water solutions.
Figure 4 sets forth a block diagram flow sheet indicating the preparation of the flavored orally consumable materials of our invention as~more fully described in the Examples, infra.

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, , -10 Objects of the Invention:

It is an object o~ this invention to provide an orally utilizable composition containing a 1avoring composition characterized by (i) an almost instantaneous flavor perception and (ii) over an extended period of time controlled constant and continuous, non-interrupted high impact flavor release.

It is a further object of this invention to provide a smoking tobacco composition or substitute smoking tobacco composition containing a flavoring composition charact-erized by (i) an almost instantaneous flavor perception prior to smoking and on smoking and (ii1 over an extended period of time on smoking, controlled constant and continuous non-interrupted high impact flavor release.
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An additional object of this invention is to increase the total amount of flavor release during the smoking activity of the smoking article containing the herein described flavoring composition.

An additional object of this invention is to provide a hot beverage mix composition which on admixin~ with a heated edible liquid yields a high fla~or intensity r~lease substantially evenly and uniformly over an ; extended use period. -.~ .
An additional object of this invention is to increase the total amount of flavor released during the chewing period of chewing gums, chewing tobacco and chewable medicinal tablets or during the toothbrushing period of toothpastes containing the herein described flavoring composition.
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'~ 30 Further objects of this invention will be apparent to those skilled in the art from the following detailed description of the invention.
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Description of the Preferred Embodimentso This invention relates to improved orally utilizable compositions such as chewing gum, chewable medicinal tablets, chewing tobacco and toothpaste having a flavor with good evenly distributed initial strength and.which flavor is controllably released with continuous non~
. interrupted high flavor impact over an extended period . of time; to processes for preparing the same and to processes for preparing such flavoring compositions.
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This invention also relates to flavor compositions for use in smoking tobacco or substitute smoking tobacco . compositions which are, in turn, used in smoking tobacco . articles or substitute smoking tobacco articles such as cigarettes and cigars. The said smoking tobacco or substituted smoking tobacco has a flavor with good evenly . distributed initial strength and this flavor is controll-.. ably released with continuous non-interrupted high flavor . impact over an extended period of time during the smoking activity; and to processes for preparing such flavoring compositions.

:~ This invention in addition relates to hot beverage mix~: compositions which on admixing with a heated edible ; liquid such as water or ethanol (food grade) yield a . . high flavor intensity release substantially evenly and ~ uninformly over an extended use period, the hot beverage : mix containing a mixture of (i) a non-confi.ned flavor . oil; (ii) a flavor oil which is physically entrapped in : solid edible particles and (iii~ a suspendiny agent such as hydroxypropyl cellulose, ethyl cellulose, silica or .
xanthan gum, the non-confined oil, the flavor oil which .
is physically entrapped in solid particles and suspending agent being premixed prior to addition to said beverage mix composition. .

3t7~3 Chewing gum and chewable medicinal tablets may comprise a substantially water insoluble, chewable, plastic gum base such as chicle, or substitutes therefor, including jelutong, gutt,,akay, rubber,or certain comestible natural or synthetic,,resins or waxes. Incorporated with the gum base, and in intimate admixture therewith,,may be plasticizers or softening,agents, e.g.,, glycerine;
f,lavoring age,nts, e-.g,, o,il:o$ win,tergre,en,,oil of, spear,mint, oil of pepp,ermint, li,corice, fruit flavors, 10 ' spice,oils, ,etc,., or swee,tening agents which-may be ~; sugars including sucrose or dextrose and/or they may be artificial-sweeteners such as cyclamates or saccharinO
. 9ther,optional ingredients m,ay also be presen~.

Chewing tobacco,may comprise specifi,cally grown tobacco for chewing which would include 85 ~ercen-t P,ennsylvania Leaf T,obacco having a ,','casing" spray dried at a rate of about-25 percent up t,o about 40 p,ercen,t which,casing would contain such ingredients as corn syrup, licorice, glycerin, f,ig,juice~ prune juice,and a,s is the case ,i,n this invention, a~flavor ma,terial. The resultant,-,,product ,is,redried to , a moisture content of between 10 and 30 percent.
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~ ~Toothpaste-s~may comprise~four-~roups of'ada'itïves:
.~ . : -Group A: Glycerine,'distilled water; sodium .
benzoate-; if'desired, a~tificial sweetener such as sodium saccharin and,- i desired,'stannous fluoride.

Group B: A basic pH'buffer such as calcium , carbonate and/or dicalcium phosphate.
~' ' . , , . .' - Group C: A foaming agent such as sodium n-lauroyl -sarcosinate. : -; . . , ~
- Group D: A flavor material.

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A standard technique for formulating the above groups into the toothpaste is exemplified as follows:
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: lo The ingredients in Group A are stirred and ~ heated in a steam jacketed kettle to lÇ0~.
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2~ Stirring is continued for an additional three to five minutes to form a homogeneous gelO

~; 3~ The powders of Group B are added to the gel, while mixing until a homogeneous paste is formed.
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4. With stirring, the flavor of D is added and lastly the foaming agent. -. ..

5. The resultant slurry is then blended for 1 hour.
; The completed paste is then transferred to a `~ three roller mill and then homogenized, and finally tubed ,-~. '' It is found that when most flavored chewing gums such a-s-slab gums, and when most flavored chewin~ tobacco and chewable medicinal tablets are chewed and when most tooth-pastes are used in a normal toothbrushing procedure of 1-2 minutes, the initial perception of flavor appears after a minute or more at a low level, and after 3 or 4 minutes of chewing the flavor intensit~ drops to an uninteresting level. It is also found upon analysis in several instances that chewable medicinal tablets or chewing gum or tobacco chewed or toothpaste utilized for as long as thirty min-utes may retain as much as 60 percent of the flavor inltially present, and that this part of the flavoring agenk is thus not effecti ly used. ¦~

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As used herein w.ith regard to tobacco flavors the terms "alter" and "modify" in their various forms mean "supplying or imparting flavor character or note to otherwise bland tobacco, tobacco substitutes, or tobacco flavor formulations or augmenting the existing flavor characterlstic where a natural flavor is deficient in some regard or supplementing the existing flavor impression to modify its quality, character or taste"O

As used herein with regard to hot beverage flavor sub-stances, the terms "alter" and "modify" in their various forms means "supplying or imparting flavor character or note to otherwise bland dry or substantially dry hot beverage mix compositions or beverage mix flavor formu-lations or augmenting the existing flavor characteristics where a natural flavor is deficient in some regard or supplementing the existing flavor impression to modify its quality character or taste".

As used herein, the term "enhance" is intended to mean, interalia, the intensification (without change in kind of quality of aroma or taste) of one or more taste and/or aroma nuances present in the organoleptic impression of tobacco or a tobacco subst.itute or a tobacco flavor or in the organoleptic impression of a hot beverage mix which is dry or substantially dry or a flavor for said hot .
beverage mix such as a lemon or tea or mint flavor.
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Our invention thus provides (l) an organoleptically improved smoking tobacco product and additives therefor, as well as methods of making same which overcome specific ; - problems heretofore encountered in which improved smoking tobacco compositions having a flavor with good initial strength and having a flavor which is controllably released during the smoking activity at a consistently high level over an extended period of time priox to smoking and in the main and sidestreams on smoking are created or enhanced and may be readily controlled and maintained at desired uniform levels .~ regardless o variations in the tobacco components of the r' blend and, in addition, (2) an organoleptically improved "hot"
beverage powder which .is dry or substantially dry as well as methods of ma~ing same which overcome specific problems here-tofore encountered in which improved hot beverage dry or substantially dry compositions having a flavor with good initial strength and having a flavor which is controllably released during the ingestion activity at a consistently high .. .. .
leyel over an extended period of time are created or enhanced and may be readily controlled and maintained àt desired uniform l.evels regardless of variations in the components of the hot beverage.mix blend.
The flavoring composition of our invention comprises:
a~ From about 3~up to about 7 parts by weight of a non~
. confined hydrophobic flavor oil;
b. From about 3-up to about 7 parts by weight of a hydro-` lytically.releasable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, sai.d solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hyarophobic flavor oil; and .~ c. From about 0.1 up to about 1 part by weight of a solid . suspending agent selected from the group consisting of hydroxypropyl cellulose, colloidal silica t xanthan gum and ethyl cellulose.
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This invention further provides improved tobacco additives and methods whereby various nuances prior to smoking and in the main and sidestreams on smoking may be imparted to smoking tobacco products and may be readily varied and controlled to produce the desired uniform flavor characteristics wherein the -~ flavor has a good initial strength and wherein ~he flavor is controllably released during the smoking activity of a consis-tently high level over an extended period of time.

This invention in addition provides improved additives for beverage powders for incorporation with hot liquids in order to produce "hot" beverages and methods whereby various nuances in the hot beverage flavor may be imparted to such pro--~ ducts and may be readily varied and controlled to produce the ` 15 desired uniform flavor characteristics wherein the flavor has a good initial strength and wherein the flavor is controllably released during injestion of the hot beverage of a consistently ~ high level over an extended period of time.

;( 20 Thus, it has been found that it is now possible to obtain a smoking tobacco composition or substitute smoking tobacco composition containing a flavoring composition which provides an almost instantaneous flavor release prior to smoking and on smoking, in extended high intensity constant flavor percept-ion time during smoking, true flavor character and controlled release of the major proportions of flavoring agent initially present in the flavoring co~iposition. It has been further found that it is now possible to obtain a hot beverage powder compo-sition containing a flavoring composition which provides an - 30 almost instantaneous flavor release immediatley on adding the powder to a hot liquid such as alcohol or water and on injes-tion, in extended high intensity`constant flavor perception time during injestion, true flavor character and controlled release of the major proportions of flavoring agent initially present in the flavor composition. These flavoring composit-ions of our invention consist essentially of:

7~3 a. From about 3 up ~o about 7 parts by weight of a non-confined hydrophobic flavor oil;

bo From about 3 up to 7 parts by weight o~ a hydrolyti-cally releasable flavor oil physically entrapped in an edible solid material, said solid material having ; a particle size of from about 5 microns up to about 400 microns, said physioally en~rapped flavor oil being organoleptically compatible with said non-con-finred hydrophobic flavor oil~ and '' . ' ' ~
cr From about 0.1 up to about 1 part by weight of the solid suspending agent selected from the group con-sisting of hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000, a : structure as follows.

OH
OCH;~CHCH~ OH `
' CH~ OCH2CHC~3 -~- 0~ ~_ _ H Ot HzCHCH~ CH2 OH OCH2 CHCH~ :
` i ;2 5 , . - - OCH2C~tCH, OH
having a particle size such that 95% of the particle is passed through 30 mesh screens and 99~ of the part-icles are passed through 20 mesh screens and having a viscosity defined according to Figure 2; or colloidal -l silica, xanthan gum and ethyl cellulose having a part-icle size of from about 0.004 up to about 0.130 mic- .
rons, a surface area of from about 100 up to about 500 m2/gm and a density of from about 1~0 up to about 4.0 3~bsa/cu.ft.
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-~8- c Preparation of the flavoring compositions employed in the smoking tobacco or substitute smoking tobacco compositions or in the hot be~erage powder compositions of our invention may be effected by:

1. Admixillg a. From about 3 up to about 7 parts by weight of - . a non-confined hydrophobic flavor oil; and , .
b. From about 0.1 up to about 1 part by weight of a solid suspending agent selected from the group consisting of hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800tO00, having a structure:
OH
Ol:H~CHCH~ OH
CH2 ~ . O~H~CtlCH~

~( 20 ~~~ - ~ ~ - C '~~~
1~1 C)CHlCH''Hl CH.
.'i OH OCH2 CHCH~
OCHl CHCH3 ; 25 having a particle si~e such that 95% of the part-icles are passed through 30 mesh screens and 99% of the particles are passed through 2C mesh screens; having a viscosity defined according to Figure 2; and colloidal silica, xanthan gum !~ 30 and ethyl cellulose having a particle size of from about 0.004 up to about 0.130 microns, a surface area of from about 100 up to about 500 ; m /gm and a density of from about 1.0 up to about 4.0 lbs~cu.ft., thereby forming a first suspen-sion; and then .~ ~
` . , ii il~lL~793 -19- , .` .

Admixing said first suspension with from about 3 up to about 7 parts by weight of a hydrolytic~lly relea-: sable flavor oil physically entrapped in an edible solid material, said solid material having a particle size from about 5 microns up to abou~ 400 microns thereby forming a second suspension, said physically entrapped flavor oil being organoleptically compat-ible in either (i) a tobacco m~dium or in a substi-tute tobacco medium useful for fabrication of smoking l¢ articles, or (ii) a flavored hot beverage powder and ultimate beverage into which said flavored hot bev-erage powder is incorporated, with said non-confined hydrophobic flavor oil.

The smoking tobacco or substitute smoking tobacco compo-sition of our invention or the hot beverage powder of our in- .
~ vention may be prepared by the steps ofO
.: .
` 1. Admixing , 20 Ro From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil; and .. , :

b. From about 0.1 up to about 1 part ~y weight .
of a solid suspending agent selected from the group consisting of hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000, having a structure:
3~ oH .
OeH~t:HCM~ OH
CHz ~I S7CH~CHCH3 3~O _ ~OCH CHCH~ H~ ~H ~
H H ~ o OCH.CHCH~ CH2 OH OCI-I~ CHCH~
OCH, CHCH~
OM

37~3 having a particle size such ~hat 95% of ~he - particles are passed through 30 mesh screens : . and 99~ of the particles are passed through : 20 mesh screens; having a viscosity defined according to Figure 2, and colloidal silica, xanthan gum and ethyl cellulose having a particle size of from about 0O004 up to about :f 0.130 microns, a surface area of from about 100 up to about 500 m2/gm and a density of ~ 10 from about 1.0 up to about 4.0 lbs/cu.ft.,; thereby forming a first suspension (if desiredan additional product stabilizer such as propy-lene glycol may also be incorporated into the mixture);
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.` 2. Admixing said first suspension with from about 3 up to about 7 parts by weight of a hydrolytically relea-. . sable flavor oil physically entrapped in an edible solid material, said solid material having a particle size of from about 5 microns up to about 400 microns (preferably from 70 up to 300 microns) thereby form~
ing a second suspension, said physically entrapped ~i flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil; and .-. 3. Substantially uniformly distributing said second sus-. pension within either (i) the interstices of shredded ',~ smoking tobacco or a smoking tobacco substitute or ~ (ii) the body of a "hot" beverage powder.
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.; . .

. .. ...

~21- -The solid physical entrapment material used to entrap the thermally~hydrolytically releasable flavor oil may be of arious convenient physical shapes; e.g., capsules having gelatin shells; particles of dextrin ; 5 and/or modified food starch and/or gum acacia capable of adsorbing and/or absorbing and re~aining flavor oils until either (a~ subjected to smoking activity or ( to the heat transferred from smoking burning tobacco to ; tobacco which is not being smoked but being subjected to the organoleptic senses of the smoker, eOg., taste and smell or (b~ subjected to heat transferred from hot beverage liquid (e.g., liquid having a temperature of ~ from 50C up to about 100C) to the "hot" beverage ; powder being admixed with said "hot" liquid, said ' 15 liquid being used to facilitate injestion of the beverage such as coffee or ~ea.
. ., ; In carrying out the process of our invention, ( sustained release flavors are prepared by combining ~ 20 non-confined flavor oils with encapsulated or physically `~ entrapped flavor oils. These combinations are fashioned so that the free oil is bound in a network of physically ; entrapped flavor and suspending agent. The thixotropic pastes, or free flowing powders which result are products where the unconfined flavor oil, the "encapsulated" or physically entrapped flavor oil and suspending agent are held together by physical forces.

When acacia is used as the entrapment agent for ~ 30 the physically entrapped flavor oil, a suitable product ~ ~
;` results when, for example, the following combination is prepared:

~ ~22-. .
"~

.. , .... ~ ., . . .. . .. .. . ...... .. ..... . ... _ . _ _ _ _ _ _ _ _ .
~ Ingredient Parts by Weight .. , ... . _ _ _ , Spray dried menthol on 35 ; gum acacia Ethyl Alcohol (95% USP) 29 Menthol crystal~ Brazilian 35 KLUCEL ~ HF ~brand of hydroxypropyl ' cellulose manufactured by ~ Hercules Inc. of Wilmington, -~ ~ ' Delaware having a molecular weight of about 800,000 and a viscosity defined according to , Figure 23 .
~, The KLUCEL ~ HF is dispersed in the alcohol and al-lowed to hydrate~ The menthol crystals are then dissolved ` 15 in the alcohol. The spray dried menthol-gum acacia com-( bination is then dispersed in the solution. A viscous ;~~ suspension results. This suspension is then diluted with ; 95% USP ethyl alcohol and an amount equivalent to 0.3%
menthol is added to tobacco.
Two sets of 75 cigarettes each are prepared. One ` set contains 0.3% menthol applied in the traditional manner - by spraying an alcoholic solution onto the tobacco. The other set contains 0.3~ menthol in the product as set forth 25 in Table I above. The two sets of cigarettes are prepared for comparative evaluations and yield the following evalu-ations:

DAYS AFTER PR~:PARATION DIFFERENCE
7 , No difference 21 Slight Preference for product of Table I
34 Great Preference for product of Table I

'I :

.:
When ~enthol is put in solution with a film forming agent such as KLUCEL ~ HF, this agent will provide a greater barrier to retard the loss of the menthol, than if the menthol is simply added alone to the tobacco~ The inclu-sion of a spray dried menthol, e.g. spray dried on gum arabic, wiil serve to greatly extend the shelf lie. The vehicle used in the menthol product, ethyl alcohol, is a "non-solvent" for the gum arabic carrier of the spray ' dried menthol. This spray dried component of the menthol - 10 product will therefore remain intact u ntil such time as it is released by ignitiion of the tobacco during the smoking activity.

~; ~ The film forming agent selected must be soluble in the vehicle used, and it should provide sufficient viscosity so that after the addition of the spray dried component, a stable suspension results. The addition of menthol and spray dried menthol, e.g., spray dried gum arabic holding the menthol, added separately without a film forming agent resul~s in an unsatisfactory product.

This is due to differences in bulk density of the `i tobacco or the dry beverage powder ~as the case may be) and the spray dried menthol, resulting in segregation of ~S these two diferent components.

In addition to the use of such flavorants as menthol for tobacco or for flavoring or augmenting or enhancing the flavor or aroma of a "hot" beverage powder, there exists a potential use for other flavors for tobacco and in hot beverage powders, such as lemon. Thus, the following lemon f lavored produce- is yr~pared:

7~3 -2~

TABLE III
Inqredients Parts by Weight KLUCEL ~ HF (Hercules...O.- 0.8 brand of hydroxy-~` 5 propyl cellulose) Ethyl alcohol 95% o~ oo~39~2 ~food grade) Lemon flavor containing the ollowing r 10 ingredients~ -O-O- 20.0 Methyl Heptenone..... ~ 0.50 parts per 1000 of lemon flavor) Terpineol.......... ,.( 1.00 parts per 1000 of lemon flavor) Linalool............. ~ 1.00 parts per 1000 of lemon flavor) n~Decanal............ l 1.25 parts per 1000 of lemon flavor) n-Octanal........... ~ 1.25 parts per 1000 of lemon flavor) Geranyl Acetate...... ( 1.75 parts per 1000 of lemon flavor) Citral............... ( 60.00 parts per 1000 of lemon flavor) Oil of lemon, cold pressed...... ( 100.00 parts per 1000 of lemon flavor) Orange Terpenes..... ( 833.25 parts per 1000 of lemon flavor) ~, Spray Dried Lemon ~lavor (or gum arabic) containing i the following ingredients:.~............................................ 40.0 Methyl Heptenone...... ~ 0.50 parts per 1000 of lemon flavor) Terpineol............. ~ 1.00 parts per 1000 of lemon flavor) Linallol...~.......... ~ ~ 1.00 parts per 1000 of lemon flavor) n-Decanal.......... ..... ~ 1.25 parts per looa of lemon flavor) n-Octanal.......... ..... ~ 1.25 parts per 1000 of lemon flavor) - Geranyl Acetate....... ( 1.75 parts per 1000 of lemon flavor)Citral............... ( 60.03 parts per 1000 of lemon flavor) Oil of lemon, cold pressed........... ( 100.00 parts per 1000 of lemon flavor) Orange Terpenes..... ~ 833.25 parts per 1000 of lemon flavor) :; .
--.
.
.

~: ~s~

Another area where this type of flavoring system is o value is in the flavoring of tea.
:. :
The same shelf life problems exist when liquid flavors are sprayed onto tea. Attempts have been made to prepare flavored particles of the same bulk density as tea to pre-a vent segregation of the tea and flavor particle~.

, ~ F1aYOr systems consisting of liquid flavor, film form-`~ 10 ing agent, and spray dried flavor, are prepared and added - to a tea pre-mix, representing 5-10% of the complete tea blend to provide sufficient flavor for the complete blend.

Flavors such as lemon, mint, spice, orange and rum - 15 are presently ascertained to be useful.
,::
The following is an example of a mint flavored system within the scope of this invention:

`

'. ' ' . . . . .

, ; TABLE IV
:;
Ingredient Parts by_We ~ht Shellac, #3 confectionary........................................ 25.00 produced by William Zinsser & Co. of 521 West 58th St.
New York, New York . !
Ethyl alcohol 95% USP...q...,.. 25.00 KLUCEL R HF (HerculesO.c,0.25 brand of hydroxypropyl cellulose) :: I .
Mint flavor having the........................................... 20.00 following formulationo -~ - Eugenol.. -O..... O--O.~ -00 parts per 1000 of mint flavor) Methyl salicylate........... ( 1.00 parts per 1000 of mint flavor) Anethole.................... ( 2.00 parts per 1000 of mint flavor) Spearmint Oil............... (25.00 parts per 1000 of mint flavor) Menthol..................... (21.00 parts per 1000 of mint flavor) L-carvone................. O.~50.00 parts per 1000 of mint flavor) .
. Mint spray dried flavor (yum29.75 arabic) having the following formulation:
Eugenol.......................... ( 1.00 parts per 1000 of mint flavor) Methyl salicylate................ ~ 1.00 parts per 1000 of mint flavor) Anethol.............~............ ( 2.00 parts per 1000 of mint flavor) 25 Spearmint Oil.............. ...... (25.00 parts per 1000 of mint flavor) Menthol.............,............ (21.00 parts per 1000 of mint flavor) L-carvone........O.......................... (50.00 parts per 1000 of mint flavor) 7~3 ~ ! -27- ~
.~ .

In carrying out one particular aspect of the process of this invention a solution of physical entrapment agent, e.g., gelatin, modified food starch, dextrin, or gum acacia, may be formed containing 5 to 100 parts of entrapment agent per hundred parts of water, the latter being preferably at a temperature of 90F. to 180F. d uring dissolution of the entrapment agent.
:., .
~ The solution is allowed to cool preferably to 33F.
;`~ 10 to 75F. and is then solidified by spray~drying.
: ~ .
Prior to the spray-drying of the solution of entrap-ment agent and preferably after cooling to 80F. to 140F.
the desired volatile, water-immiscible flavoring agent may be added to the solution and homogenized to form an emulsion. The flavoring agents which may be employed in-clude menthol, oil of peppermint, tea flavor, cherry flavor, orange oil, lemon flavor, lime flavor oil of spearmint, fruit essences, licorice, spice oils and the like. The selected flavoring agent may be added to an amount equal to 10 to 100 percent of the weight of the entrapment agent.
Examples of the physically entrapped flavor material utili-zable in our invention are: ;

; 25 à. Cherry flavor oil physically entrapped in dextrin;
b. Cherry flavor oil encapsulated in gelatin capsules;
c. Cherry flavor oil entrapped in gum acacia;
d. Lemon flavor oil physically entrapped in dextrin;
e. Lemon flavor oil encapsulated in gelatin capsules;
f. Lemon flavor oil entrapped in gum acacia;
g. Lime flavor oil physically entrapped in dextrin;
h. Lime 1avor oil encapsulated in gelatin capsules;
i. Lime flas7Or oil entrapped in gum acacia;
j. Peppermint flavor oil physically entrapped in dextrin, k. Peppermint flavor oil encapsulated in gelatin capsules; -: -28- , "

1. Peppermint flavor oil entrapped in gum acacia;
,~ m. Oil of wintergreen physically entrapped in dextrin;
n~ Oil of wintergreen encapsulated in gelatin capsules;
O. Oil of wintergreen entrapped in gum acaia;
7 5 p. Orange flavor oil physically entrapped in dextrin;
qO Orange flavor oil encapsulated in yelatin capsules;
,.,, r~ Orange flavor oil entrapped in gum acacia;
. Cherry flavor oil entrapped in modified food ~, starch; . ' .. ~ 10 t. Lemon flavor oil entrapped in modified food ':, starch;
' . u. Lime flavor oil entrapped in modified food starch;
: v~ Peppermint flavor oil entrapped in modi,fied food starch;
w. Oil of wintergreen entrapped in modified food starch; and x. Orange flavor oil entrapped in modified food starch;
y. Dextrin menthol éntrapped in gelatin capsules;
zO Menthol entrapped in gum acacia;
ba. Tea flavor trapped :in gelatin capsules;
bb. Tea flavor trapped :in gum acacia;
bc. Tea flavor entrapped in dextrin;
-' , ' 'ca. Coffee flavor entrapped in gelatin capsules;
'" 25 ~. Coffee flavor entrapped 'in gum acacia;
: ~ ' cc. Coffee flavor entrapped in dextrin~

When the emulsion of flavoring agent in solution of entrapment agent is solidified as by spray drying the result-' 30 ant spray-dried emulsion may have the flavoring agent for '~ tobacco or a "hot" beverage powder such as an ~f instant tea" (as described more particularly in Canadian Patent 1,039,563, particularly examples 13 and 14 on page 19 of . the specification of Canadian Patent 1,039,563) or an "instant coffee" powder using, for example, the coffee flavor as more particularly described in U.S. Patent 4,145,354, issued on March 20, 1979 (particularly with reference to Example -IV at column 29, lines 1-35 of U.S. Patent 4~145,354~ or , , , ~, ~29 .

~n instant tea beverage as described more particularly in German Auslegeschrift 1,692,282 or United Kingdom Patent 1,203,729, in the form of discrete micro-droplets encap-~ulated in very fine particles of dried gelatin or it may have the flavor oil absorbed into solid particles as is the case with gum arabic or gum acaciac The solid spray-dried em~lsion will be in powder form which may be 5 microns to 400 microns in particle diameter. The preferred siæe to 70-300 microns in particle diameter.
, 10 Formation of a flavored tobacco or a flavored "hot"
beverage powder, for example, may be effected by:

1. Admixing a~ From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil ~` such as peppermint oil; and bo From about 0.1 up to about 1 part by weight of a solid suspending agent selected from the group consisting of hydroxypropyl cellulose having a molecular weight of from about S0,000 up to about 800,000, having a structure:
.

OH
OCH~ CHCHl OH
CH, ~1 OCH,CHCH, H~/~;;~O ~;~

C~ ~H H~ O
i~ ., H OCH~ CH'`H3 CH3 c.
01-1 OCH~ CHCH~
OCH 2 C?1CH, - ._ . ,. OJ1 ~30-.
... . .

having a particle size such that 95% of I
the particles are passed through 30 mesh screens and 99~ of the particles are passed through 20 mesh screens; having a viscosity defined according to Figure 2;
and colloidal silica, xanthan gum and ethyl cellulose having a particle size of from about 0~004 up to about 0.130 microns/ a surface area of from about 100 up to about 500 m /gm and a density of from abo~t 1.0 up to about 4.0 lbs/cu.ft., thereby forming a first suspension;

., , 2. Admixing said first suspension with from about iS 3 up to about 7 parts by wei~ht of a hydrolyti-cally releasable flavor oil ~uch as peppermint oil phy6ically entrapped in an edible solid mat-erial said solid material having a particle size of from about 5 microns up to about 400 microns (outside diameter) thereby forming a second sus-pension said physically entrapped flavor oil being organoleptically compatible with said non-` confined hydrophobic flavor oil ~e.g., menthol ~ being the physically entrapped oil and pepper-`` mint oil being the non confined hydrophobic flavor oil); and then either 3(a) Substantially uniformly distributing said second --suspension within an all-enveloping mass of shred-ded tobacco, e~., shredded Virginia tobacco.
~r, 3~b) Substantially uniformly distributing said second suspension as by admixing said second suspension in a previously flavored or unflavored "hot"
3S beverage powder as~ for example, described in United Kingdom Patent 1j203,7~9.

` ' ~

. -31- ~
, ;
A preferred to~acco composition has 0.5-3.0~ of flavor-ing composition in 97-99.5% by weight of tobacco, more preferably, 1 percent flavoring composition: 99 percent tobacco (based on dry weight of tobacco). Typically the tobacco will be burley, turkish, Virginia, or a suitable substitute therefor (eOg., dried lettuce leaves). In ad-dition to the above-mentioned flavors useful in our invention, other flavoring and aroma additives may be added to the ~, smoking tobacco materials or substitutes therefor either :~ 10 separately or in admixture with the above-mentioned flavor materials. These additional ma~erials are as follows:
"~ ' ~
I Synthetic Materials:
Beta-ethyl-cinnamaldehyde;
Eugenol;
Dipentene;
Beta-Damascenone;
Beta-Damascone;
Maltol;
~ 20 Ethyl ~altol;
; Delta undecalactone;
Delta decalactone;
. . Benzaldehyde;
Amyl acetate;
Ethyl butyrate;
Ethyl valerate;
Ethyl acetate;
; Beta-cyclohomocitral;
2-Hexenol~
2-methyl-5-isopropyl-1,3-nonadiene-8-one;
2~6-Dimethyl-2,6-undecadiene-10-one;
. 2~Methyl-5-isopropyl acetophenone;
- 2-Hydroxy-2,5,5,8a-tetramethyl-1-(2-hydroxyethyl)-decahydrona~hthalene;
/ 3~ . Dodecahydro-3a,6,6,9a-tetramethylnaphtho-i ~2,1-b)-furan;
4-Hydroxy hexanoic acid, gamma lactone;
. Polyisoprenoid hydrocarbons defined in Example V
I of U.S. Patent 3,589,372 issued on ~une 29, 1971; and 1 One or more 5-acyl-2-(furfurylthio)-dihydro-2,s-¦ dialkyl-3-[2H]furanones having the generic ~tructure:

$~ ~.3 R ' R j O

wherein Rl', R2', R3' and R4' are each the same or different and each represents hydrogen or methyl~

IIo Natural Oils 1~ . ' Celery seed oil;
Coffee extract;
`~ Bergamot Oil;
Cocoa extract;
lS Nutmet 3il Origanum oil.
:`
An aroma and flavoring concentrate containing the mixture of liquid non-confined flavor and physically en-trapped flavor of our invention and if desired one or more of the above indicated additional flavoring additives con-fined and/or non-confined may be added to the smoking tobacco material, to the filter or to the leaf or paper wrapper.
The smoking tobacco material may be shredded, cured, cased and blended tobacco material or reconstituted tobacco mat-erial or tobacco substitutes (e.g., lettuce leaves) or mixtures thereof. The proportions of flavoring additives ~total) may be varied in accordance with taste but insofar as enhancement or the imparting of natural, sweet or other types of desirable tobacco flavor or aroma nuances are concerned, we have found that satisfactory results are obtained if the proportion by weight of the sum total of all flavor additives both confined and non-confined of our invention to smoking tobacco material is between 250 ppm and 1,500 pm (0.025%-0.15~) of the active ingredients to the smoking tobacco material.
g .

7~3 Any convenient method for incorporating the mixture of confined and non-confined flavor materials may be em-ployed. Thus~ the confined and non confined additives of our invention taken together with hydroxypropyl cellu- ;
lose having a molecular weight of from about 50,000 up to about 800,000 or silica or ethyl cellulose or xanthan ~ gum and a suitable solvent such as foodgrade ethanol may - be made up into a paste and ~he resulting solution may ( be spread on the cured, cased and blended tobacco material or the tobacco material may be dipped into such paste.
Under certain circumstances the said paste taken alone or taken further together with other flavoring additives as set forth above may be applied by means of a suitable applicator which is a brush or roller on the paper or leaf wrapper for the smokin~ product, or it may be applied to the filter by either spraying or dipping or coating.

Furthermore, it will be apparent that only a portion of the tobacco or substitute therefor need be treate2 and C 20 the thus treated tobacco may be blended with other tobaccos ; before the ultimate tobacco product is formed. In such ` cases, the tobacco treated may have the mixture of confined and non confined flavor additives with the carrier, e~g.
hydroxypropyl cellulose of our invention in excess in the amounts or concentrations above indicated so taht when blended with other tobaccos the final product will have the percentage within the indicated range.
.. . .
In accordance with one specific example of our inven-tion, an aged, cured and shredded domestic burley tobacco is coated with a paste made up as follows:

Spray dr.ed menthol on gum arabic ~35 parts by weight; 3.0% menthol in gum arabic);

.' ' ' ' Poodqrade ethanol 95% USP
29 parts ~y weight;
,~ .
- Menthol crystals, B~azilian 35 parts hy weight;

XLUCEL6~ GF brand of hydroxypropyl cellulose : manufactured by Hercules Corp. of : . Wilmington, Delaware (molecular weight: :
~i~
about 300,000) . 1.0 parts by weight.
s Therea~ter, the alcohol is removed by evaporation ; .
and the tobacco is manufactured into cigarettes by the usual techniques. The resulting cigarettes, when treated .:
as indicated, have desired and pleasing aromas (with deli-cate, pleasant esthetic menthol nuances) which are detect-.. able in the main and sidestreams when the cigarette is : . smoked. The resulting aroma may also have green, sweet, fruity, floral or Virginia tobacco~like nuances prior to smoking and in the main and sidestreams on smoking if other : : materials as indicated above are added, e.g., l-acetyl-3,3-dimethyl-cyclohexane derivatives as specified in United States Application for Letters Patent Serial No. 834,501 filed on September 19, 1977.
' :
While our invention is particularly useful in the manufacture of smoking tobacco such as cigarette tobacco, . ~ cigar tobacco and pipe tobacco, other tobacco products ~` 3~ formed from sheeted tobacco dust or fines may also be used.
Likewise, the mixture of confined and non-confined flavor additives taken further toyether with the suspending agent ; such as hydroxypropyl cellulose or ethyl cellulose or silica~ or xanthan gum or mixtures thereof of our invention can 35 - b~ ~ncorporated with materi~ls such as filter tip materials, seam paste, packaging and the like which are used along with eobacco to form a product adapted ior smoking.

' I~

-~ ~ ~

Furthermore, the mixture of confined and non-confined flavors taken together with the carrier such as hydroxy-propyl cellulose of our invention can be added to certain tobacco substitutes of natural or synthetic origin, e.g., dried lettuce leaves, and accordingly, by the term "tobacco"
and the term "smoking tobacco" as used throughout the specification is meant any composition intended for human consumption by smoking or otherwise, whether composed of tobacco, plant parts or subs~itute materials or bot~.
. ~
Although the smoking tobacco and tea and lemon flavored products (hereinafter referred to as "first group of orally utilizable composïtions") of this inven-tion can be prepar~d from a single flavoring agent, e.g., lemon flavor or menthol Elavor, it is possible to ext~nt the range of properties of each of the members of this first group of orally utilizable compositions by use of com- -binations of two or more spray-dried flavoring compositions and two or more non-confined flavors which may or may not be different but which are organoleptically compatible with the physically entrapped flavors~ For example, it is possible to separately prepare spray-dried flavoring compositions from gelatins of various Blooms and then to add these compositions to the ~irst suspension of 1avor oil and suspension agent (e.g., hydroxypropyl cellulose) and also add spray-dried flavor to such material as ; tobacco, separately. Thus, such an orally utilizable material may, for example, contain a mixture o~ flavoring compositions prepared from a low Bloom gelatin (character-ized by a rapid flavor release~ and a high Bloom gelatin (characterized by a longer flavor release) as well as non-confined flavor oil (very rapid release). The ~ ~-properties of these resultant first group of orally utilizable materials will be intermediate to the properties obtained from each of the flavoring compositions when used separately. Specifically, if a flavoring composition formed from 50 B100M gelatin is mixed with a flavoring composition formed from 200 Bloom gelatin, and the mixture ; is both (i) added to a flavor oil and suspension ayent which composition is added to, ~or example, tokacco and (ii) added to tobacco alone, the product may have a ~lavor release wllich is substantially more even over the smoking pe~iod than i9 the case when a single ~lavoring . .
composition jllSt containing the entrapped and non-confined flavor oil and suspension is employed~

Similarly, it is possible to modify the properties of each o~ the members of the first group o~ orally utilizable materials by use of mixtures of spray-dried flav~ring compositions characterized by different ratios of entrap-ment agent to flavor oil. If t for example, a composition containing 10% flavoring agent and 90~ gelatin is mixed with one containiny 50% flavoring agent and 50~ gelatin the resulting blended flavorin~ composition, after adding non-confined flavor oil and suspension agent, will yield and orally utilizable composition having a more e~en (relation to duration of smoking activity time) liberation of flavor then is obtain~d by use of either flc~voring agent alone, . .
Liberation of flavor of the members of the ~irst group of Qrally utilizable compositions of this invention may also be modified in a controlled manner to obtain an eyen, sustained flavor level from the time that use ~e~g., - 20 smoking or stirring the tea leaves in boiling w~ter~
begins and there~ter ~or a protracted period of time far in excess of that obtained toda~ in such orally utili~able material by using various mixtures of ~lavoring ~-i compositions (a) having di~ferent particle size o~
physically entrapped fla~or, the resulting product deri~ing much of its initial flavor from the smaller particles and much of its later flavor from the larger particles, or (b) formed from gelatins of di~ferent pH (the composition formed from gelatin of higher pH (e.g., 6; giving quick release of flavor, while that formed from lower pH (e.g., 2.5) giving slower release).

A particularly desirable flavor composition of our invention contains unfixed flavor, spray-dried flavor, and suspension~ hyd~oxypropyl cellulose, in proportions of about 1~ This product is characterized by an interesting or pleasing fl~vor level which may start at 0.25 seconds from the point of lighting up the smoking :iLi'19'7~3 ~37-article and last for the entire period of smoking when admixed with the tobacco or a filter tip if such is provided with the smoking article or the wrapper.
Ovex substantially its entire period of flavor release, the flavor lev~l is higher than that of the standard flavored tobacco and the flavor is continuous, rich, full and true.

It is particularly characteristic of the orally utilizable ,~ compositions of this invention that they have almost instantaneous to very early flavor perception when used in the mouth. Usually flavor is apparent in not more than 0.25 seconds when orally utili~able compositions are prepared in accordance wi~h this invention. Prior art tobaccos and prior art teas and lemon flavors used in hot prepared beverages have initial flavor perception after 4-5 seconds and fre~uently after times as long as one minute.

It is also characteristic of each of the members of the first group of our orally utilizable compositions that they retain the flavors under conditions of use, e.g., smoking or in a hot liquid which is consumable, e.g., alcohol or water for extended periods of which may be triple that of compositions heretofore known to those skilled in the art. For example, the flavor perception time may be as long as 20 minutes in contrast to the usual 3-10 minutes which is the flavor perception time of comparable products heretofore known (e.g., U.S.
Patent No. 2,886,440).

The greater availability of flavor for use of the flavoring compositions herein described also permits attainment of high flavor level in the first group of orally utilizable compositions with use of lower amounts of flavoring oils. Orally utilizable compositions pre-pared with the flavor composition in accordance with this invention have a ~lavor character more nearly that of the original natural flavor oil than orally utilizable compositions prepared by merely the direct incorporation of the flavoring oil into the orally utilizable material without concomitant use o the phy cally entrapped ilavors and suspensicn acent-.

.
.. The term "encapsulate" may be used to describe the relation of the entrapment agent and the flavoring -.~. agent and means that the latter in the form of spray-.~ dried emuls.ion of discrete micro-droplets, is distributed substantially uniformly within or in the interstices . of finally di~ided particles of the former. The . flavoring agent is locked in within the entrapment agent (e~gO, gelatin, gum acacia, dextrin and modified fosd starch) to the exten~ that the former i5 released substantially only as the molecules of entrapment agent . are dissolved from the surface o the individual entrapment : agent particles by the hydrolytic action of the salivary . liquids.

In addition, it has now been discovered that it is ~ possible to obtain a second group of orally utilizable .; eompositions such as chewing gum, chewable medieinal ~: tablets, chewing tobacco and toothpaste containing a .. flavoring composition which provides almost instantaneous .; flavor release, extended high intensity contstant flavor perception time, true flavor character and controlled release of the major proportion of flavoring agent .: initially present in the flavoring composition. This flavoring composition of our invention consists essentially of: . . . :
.
a. From about 3 up to about 7 parts by weight of a .
non-confined hydrophobic flavor oil; .

b. From about 3 up to about 7 parts by weight of a hydrolytically releasable flavor oil physically entrapped in an edible solid material, said solid material having a particle size of from about .
: 5 microns up to about 400 microns said physically entrapped flavor oil being organoleptically :: eomp.atible with said non-confined hydrophobic fla~or oil; and ' c. From about 0.1 up to about 1 part by weight of a .
solid suspending agent which is a hydroxypropyl . eellulose having a molecular weight of from 50,000 ;1 up to 800,000 and a viscosity in solution as defined according to E'igure 2.

~ 3 -39- .

Preparation of the 1avoring composi~ion employed in conjunction with this second group of orally utilizable compositions of our inv~ntion may be effected by:

: 1~ Admixing a. From about 3 up to about 7 parts by weight of a non~confined hydrophobic flavor oil;
. and : b. From about 0.1 up to about 1 part by weight of a solid suspending agent which is a hydroxy-propyl cellulose having a molecular weight of from 50,000 up to 800,000 and a viscosity defined according to the graph in Figure 2;
. thereby forming a first suspension; and then .:.
2. Admixing said first suspension with from about .: 3 up to about 7 parts by weight of a hydrolytically releasable flavor oil physically entrapped in an edible solid material, said solid material having . a particle size of from about 5 microns up to ! ~ ' about 400 microns thereby forming a second suspension, said physically entrapE~ed flavor oil being organo-. leptically compatible with said non-confined hydrophobic flavor oil. . -:
~- i ' ' ' ` s j~ ~his second group of members of orally utilizable .
: ~i compositions of our invention such as chewing gum, chewable medicinal tablets, chewing tobacco, and toothpaste may .: be prepared by the steps of:
;~;
.~ 1. Admixing .
a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil; .
. 30 and b. From about 0.1 up to about 1 part by weight ' ic , of a solid suspending agent which is a hydroxy-~ propyl cellulose having a molecular weight : of rom 50,000 up to 800,000 and a viscosity .~ defined according to Figure 2 thereby forming .
a first suspension tif desired an additional pxoduct stabilizer such as propylene glycol may also be incorporated into the mixture);

:

.
~40-.~
:
20 Admixiny said first suspension with from about 3 up to about 7 parts by weight of a hydrolytically :~ releasable flavor oil physically entrapped in an edible solid material, said solid material having a particle size of from about 5 microns up to abou~ 400 microns (preferably from 7~ up to 300 microns) thereby forming a second suspension, `. said physically entrapped flavor oil being organo-leptically compatible with said non-confined hydrophobic flavor oil; and ( ::
~ 3. Substantially uniformly distributing said second ~ : suspension with an all-en~eloping base selected ~: from the group consisting of ~1) chewing~gum base, (2) chewable vitamin tablet base, (3) chewing tobacco, and t4) toothpaste base, depending ùpon the ultimately desired orally usable composition.
,, " ~
: The solid physical entrapment material used to entrap : 20 the hydrolytically releasable flavor oil may be~of various :: ~ csnvenient physical shapes, e.g., capsules having gelatin . I
~ shells; particles of dextrin and/or modified food starch i~ and/or gum acacia capable of adsorbing and/or absorbin~
and retaining flavor oils until exposed to the hydrolytic ~ conditions o~ the human mouth.
~1 . The gelatin which may be employ~ in this invention may be any o the grades and types o gelatin, including those obtained from e.g., tanner's ~tock, ossein, pigskin, . i ~! 30 etc. The Bloom of the gelatin which is employed may vary widely, although a particularly rapid relea~ from that ` ~ portion of the flavor which is physically entrapped may be obtained by use of gelatin having a Bloom of about 50 ~r less, the Bloom may be as high as 20Q or even higher~ 'I
Although the pH of the gelatin solution employed may all within the range of 2 to 10, it is pre~erred that it be maintained in the acid region, e.~., 2 to S.

\
' ~1 , .

In carrying out the process of our invention, sustained release flavors are prepared by combining non-confined flavor oils with encapsulated or physically entrapped flavor - QilS. These combinations are fashioned so that the free ~ 5 oil is bound in a netw~rk of physically entrapped flavor `~ and suspending agent. The thixotropic pastes, or free flowing powders which result are products where the uncon-fined flavor oil, the "encapsulated" or physically entrap-ped flavor oil and suspending agent are held to~ether by J
physical forces.
.~ ,.
~hen acacia is used as the entrapment agent ~or the ~" physically entrapped flavor oil, a suitable product results - when, for example, the followirlg combination is prepared: ;
` 15 Ingredient ~ arts by Weight Oil Peppermint 48.4 ;` Physically entrapped peppermint oil 48.4 ~
KLUCEL@ type HF manufactured by 3.2 ' Hercules Incorporated of Wilmington, Delaware having a molecular weight of approximately 800,000 _ __ __ :, . ..
Acacia may be replaced with various modified food ` 25 starches, such as Caps~l~ manufactured by the National ; Starch and Chemical Company of New York, New York, or dex-trins such as Schardinger Dextrins produced according to Example 1 to 14 of U.S. Pat. No. 3,472,835 issued on Oct.
14, 1969; or such dextrins as "Nadex'~ manufactured by the National Starch and Chemical Company of New ~ork, New York. The physical forces of these modified starches or dextrins are different from those of acaciar so that when such formulations as ~he above formulation are prepared using a modified starch or dextrin (entrapped flavor oil 3S a thin rapidly separa~ing unstable mixture results. This difficulty is corrected, however, by making adjustment ln the formulation by adding low molecular weight polyhydroxy alkanes such as propylene glycol to modify the physlcal forces of the system.

~:, O

7~3 -4~

The following composition, for example, where modif ied ; starch is used as the physically entrapment ma~erial orms a stable product:

` 5 Oil of Peppermint..... 0.,........ 0.................. 00047.25 Physically entrapped Peppermint......... 0.047025 oil produced by the spray-drying of an emulsion of modified starch, peppermint oil and water - KLUCEL~ H~............ ~................... ...5.00 Propylene Glycol...... ~................... ..Ø50 _. .

The Propylene Glycol adjusts the forces and bonding network improving the product stability.

The preparation of sustained release flavors of the various types requires formulations produced in accordance with the physical properties of the specific flavor oil 2D and encapsulating agent desired.

In the case of preparing dry, free flowing sustained release flavors, compositions having a high ratio ( from 2.-3:1 up to 5:1~ of physically entrapped oil:non-confined -~ 25 oil are used, for example:
. ~. ' ' ~

.: " ' ..
. .

-~3- ' ' ~nqredient Parts by W~ht ~a) Peppermin~ Flavor ,~ - , - Non-confined oil of......... ~..... O... ~20 peppermint ' `~
KLUCEL MF having a molecular...O~ 9 ' weight of 700,000 Physically entrapped peppermint.................................... 71 --~}1 produced by--spray dryi-ng an ~--- -~--~ -~'~~
emulsion of gum acacia, peppermint oil and waterO ~ -(b) Cherry Flavor ' ~
Non-confined cherry flavor....O.............................. ~26 ~LUC'EL~ MF.................................................... 9 -Physically entrapped--ch-erry.~ .~;~..'..-.-6'5''-`'''' ~' flavor produced by spray-drying an emulsion of modi-fied food -` ''`_t~arch, cherry' flavor and water. ~ ' These flavors have an appearance identical to standard, commercial spray dried 'flav'ors but have much more aroma resulting from the`pr`e`sence of the non-conflned flavor oil portion which is mixed w'ith^ the physically entrapped, e.g., ~pray dried, or encàpsulated portion.
.. i ~`d~ ~he value of using these-sustained release flavors in members of t~e second group of orally utilizable - compositions of our invention such as chewing gum and - chewing tobacco, other than the fact that they provide ease and convenience when used in flavoring products, as compared to adding a free flavor oil portion and an encapsulated flavor oil portion separately is:

.~
I . ':
' . . . ,~

7~
.

A. The non-confined flavor oil is not "free" in the flavor composition of our invention release form; but it is bonded by physical forces in a networ~ with the physically entrapped or "en-capsulated" oil and suspension agent, and is therefore highly protected from its environment compared to the case of a non-confined flavor oil by itself; and lp B~ A more uniform distribution of flavor exists : as compared with a product created by means of ;(' the separate addition of ~i) liquid non-confined and ~ii) dry physically entrapped flavor components.

lS In the case of powdered flavor mixes which contain physically entrapped, eOg., encapsulated flavors that are reconstituted before use, sustained release flavors are also of value. Encapsulated flavors have very little aroma;
only that aroma evolved from the residual oil which is not enrobed. A jar of cherry flavored drink powder while - having the proper amount of flavor when-reconstituted, ;; from its "encapsulated" fla~or, lacks suitable "jar aroma"
;~ w~en opened by the consumer. The use of the dry sustained ~`~ release cherry flavor of our invention provides the drink mix with good jar aroma as well as the proper flavor when reconstituted.
' ` In carrying out one particular aspect of the process of this invention, a solution of physical entrpment agent, 3D e.g. t ~elatin, modified food starch, dextrin, or gum aca-cia, may be formed containing 5 to 100 parts of entrapment agent per one hundred parts of water, the latter being pr~ferably at a temperature of 90F. to 180~F. during dis solution of the entrapment agent.

. .

,, i ,, . ' ,. . . .

~7~

-~5-~he solution is allowed to cool preferably to 33~.
to 75Fcl and it is then solidified by spray dryingO

Prior to the spray-drying of the solution of entrap-ment agent and preferably after cooling to 80F. to 140F., the desired volatile, water-immiscible flavoring agent may be added to the solution and homogeni2ed to form an ~ emulsion. The flavoring agents which may be employed in-; clude oil of peppermint, cherry flavor, orange oil, lemon flavor, lime flavor, oil of spearmint, fruit essences, licorice, spice oils and the like. The selected flavoring agent may be added in an amount equal to 10 to 100 percent - of the weight of the entrapment agent. Examples of the physically entrapped flavor material utilizable in our invention are:
.~
. a. Cherry flavor oil physically entrapped in dextrin;
b. Cherry flavor oil encapsulated in gelatin capsules;
cO Cherry flavor oil entrapped in gum acacia;
d. Lemon flavor oil physically entrapped in dextrin;
e. Lemon flavor oil encapsulated in gelatin capsules;
f. Lemon flavor oil entrapped in gum acacia;
~ g. Lime flavor oil physically ent~apped in dextrin;
h. Lime flavor oil encapsulated in gelatin capsules;
i. Lime flavor oil entrapped in gum acacia;
j. Peppermint flavor oil physically entrapped in dextrin;
k. Peppermint flavor oil encapsulated in gelatin capsules;
1. Peppermint flavor oil entrapped in gum acacia;
m. Oil of wint~rgreen physically entrapped in dextrin;
n. Oil of wintergreen encapsulated in gelatin capsules;
o. Oil of wintergreen entrapped in gum acacia;
pO Orange flavor oil physically entrapped in dextrin;
q. Orange flavor oil encapsulated in gelatin capsule6;
r. Orange flavor oil entrapped in gum acacia;
s. . Cherry flavor oil entrapped in modified food ~tarch;

.~ ~., , , I .

t. Lemon fla~or oil entrapped in modified food starch;
u. Lemon flavor oil entrapped in modified food starch;
v. Peppermint flavor oil entrapped in modified food starch;
w. Oil of wintergreen entrapped in modified food starch; and xO Orange flavor oil entrapped in modified food starch.
~ .
.~ 10 When the emulsion of flavoring agent in solution of entrapment agent is solidified as by spray-drying ~he re-sultant spray-dried emulsion may have the flavoring agent . ~ in the form of discrete micro-droplets encapsulated in ;~:/ very fine particles of dried gelatin or it may have the flavor oil absorbed into solid p`articles as is the case with gum arabic or gum acacia. The solid spray-dried emul-sion will be in powder form which may be 5 microns to 400 microns~ The preferred size being 70-300 microns.
.,, Formation of a flavored chewing gum, for example, , may be effected by:
. . , 1. Admixing a. From about 3 up to about 7 parts by weight ; 25 of a non-confined hydrophobic flavor oil;
'~ and b. From about 0.1 up to about 1 part by weight of a solid suspending agent which is hydroxy-propyl cellulose having a molecular weight of from about 50,000 up to abo~t 800, 000 and :~aving a viscosity defined according to Figure 2; thereby formlng a first sus-penslon ' ; I

~ 7;~3 ; 2. ~dmixing said first suspension with from about 3 up to about 7 parts by weight of a hydrolytically ;; releasable flavor oil physically entrapped in an edible solid material, said solid material having a particle size of Çrom about 5 microns up to about 400 microns thereby forming a second suspension said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil; and ~ .
3. S~bstantially uniformly distributing said second suspension within an all-enveloping mass of a chewable gum base~ `
,,, .
A preferred composition has 0.5-3.0 percent of fla-voring composition in 97-99.5 percent by weight of gum base, more preferably, 1 percent flavoring composition:
99 percent gum base. Typically the gum base ~ill be chicle, although it may be jelutong, guttakay, etc. Other ingred-ients including sweetening agents, coloring agents, etc~
may be present in desired amount.
',. . , Although the members of the second group of orally t~', utilizable compositions of our invention may be prepared from a single flavoring agent, e.g., cherry flavor, it ` is possible to extend the range of properties o~ the gum :
; by use of combinations of two or more spray-dried flavoring compositions and two or more non-confined flavors which may or may not be dif~erent but which are organoleptically compatible with the physically entrapped flavors. For example, it is possible to s~parately prepare spray-dried flavoring compositions from gelatins of various Blooms, and then to add these compositions to the first suspension of flavor oil and suspension agent and also ~dd the spray-dried flavor to the such material as chewing gum separately. Thus such a chewing gum may~ for example, contain a mixture of flavoring compositions prepared from a low Bloom gelatin, (characterized by a rapid ~lavor re-lease~ and a high Bloom gelatin (characterized by a longer . , .

~ 7~
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flaYor release) as well as non-confined flavor oil (very rapid release). The properties of t~e chewing gum product will be intermediate to the properties obtained from each of the flavoring compositions when used separately. Spec-ifically, if a flavoring composition formed from 50 Bloom gelatin is mixed with a flavoring composition formed from 200 Bloom gelatin, and the mixt~re is both (i) added to a flavor oil and suspension agent which composition is added to chewing gum and (ii) added to a chewing gum alone, the product may have a flavor release which is substantially more even over the chewing gum period than is the case when a single flavoring composition just con~aining the entrapped and non-confined flavor oil and suspension agent is employed.
'.~ .
Similarly, it is possible to modify the propertles of the product gum by use of mixtures of spray-dried fla-voring ~ompositions characterized by different ratios of entrapment agent to flavor oilu If, for example, a composi-tion containing 10 percent flavoring agent and 90 percent gelatin is mixed with one containing 50 percent flavoring agent and 50 percent gelatin the resulting blended flav-orin~ composition, ater adding non-confined flavor oil and suspension agent, will yield a chewing gum having a more even (relating to duration of chewing time) liberation of flavor than is obtained by use of either flavoring agent alone. ~

Liberation of the flavor of the members of the secona group of oxally utilizable compositions of our invention may also be modified in a controlled manner to obtain an even, sustained flavor level from the time that use te.g., chewing) in the mouth begins and thereafter for a protected period of time ar in excess of that obtained today in any such chewing gum, chewing tobacco, chewable medicinal tablet or toothpaste, by using various mixtures of flavoring compositions ta) having diferent particle si2e of physically entrapped flavor, tthe resulting product deriving much of its initial flavor from the smaller particles and much of its later flavor from the larger particles); or tb) furmed from gelatins of different pH, ~tho composition ~1 ,' ~ 3 ; ~49-. .
formed from gelatin of higher pH (e.g., 6) giving quick release of flavor, while that formed from lower pH (e.g., 2.5) giving slower release).

, ., A particularly desirable flavor composition of our invention contains unfixed flavor, spray~dried flavor, and suspension agent in proportions of about 1:1:0.1.
This product is characterized by an interesting or pleasing flavor level which may start at Q.25 seconds and last for i 27-28 minutes. Over substantially its entire period o flavor release, the flavor level is higher than that of the standard gum, and the flavor is continuous, rich, full ~ . and true.
:~
It is particularly characteristic of the members of the second group of orally utilizable compositions of our invention that they have almost instantaneous to very early flavor perception when used in the mouth. Usually flavor is apparent in not more than 0.25 seconds when - orally utilizable compositions are prepared in accordance with this invention. Prior art: chewing gums containing only free unfixed ~lavor have initial flavor perception ; after 4-5 seconds and frequent]y after times as long as ^~ one minute.
. ' . .
It is also characteristic of our orally utilizable compositons that they retain the flavors under conditions of vigorous mouth use for extended periods which may be triple that of compositions heretofore known to those skilled in the art. For example, the flavor perception time may be as long as twenty minutes, in contrast, to the usual 3-10 minutes which is the flavor perception time of comparable products heretofore known (e.g. U.S. Patent No. 2,886,440).
. . ..
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197~33 so-.

.~ The greater availability of flavor by use of the flavor-ing compositions herein described also permits attainment of high flavor level in the orally utilizable composition . with use of lower amounts of the flavoring oils.

Orally utilizable compositions prepared with the flavor . composition in accordance with this invention, have a flavor .; character more nearly that of t.he original flavor oil than chewing gum prepared by merely the direct incorporation of the flavoring oil into the chewing gum without concomitant use of the physically entrapped flavors and suspension agentsO
,' . ' ..
The term "encapsulate" may be used to describe the relation of the entrapment agen~ and the flavoring agent and means that the latter, in the form of a spray-dried emulsion of discrete micro-droplets, droplets, is distri-buted substantially uniformly within or in the interstices of finely divided particles of the former. The flavoring agent is locked in within the entrapment agent (e.g., gelatin, gum acacia, dextrin and modified food starch to the extent that the former is released substantially only as the mole-cules of entrapment agent are dissolved from the surface of the individual entrapment agent particles by the hydro-lytic action of salivary }iquids.

The following E~amples A-W illustrate processes for preparing the individual flavor components necessary to produce the flavor compositions of our invention.
, '~ ' .

EXAMPLE A
CHERRY FLAVOR FORMUL~TION
The following mixture is prepared:

In~redient _ _ Parts y Weight ~ugenol 1.75 : Cinnamic Aldehyde 4.50 ~ Anisyl Acetate fi.25 ~( Anisic Aldehyde 9.25 :`; 10 Ethyl Oenanthate 12.50 Benzyl Acetate 15~50 . Vanillin 25.00 . Ethyl Methyl Phenyl Glycidate 25.00 Ethyl Butyrate 37.25 lS Amyl Butyrate 50.00 Tolyl Aldehyde 12S.OO
Benzaldehyde 558.00 ; Alcohol 95% 130.00 .( 20 EXAMPLE B
LEMON FLAVOR FORMULATION
,~
Ingredient Parts by Weight ' . Methyl Heptenone 0.50 ` 25 Terpineol 1.00 Linallol 1.00 n-Decanal - 1.~5 n~Octanal 1.25 Geranyl Acetate 1.75 Citral 60.00 Oil of lemon, cold pressed 100.00 ----- -: Orange Terpenes _ 833.25 . . .

,:
: .

-52~-~:
., .
EXAMPLE C
LIME FLAVOR FORMULATION
The following mixture is prepared:

SIngredient _ Parts_by_Weight_ Cymene loO lb.
Dipentene l.Q lb.
" Oil of Lime DistIlled 3.0 lb.
600 oz. av. citral Terpineol 2~0 lb.
~( 10 Lemon Terpenes 10.0 lb.
1~ oz. av. Lime Terpenes 82.0 lb.

EXAMPLE D

20 ,rams of ~he flavor composition of Example A is emulsified in a solution containing 300 gm gum acacia and ' 700 gm water. The emulsion is spray-dried with a Bowen Lab Model Drier utilizing 250 c.f.m. of air with an inlet ~empera~ure of 500F., an outlet temperature of 200F., and a wheel speed~of 50,000 r.p.m.

EXAMPLE E
. .
20 Grams of the flavor composition of ~xample B is emulsified in a solution containing 300 gms gum acacia and 700 gm water. The emulsion is spray-dried with a Bowen Lab Model Drier utilizing 250 c.f.m. of air with an inlet temperature of 500F., an outlet temperature of 200F., -~
and a wheel speed of 50,000 rOp.m.
EXAMPLE F

20 Grams of the flavor composition of Example C is emulsified in a solution containing 300 gm gum acacia and '$
700 gm water. The emulsion is spray-dried with a Bowen Lab Model ~rier utilizing 260 c.f.m. of air with an inlet temperature of 500F., an outlet temperature of 200F., and a wheel speed of 50,000 r.p~m.

; , ~. !

, EXAMPLE G

- 50 Grams of the flavor composition of Example A is ; emulsified in a solution containing 300 gm gum acacia and 700 gm waterO The emulsion is spray-dried with a Bowen Lab Model Drier utilizing 250 c.f.m. of air with an inlet ,; temperature of 500F., an outlet temperature of 200F., and a wheel speed of 50,000 r.p.m.
!

80 Grams of the flavor composition of Example B is emulsified in a solution containing 300 gm gum acacia and 700 gm water. The emulsion is spray-dried with a Bowen Lab Model Drier utilizing 250 c.f.m. of air with an inlet , temperature of 500F., an outlet temperature of 200F~, and a wheel speed of 50,000 r.p.m.

120 Grams of the flavor composition of Example C is emulsified in a solution containing 300 gm gum acacia and 700 gm water. The emulsion is spray-dried with a Bowen Lab Model Drier utilizing 250 c.f.m. of air with an inlet ~S temperature of 500F~, an outlet temperature of 200F., and a wheel of 50,000 r.p.m.

EXAMPLE J

130 Grams of oil of peppermint redistilled is emul-sified in a solution containing 300 gm of "Nadex" dextrin - -~` (manuactured by National Starch and Chemical Co. of New York, N.Y.) and 700 gm of water. The emulsion is spray- ~
, dried with a ~owen Lab Model Drier utilizing 250 c.f.m. t !i 35 of air with an inlet temperature of 500~F., an outlet temp~
erature of 200F~, and a wheel speed o 50,000 r.p.m~
.. . .

, , 3 , , '! l 7~ 1 EYAMPLE K
~, .
150 gm of oil of peppermint natural is emulsified ~ in a solu~ion containing 300 gm of "Capsul" madified food ; ~ starch of National Starch and Chemical Co. of New York, N.Y. and 700 ~m of water~ The emulsion is spray-dried with a Bowen Lab Model Drier utilizing 250 c~f.m. of air with an inlet temperature of 500~F., an outlet temperature of 200F., and a wheel speed of 50,000 r.p.m.
EXAMPLE L

10 Parts by weight of 50 Bloom pigskin gelatin is added to 90 parts by weight of water at a temperature of 150F. The mixture is agitated until the gelatin completely dissolved and the solution is cooled to 120F. 20 Parts by weight of methyl salicylate (oil of wintergreen) is added to the solution which is then homogenized to form an emulsion having particle size typically in the range of 2-5 microns. This material is kept at 120F. under ( which conditions the gelatin will not jell.

Coacervation is induced by adding, slowly and uniformly 40 parts by weight of a 20 percent aqueous solution of sodium sulphate. During coacervation, the gelatin mole-cules are deposited uniformly about each oil droplet as a nucleusO `
.
Gelatin is effected by pouring the heated coacervate mixture into 1,000 parts by weight of 7 percent aqueous solution of sodium sulphate at 65F. The resulting jelled coacervate may be filtered and washed with water at temp-erature below the melting point of gelatin, to remove the salt. ;~
Hardeninq of the filtered cake, in this example, is efected by washing with 200 parts by weight of 37 percent ~olution of formaldehyde in water. The cake is then washed to remove residual formaldehyde.
, , 7~

.
,, , i EXAMP~E M

; 10 Parts by weight of 50 Bloom pigskin gelatin is added to 90 parts by weight of water at a temperature of 150F. The mixture is agitated until the gelatin completely dissolved and the solution is cooled to 120~F. 20 Parts by weight of the flavor of Example A is added to the solu-tion which is then homogenized to form an emulsion having f particle size typically in the range of 2-5 microns. This material is kept at 120F. under which conditions the gela-~` tin will not jell.
.
Coacervation is induced by adding, slowly and uniformly 40 parts by weight of a 20 percent aqueous solution of sodium sulphate. During coacervation, the gelatin mole-~; cules are deposited uniformly about each oil droplet as a nucleus.

Gelatin is effected by pouring the heated coacervate ~mixture into l,OOO~parts by weight of 7 percent a~ueous solution of sodium sulphate at 65F. The resulting jelled coacervate may be filtered and washead with water at temp-eratures below the melting point of gelatin, to remove the salt.
; 25 ;` Hardening of the filtered cake, in this example, is effected by washing with 200 parts by weight of 37 percent solution of formaldehyde in water. The cake is then washed to remove residual formaldehyde.

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7~

EXAMPLE N

10 Parts by weight of 50 Bloom pigskin gelatin is added to 90 parts by weight of water at a temperature of 150F. The mixture i~ agitated until the gelatin completely dissolved and the solution is cooled to 12bF. 20 Parts by weight of the flavor of Example B is added to the solu-tion which is then homogenized to form an emulsion, having particle size typically in the range of 2-5 microns. This material is kept at 120F. under which conditions the gela-tin will not jell.
.
Coacervation is induced by adding, slowly and uniformly 40 parts by weight of a 20 percent aqueous solution of sodium sulphate. During coacervation, the gelatin mole-cules are deposited uniformly about each oil droplet as a nucleus.

Gelatin is effected by pouring the heated coacervate ~( 20 mixture into 1,000 parts by weight of 7 percent aqueous solution of sodium sulphate at 65F. The resulting jelled coacervate may be filtered and washed with water at temp-eratures below the melting poinl: of ~elatinl to remove the salt.
~5 Hardening of the filtered cake, in this example, is effected by washing with 200 parts by weight of 37 percent solution of formaldehyde in water. The cake is then washed to remove residual formaldehyde.

.. . ~

~` i EXAMPLE O
10 Parts by weight of 50 Bloom pigskin gelatin is added to 90 parts by weight of water at a temperature of 150Fo The mixture is agitated until the gelatin completely - dissolved and the solution is cooled to 120F. 20 Parts by weight of the flavor of Example C is added to the solu-tion which is then homogenized to form an emulsion, having particle size typically in the ~ange of 2-5 microns. This 10 material is kept at 120F. under which conditions the gelatin . will not jell.

Coacervation is induced by adding, slowly and uniformly 40 parts by weight of a 20 percent aqueous solution of 15 sodium sulphate. During coacervation, the gelatin mole-cules are deposited uniformly about each oil droplet as a nucleus.

Gelatin is effected by pouring the heated coacervate 20 mixture into 1,000 parts by weight of 7 percent aqueous solution of sodium sulphate at 65F. The resulting jelled coacervate may be filtered and washed with water at temp-( eratures below the melting point of gelatin, to remove the salt.
.
Hardening of the filtered cake, in this example, is effected by washing with 200 parts by weight of 37 percent solution of formaldehyde in water. The cake is then washed to remove residual formaldehyde.
ÆXAMPLE P
. ~ _ A 40 percent dextrin solution is freeze-dried. This is accomplished by a conventional technique such as that ~5 described in column 4 of U.S. Pat. No. 3,404,007. The freeze-dried material is then milled to a par~icle size ~c of 20-40 mesh.

; .

J~ 3 ~O0 Grams of this freeze-dried material are then com-bined with 50 grams Qf orange oil. This is accomplished by mix~n~ ~he materials in a suitable blender, such as a ribbon blender. This results in a dry, free flowing powder having the advantages heretofore described. ~o ensure against atmospheric reaction or vaporization of the orange oil in the solid matrix, the powder is given a protective coating to seal the entrances to the inter-stices or cavities in the poro~s particulate matrix.- One suitable form of coating is a dextrin solution which has the property of forming an impermeable film for preventing - the escape of permeation of the flavoring oil.

EXAMPLE Q
A 40 percent dextrin solution is freeze-dried. This is accomplished by a conventional technique such as that described in column 4 of U.S. Pat. No. 3,404,007. The freeze-dried material is then milled to a particle size of 20-40 mesh.
, i 100 Grams of this freeæe-dried material are then com-bined with 50 grams of the flavor of Example A. This is accomplished by mixing the materials in a suitable blender, such as a ribbon blender~ This results in a dry, free-flow-ing powder having the advantages heretofore described.
To ensure against atmospheric reaction of vaporization of the flavor of Example A in the solid matrix, the powder is given a protective coating to seal the entrances to the interstices or cavities in the porous particulate matrix.
one suitable form of coating is a dextrin solution which has the property of forming an impermeable film for pre-venting the escape o~ permeation of the flavoring oil .~ , , .

!

7~3 EXAMPLE R
:
A 40 percent dextrin sol~tion is freeze-drieda This ~s~-accomplished by a conventional technique such as that described in column 4 of U~S. Pat. No. 3~404~007O The ; freeze-dried material is then mille~ to a particle size of 2Q~40 mesh.
. . . . ~ . . . ;
~: 100 Grams-of this freeze-dried material are then com-bined with 50 grams of-the fla~or of Example B. This is accomplished by mixing the materials in a suitable blender, - ~uch as~a ribbon blender. This results in a dry, free-flow ing powder having the advantages heretofore described.
To ensure against atmospheric reaction of vaporization of the flavor of Example B in the solid matrix, the powder is given a protective coating to seal the entrances to the interstices or cavities in-the porous particulate matrix.
One suitable form of coating is a dextrin solution which .;
has the-property of forming an impermeable film for pre-venting the escape of permeation of the flavoring oil.
:
1 ~ EXAMPLE~', `
. ... ... - ... . . ........... . . .
- ~^ A-4Q percent-dextrin-solution if freeze-dried. This ~¦ 25 ~5 accomplished by a conventiona~ technique such as that described in column 4 of U.S. Pat. No. 3,404,007. The freeze-dried material is then milled to a particle size of 20-40 mesh. - - ~ :-. ,~
. , . .

.
- : : -. . .:- - . . - ;
. I 'i:
. . .. ..
. I
.
. ~ ~

J
' i ~, , , j , ., .~

7~
-60- ;

100 Grams of this freeze-dried material are then com-bined with 50 grams o~ the flavor of Example C. This is accompl ished by mixing the materials in a sui~able blender, such as a ribbon blender. This results in a dry, free-flow-ing powder having the advantages heretofore described.
To ensure against atmospheric reaction or vaporization of the flavor of Example C in the solid ma~rix, the powder is given a protective coating to seal the entrances of the interstices or cavities in the porous particulate matrix.
One suitable form of coating is a dextrin solution which ~ has the property of forming an impermeable film for pre--~ venting the escape of permeation of the flavoring oil.

EXAMPLE T
Hydroxyethyl methacrylate (100 parts) is stirred with 0.05 part t butyl peroctoate in a nitrogen atmosphere at a temperature of ~0~C for 30 minutes. The resultant mixture is cooled to 25C and further 0.10 part t butyl peroctoate is added, ethylene glycol dimethacrylate (0.1 ( part) being added at the same tlme. To this casting solu-tion oil of peppermint, added in an amount of 10 parts.
After curing and granulation, the flavored powder is used as part of a flavor releasing form~lation in-smoking tobaccos or "hot" beveraye powders as exemplified infra.

XAMPLE U

Distilled 2-hydroxyethyl methacrylate (100 gm) is stirred with 0.05 gm tertiary butyl peroctoate in an an- -aerobic atmosphere at 25-70~C for 14-40 minu~es~ The resultant mixture is cooled to 25C and a further 0.10 gm o tertiary butyl peroctoate is added together with 0.15 gm of ethylene glycol dimethacrylate~ Oil of p~ppermint syrup to yield a flavored prepolylmer syrup which is s~itable for storing. After curing and granulation, the flavor-car-rying granules are added as a flavoring releasing component.
to smoking tobacco or "hot" beverage powders as set forth infra.

O

EXAMPLE W
; A. PREPARATION OF LE~ON OIL CAPSULES
PREPARATION OF THE SHELL COMPOSITION AND SOLUTION
!

Five hundred grams of water are heated ~o boil and 500 grams dextrin ~National Starch and Chemical Corporation, 78-1523) is added with rapid and efficient mixing, using a closed turbine, high shear mixer (Barrington CONVERTI JET
Model CJ-5B). Mixing is continued until a homogeneous solution is obtained.

B~ PREPARATION OF LEMON OIL CAPSULE COMPOSITION

81 Grams of lemon oil (California cold pressed oil~
is emulsified in 300 grams of the shell composition solu- , tion (A) by means of a homogenizing mixer (~arrington CONVERTI JET Model CJ-5B operated as a closed turbine unit).
At the start of the operation the temperature of the matrix composition solution is 20~C and of the lemon oil 15C
The mixing vessel is cooled during the operation of the mixture in order to prevent a rise in the temperature and to keep the temperature below 25C.
.
C. CAPSULE FORMATION AND DEHYDRATION ~--:~ ~5 One thousand grams of polyethylene glycol having an average molecular weight of 400 (Union Carbide Corporation, Carbowax 400) and at a temperature of about 25C is placed in a vessel equipped with a homogenizing mixer (Barrington CONVERTI JET Model CJ-5B operated as an open turbine unit).
One hundred grams of the lemon oil capsule composition ~B) is in~roduced into the polyethylene glycol in a thin stream with steady medium speed operation of the mixer (about 1,500 rpm shaft speed). By the action of the mixer, the lemon oil emulsion is broken up into coarse liquid particles, which in contact with the polyethylene glycol, are rapidly converted into gel particles and finally into virtually anhydrous capsule granules. t ~.
, 1 , , 7~
, 62-~ j The capsule granules are separated from the excess polyethylene glycol by means of a basket centrifuge and ~dded to smoking tobacco or ~hot" beverage powders as set :; . forth infra.

EXAMPLE Y

COFFEE FLAVOR FORMULATION

l0The following basic coffee formulation is prepared:

Ingred ents _ Parts by Weight Diacetyl (10% in 95% food grade aqueous . : ' ethanol) ~ lS Benzaldehyde Furfural 0 n 5 : Furfural Propionate l0 Trimethyl Pyrazine (10%
in 95% aqueous food grade ethanol) : 2,6-Dimethoxy phenol 2 ( 20 Pyruvic acid 15 : Furfural Mercaptan (1%l.0 solution in 95~ food grade ethanol) Furfural acetate 0.5 . Propylene glycol 68 5-Acetyl-2-(furfurylthio)-20 dihydro-2,5-dimethyl-3-12}11-furanone . , , _,.

; i , , i ~ - ~ \

-~3-.
, .
The following examples are given to illustrate embodi-!~ ments of the invention as it is presently preferred to practice it~ It will be understood that these examples are illustrative and the invention is not to be considered as restricted thereto except as indicated in the appended '~ claimsO

EXAMPLE I
~ The following mixture is prepared:
'~ ~0 - Ingredient Parts by Weight Liquid Flavor Composition....~....48.4 of Example A
Cab - O - Sil ~ M-5~ 3.2 ~Brand of Silica produced by the Cabot Corporation of 125 High Street, Boston, _ Mass. 02110;
Physical Properties:
Area: 200 m /gm Nomin~ Particle Size:
0.012 microns Density: 2.3 lbs/cu.ft.) .
The Cab-O-Sil~is dispersed in the liquid ~lavor compo-sition of Example A with vigorous stirring, thereby result-ing in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the 3~ said viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained relea~e flavor paste.

,.
.. ' ;
.

,, :

. -64- .

.
EXAMPLE II
, The followiny mixture is prepared:
;' ` ..
Ingredient _ _ Parts by Weight Liquid flavor composition of...... ..... 26 Example A
Cab-0-Sil~ M-5~ o 9 ~Brand of Silica produced by the Cabot Corporation of 125 High St., . ~ Boston, Mass. 02110;
Physical Properties:
Surface Area: 200 m2/gm Nominal particle size:
0.012 microns Density: 2.3 lbs/cu.ft.) , :~ lS TheCa~ -O-Sil ~ is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting ln a viscous liquid. 65 Parts by weiyht of the powder flavor compositions of Example D is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a dry, free flowing sustained release flavor powder.
.... .. ~
EXAMPL~ III - ... _ The following mixture is prepared~
.~, .
1 ~~` 25 ~ t `;~ Peppermint oil.......................... 47.25 ~ Propylene glycol... ,..... ~.... ~......... Ø50 ;¦ ~ab-0-Sil ~ M-5~ o~ 5.00 . (Brand of Silica produced by the . 30 Cabo~ Corporation of 125 High Street, : Boston, Mass. 02110;
Physical Properties:
. Surface Area: 200 m2/gm : _ Nominal particle size:
0.012 microns . DensitY: 2.3 lbs/cu.ft.) . . ., ~
., I . .~

.
'I
. ~
:~ i . ~ .

` - `

The Cab-O-Sil~ is dispersed in the peppermint oil with vigorous stirring, ~hereby resulting in a viscous liquid. 47.25 Parts by weight of the powder flavor comp-osition of Example J is then blended into the said viscous liquid/ with stirring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

EXAMPLE IV
~ The following mixture is prepared:
; lS
Ingredient _ _ Parts by Weight Peppermint oil.... O............. ~... 20 Propylene glycol................ ... ~ 9 Cab-O-Sil~ M-5.................. ... ~. 5 ~Brand of Silica produced by the Cabot Corporation of 125 High St.
Boston, Mass. 02110;
Physical Properties:
~ 25 Surface Area: 200 m2/gm : Nominal particle size.
0.012 microns Density: 2.1 lbs/cu.ft~) The Cab-O-Sil~ is dispersed in the peppermint oil with vigorous stirring, thereby resulting in a viscous ~ liquid. 71 Parts by weight of the powder flavor composition : of Example K is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting 3S ir. a dry, free flowing sustained release flavor powder.

' ~

7? '1t3 3 66- -, EXAMPLE V
The following mixture is preparedO

Ingredient _ _ Parts ~ Weight .
Liquid flavor composition.O... OO...... o20 of Example B
Propyl ~lycol......... O............................ O0...... O 9 Cab-0-Sil~ M 5~o~ o~o~o 5 (Brand of Silica produced by the Cabot Corp9ration of 125 High 5t. r Boston, Mass. 02110;
Physical Properties:
Surface Area: 200 m /gm Nominal Particle Size:
I5 0.012 microns Density: 2.3 lbs/cu.ft.) The Cab-0-Sil~ is dispersed in the liquid flavor comp-osition of Example ~ with vigorous stirring, thereby result-ing in a viscous liquid. 65 Parts by weight of the powder flavor composition of Example E is then blended into the said viscous liquid, with stirring at 25C or a period ; of 30 minutes resulting in a dry, free flowing sustained r lease flavor powder.
, 25 EXAMPLE VI
` ~ The following mixture is prepared:

Ingredient Parts by Weight Liquid Flavor composition................ 48.4 ~ of Example C
', Ethy~ Cellulose....... ~ O................ .3~2 r .~.

~67 The ethyl cellulose is dispersed in the liquid flavor composition of Example C with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example F is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

EXAMPLE VII
The following mixture ls prepared:

Ingredient Parts by Weight Oil of wintergreen....................... 47.25 Propylene glycol................ O~.. O.... Ø50 Cab-O-Sil~ M-5...................... ..... .5.00 (Brand of Silica produced by the Cabot Corporation of 125 High St., --Boston, Mass. 02110;
Physical Properties:
" : ~
Surface Area: 200 m /gm Nominal particle size: 0.012 microns .f Density: 2.3 lbs/cu.ft.) The Cab-O-Sil~ is dispersed in the oil of wintergreen with vigorous stirring, thereby resulting in a viscous liquid. 47.25 Parts by weight of the powder flavor compo-sition of Example L is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic sastained release flavor paste.

. ;
,~ ' ' " ' .

jl . .
EXAMPLE VIII
The following mixture is prepared-I In~redient _ _ arts by ~Wei~ht ..
i 5 ~ Liquid flavor composition of........ O~26 Example A
Propylene glycol.... O.O.O~ ......... 5.... 1 Cab-0-Sil~ M-5~ o~ o~ 9 (Brand of Silica produced by the Cabot Corporation of 125 High St., Boston, Mass~ 02110;
. Physical Properties:
-~ Surface Area: 200 m2/gm - Nominal particle si~e: 0.012 microns Density: 2.3 lbs/cu.ft.
.
The Cab-0-Sil~ is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting . in a viscous liquid. 65 Parts by weight of the powdered flavor composition of Example M is then blended into the said viscous liquid, with stirr.ing at 25C for a period of 30 minutes result.ing in a dry, free flowing sustained release flavor powder.
. . . I

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ll -69~
. .

EXAMPLE IX
- The following mixture is prepared:
`., ! I
¦' In~redient Parts by Wei ¦' Liquid flavor composition..... ,.O...... 48.4 , of Example B
! Propylene glycolD .~O.O . 2 ; Cab-O~ M-S~ o~ o~o~ 3~4 , (Brand of Silica produced by the ~ 10 i Cabot Corporation of 125 High St., ; j Boston, Mass. 02110;
' Ph~_~al Properties:
Surface Area: 200 m /gm Nominal particle size: 0.012 microns Density: 2.3 lbs/cu.ft.
- ..., .

The Cab-O-Sil~ is dispersed in the liquid flavor compo-sition of Example B with vigorous stirring, thereby result-;~ ing in a viscous liquid. 48.4 Parts by weight of the powder ` 20 flavor composition of Example N is then blended into the '~ said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.
", ~ 25 EXAMPLE X ¦
~, , . . I
The following mixture is prepared:

IngredientParts by Weight Liquid flavor composition.~.. O......... 48.4 of Example C
Propylene Glycol............. ~........ , 5 Ethyl Cellulose........................ .4.1 .
., ,. , I

,t ~1 il ~

~L11~'93 -7~-.~ . I
The ethyl cellulose is dispersed in the liquid flavor composition of Example C with vigorous stirring, thereby resulting in a viscous liquidc 48.4 Parts by weight of the powder flavor composition of Example O is then blended S in the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in thixotropic sustained release flavor paste.

;( EXAMPLE XI
, The following mixture i5 prepared:

Ingredient Parts by Weight Orange oil............ ~.................... 48.4 ~ Cab~O-Sil~ M-5~ o~ 3.2 ~ -(Brand of Silica produced by the Cabot Corporation of 125 High St., Boston, Mass. 02110;
, Ph~sical Properties: j :. Surface Area: 200 m2/gm 2~ Nominal Particle Size~ 0~012 microns Density: 2.3 lbs/cu.ft.J

i~ The Cab-O~Sil~ i9 dispersed in the orange oil with vigorous stirring, thereby resu:Lting in a viscous liquid.
48.4 Parts by weight of the powder flavor composition of ~xample P is then lended into the said viscous 1 iquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

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.
E ~PLE XI A

The following mixture is prepared:
.
In~red_ent _ Parts by Wei~ht ~love Oil. ~ o~48~4 Cab-O-Sil M-5~ 3~2 (Brand of Silica produced by the Ca~ot Corporation of 125 High Street, .
: Boston, Mass~ 02110;
.~ . Physical Properties:
"
; 10 Surface Area: 200 mG/gm ~ Nominal Particle Size: 0.012 microns .: . Density: 2.3 lbs./cu.ft.) .: ~ Xanthan gum................................ 4.2 . KLUCEL HF (Brand of hydroxypropyl..... ~.... l.0 .~ cellulose produced by the Hercules ~ Corporation of Wilmington, Delaware ................ having a molecular weight of 800,000 .
;. and a viscosity defined according . . .
. to Figure 2) ' . . . ... _ - . 20 The Cab-O-Sil , hydroxypropyl cellulose and xanthan . gum are intimately admixed. The resulting mixture of .
. Cab-O-Sil, xanthan gum and hydroxypropyl cellulosé i5 .. dispersed in the clove oil with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example Q
:. is the~ blended into the said viscous liquid, with ..
stirring at 25C for a period of 30 minutes resulting .
in a thirotr ic sustained release flavor paste.

.' . , l' -72;

EXAMPLE XII
The following mixture is prepared:

Ingredient _ _ Parts by Weight . 5 Liquid flavor composition.O... 0.~... ~.... ~ o20 ;., ;; of Example A
: Propylene glycol..... O.-O.. Y.. O~o.o.o~...... ...2 Cab~o-Sil~ M-5~ 9~ o~ 4.2 (Brand of 5ilica produced by the ( 10 Cabot Corporation of 125 High Street, Boston, Mass. 02110;
;, Physical Properties:
` Surface Area: 200 m2/gm Nominal Particle Size: 0.012 microns Density: 2.3 lbs/cu.ftl) Eth~ Cellulose...... O.. O.................... ..1.0 ~ I .
`. The Cab-O-Sil~and ethyl cellulose is dispersed in the liquid flavor composition of Example A with vigorous - 20 stirring, thereby resulting in a viscous liquid. 70 Parts ; by weight of the powder flavor composition of Example Q
( is then blended into the said viscous liquid, with s.tirring at 25C for a period of 30 minut:es resulting in a dry, ree flowing sustained release flavor powderc ¦

EXAMPLE XIII
7 The following mixture is prepared: j In~redient Par~s by Weight .. . ' 1 Li~uid flavor composition,.,................ 20 of Example A
Propylene glycol.... O..~... O.OO....... ~........ 1 , t . Cab-O-Sil M-5.......... ............... .... ... , 3 ¦
(Brand of Silica produced by the -I 35 Ca~ot Corporation of 125 High St., Boston, Mass. 02110; ¦

Physical Properties~
. Surface Area: 200 m2/gmj Nominal Particle Size; 0.012 microns .
Density: 2.3 lbs/cu.ft.) Ethyl Cellulos = = _ 3 - ~

Il I ii :,.... ~ ' . ~

The Ca~-0-Sil~ and ethyl cellulose are dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 65 Parts ! by weight of the powder flavor composition of Example Q
,; is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a dry, free flowing sustained release flavor powder.

.'~ !
EXAMPLE XIV
The following mixture is prepared:

- In~redient __ Parts by Weight .
Liquid flavor composition of....................... O.~..... ..48.4 Example B
Propylene glycol...... O............ ..,O.... ,. 2 ; C~b-O-Sil~ M-5........ ~ ................... ...3.2 ` (Brand of Silica produced by the Cabot Corporation of 125 I~igh Street, ~ Boston, Mass. 02110;
`; 20 Physical Properties:
~ Surface ~rea: 200 m /c~m :~ Nominal Particle Size: 0.012 microns ; Density: 2.3 lbs/cu.ft:.J
Ethyl cellulose............................ .~ 1.5 The Cab-O-Sil~ and ethyl cellulose is dispersed in the liquid flavor composition of Example B with vigorous ` ! stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example R is then blended into the said viscous liquid, with stir-ring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

. , .

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.~ EXAMPLE XV
; ~he following mixture is prepared:
. ~
. ~ Liquid flavor composition of........ ~.... O. ol8 , Example C
~ Propylene glycol.. O.O..... O... O...... ~....................... ....1 :~ Cab-O-Sil~ M-5~ o~ o~ 3 ~: tarand of Silica produced by the '~; ld Cabot Corporation of 125 ~igh Street, :~ 3 Boston, Mass. 02110;
Physical Pro~erties:
. Surface Area: 200 m2/gm .~ . Nominal Particle Size. 0.012 microns .
~, 15 Density: 2.3 lbs/cu.ft.~
Ethyl cellulose~.. O........................................... ...1 ;; The Cab-O-Sil~ and ethyl cellulose is dispersed in the liquid flavor composition of Example C with vigorous ¦ 20 stirring, thereby resulting in a viscous liquid. 62 Parts by weight of the powder flavor composition of Example S
::~ is then blended into the said viscous liquid, with stir-ring at 25C for a period of 30 minutes resulting in a ~`:i dry, free flowing sustained rel~ease flavor powder.
~ 25 : EXAMPLE XVI . .
~ The following mixture is prepared.
': ~
. . Ingredient _ Parts by Weight :~ 30 Peppermint oil......... ~,.................. 48.A
Propylene glycol....... ~ 2 Cab-O-Sil~ M-5~ o~ 3~8 . (Brand of Silica produced by the Ca~ot Corporation of 125 High Stre t, ~S Boston, Mass. 02110;
Physlcal Properties:
. Surface Area: 200 m2/gm Nominal Particle Size 0.912 microns Density: 2.3 lbs/co.ft.
. .
'~ ' .~ .
~ , . .
r t ~i "
$~ 7~3 The Cab-O-Sil~ is dispersed in the peppermint oil with vigorous stirring, thereby resulting in a viscous l~quid. 48.4 Parts by weight of the powder flavor compo-sition in Example T is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

~ EXAMPLE XVII
`( The following mixture is prepared:
' 10 Ingredien~ Parts by h7eight .. _ ......... , ...... ", , . _ , Peppermint oil...... O..................... O.21 Propylene glycol.... O..................... .O 1.0 t Cab-O Sil~ M-5...... ~.~......... ,......... ..2.0 (Brand of Silica produced by the t:
Cabot Corporation of 125 High Street, : Boston, Mass. 02110;
Physlcal Properties:
::: Surface Area: 200 m2/gm Nominal Particle Size: 0.012 microns Density: 2.3 lbs./cu.ft.) Ethyl cellulose............................ 3.2 The Cab-O-Sil~ and ethyl cellulose is dispersed in ~-the peppermint oil with vigorous stirring, thereby result-inq in a viscous liquid. 65 Parts by weight of the powder flavor composition of Example U is then blended into the said viscous liquid/ wi.th stirring at 25C for a period of 30 minutes in a dry, free flowing sustained release t flavor powder.

7~ :
~76-` EXA~PLE XVIII
The following mixture is prepared:
;'.~
~ Inaredient Parts bv Weiaht Liquid flavor composition of........ ~............ 52 , Example B -Propylene glycol...... O........ O... ,........ 1 Cab-O-Sil~ M-5 .~.~........... .... ....... ~. 3.8 (Brand of Silica produced by the (10 Cabot Corporation of 125 High Sto ~ . .
Boston, Mass. 02110;
Physical Properties:
- Surface Area: 200 m2/gm -- _ `~. Nominal Particle Size: 0.012 microns Density. 2.3 lbs./cu.ft.) -` EthYl cellulose............................ 2.2 f , -;` The Cab-O-Sil~ and ethyl cellulose is dispersed in the liquid flavor composition oE Example B with vigorous 2Q stirrin~, thereby resulting in a viscous liquid. 44 Parts by wei~ht of the powder flavor composition of Example V
r is then blended into the said viscous liquid, with stir-ring at 25C for a period of 30 minutes resulting-in-a thixotropic sustained release flavor paste.
-- -~----EXAMPLE XIX - - - ------- ~
The following mixture is prepared: 5 Ingredient _ Parts by Weight Liquid flavor composition.... O..... ~......... 48~4 of Example A
Propylene glycol.............~................ 3 Cab-O-Sil~ M-5 ..............l............... 5.2 ~Brand of Silica produced by the --~
Cabot Corporation of 125 High St., Boston, Mass. 02110;
Physlcal Properties- ~
.~ ~ ~.,. I
Surface Prea: 200 m~/gm Nominal Particle Size: 0.012 microns Density: 2.3 lbs./cu.ft.) T

,- : ~
' .` : I
-'' The Cab-O~Sil~ is dispersed in the liquid flavor compo-sition of Example A with vigorous stirring, thereby result-ing in a viscous liquidO 48.4 Parts by weight of the powder flavor composition of Example G is then blended into the ~aid viscous liquid, with stirring at 25C for a period ; of 50 minutes resulting in a thixotropic sustained release flavor paste.

EXAMPLE XX
The following mixture is prepared:
... .
Ingredient __ ~ Parts by Weight Liquid flavor composition.~.. ~...... .. 25 ; of Example B
Propylene glycol............. ~.............. O 2 Cab-O-Sil M-5 ~ o~ 10 (Brand of Silica produced by the Cabot Corporation of 125 High St., Boston, Mass. 02110;
Physical Properties:
Surface Area- 200 m2/gm ` Nominal Particle Size: 0.012 microns Density: 2.3 lbs./cu.ft.) Ethyl cellulose.............. 4 ~, ~
The Cab-O-Sil~ and ethyl cellulose is dispersed in the liquid flavor composition of Example B with vigorous -' stirring, thereby resulting in a viscous liquid. 65 Parts by weight of the powder flavor composition of Example H
is then blended into the said viscous liquid, with stir-ring at 40C for a period of 100 minutes resulting in a dry, free flowing sustained release flavor powder.

-7a~-. .
EXAMPLE XXI
The following mixture is prepared:
. I
~ redient Parts by Welght :i :l ~ . . j .
Liquid flavor composition.~O~Oc o~25 of Example C
, Propylene glycol.......... O....... 9.~... 0.. 1 ~' ¦ Cab-O-Sil~ M-5 ~ OO~ 3 rand of Silica produced by the I Cabot Corporation of 125 High Sto, s Boston, Mass. 02110;
I Physical Properties: -Surface Area: 200 m2/gm 1~ Nominal Particle Size: 0.012 microns Density: 2.3 lbs./cu.ft.) Ethyl cellulose............................ '3 :
.~ ~ .
The Cab O~Sil and ethyl cellulose is dispersed in the liquid flavor composition o Example C with vigorous stirring, thereby resulting in a viscous liquid. 65 Parts by weight of the powder flavor composition of Example I
is then blended into said ViSCOllS liquid, with stirring at 25C for a period of 30 minules resulting in a dry, free 1Owing sustained release 1avor powder.
.

. ,.
.. ..

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;; -79-EXAMPLE XXII
The following mixture is prepared-.. . .
: .
Liquid Flavor Composition............. ~0.. 48.4 of ExamDle A
KLUCEL~ HF (Brand of hydroxypropyl.~.OO.O. 3~2 cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 800,000 and viscosity properties as defined according to Figure 2 ~see note 1) r. _ The KLUCEL~ HF is dispersed in the liquid flavor composition of Example A with vigorous stirring thereby resulting in a viscous liquid. 48~4 Parts by weight of ` the powder flavor composition of Example D is then i blended into said viscous liquid with stirring at 25C
for a period of 30 minutes resulting in a thixotropic - 20 sustained release flavor paste.

KLUCEL~ is a brand of hydroxypropyl cellul~se manufactured by the Hercules Corporation of Wilmington, Delaware having the structure;

OH
3 0 ~OCH1 CHCH3 ~H
jH~ OCH2 CHCH3 I( H OH ~ o ~H H\~H
; __ _ _ O ~/ I\H /L_ _ _ H OCH2CHCH~ CH2 ~5 DH OCH,CHCH, OCH~ C~1CH3 , .
having a particle size such that 95% of the particles are passed through 30 ~esh screens and 99% of the material is passed through 20 mesh screens.

.~ , ' ,, . , , ,~ , EXAMPLE XXIII
The following mixture is prepared:

Ingredient _ _ _ Parts by Weight S Liquid Flavor Composition......Ø.......... 48.4 of Example A
KLUCEL~ EF (brand of foodgrade............ 0O 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 50,000 and viscosity properties defined according to - Fi~ure 2) The KLUCEL~ EF is dispersed in the liquid flavor compo- ~
sition of Example A with vigorous stirring, thereby result-ing in a viscous liquid. 48.4 Parts by weight of the powder ; flavor composition of Example D is then blended into the said viscous liquid, with stirring at 25C for a period - 20 of 30 minutes, resulting in a thixotropic sustained release flavor paste.
., . . ~ i.

EXAMPLE XXIV
The following mixture is prepared:
. -Ingredient Parts by Weight - .
Liquid Flavor composition............. 0.. o48~4 of Example A
KL~CEL~ F (brand of hydroxypropyl........ .. 3.2 cellulose manufactured by Hercules I Corporation of Wilmington, Delaware having a molecular weight o~ 100,000 and viscosity properties defined according to Figure 2 ) . ` ~., " ' '' ' ' .

!
.

The KLUCEL~ F is dispersed in the liquid flavor compo-~tion of Example A with vigorous stirring, thereby result-ing in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with s~irring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor pasteO
.
EXAMPLE XXV
The following mixture is prepared:

. .
Ingredient Parts by Weight , Liquid Flavor Composition.. O.......................... ...48O4 of Example A
KLVCEL~JF ~brand of foodgrade.O.~.... OO. 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Dela~!~are having a m~l~cular weight of 120,000 and viscosity properties defined according to Figure 2) : The KLUCEL~JF is dispersed in the liquid flavor compo-sition of Example A with vigoro~ls stirring, thereby result-ing in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor pasteO
.
EXAMPLE XXVI
The following mixture is prepared:
. Ingredient Parts by Weight Liquid Flavor Composition.O.O..O....O...48.4 of Example A
3$ KLUCEL~ F ~brand of foodgrade ...................... 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, ~elaware having a molecular weight of 300,000 and viscosity properties J defined accordinq to Figure 2) , i.

" , ~ '7~3 ~2-The KLUCEL~GF is dispersed in the liquid flavor compo-sition of Example A with vigorous stirring, thereby result~
J:~ ing in a viscous liquid~ 48.4 Parts by weight of the powder flavor composition of ~xample D is then blended into the said viscous liquid, with stirring at 25C for a period of 30 min~tes, resulting in a thixotropic sustained release flavor paste.
' EXAMPLE XXVII
The following mixture is prepared:
.~
Ingredient Parts by Weight Liquid Flavor composition........... O... 48.4 of Example A
KLUCEL~ F (brand of foodgrade........... 3.2 - hydroxypropyl cellulose manufactured by ~ercules Corporation of Wilmington, Delaware having a molecular weight of 700,000 and viscosity properties defined according to Figure 2) . .__ . ............................. ~.
~ 20 The KLUCEL R MF is dispersed in the liquid flavor composition i of Example ~ with vigorous stirring, thereby resulting in a viscous liquid. 48O4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid with stirring at 35C for a period of 50 minutes resultin~ in a thixotropic sustained release flavor paste.
, EXAMPLE XXVIII
The following mixt~re is prepared: -Ingredient Parts by Weight Liquid Flavor Composition of.............. 48.4 Example A
KLUCEL~ HF (brand of foodgrade............. 3.2 hyd~oxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 800,000 and viscosity properties defined according to Fia ure 2 ) ` i - ----- -- - - --- - --- -`

~3 The KLUCEL~ HF is dispersed in the liquid flavor compo-s;tion of Example A with viyorous stirring, thereby result-ing in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.

( _ AMPLE XXIX
The following mixture is prepared:

Ingredient _ _ Parts by Weight Liquid Flavor CompositionØ.......... 0............. 48.4 of Example B
lS KLUCEL~ EF (brand of foodgrade........... ............ 3.2 -`
hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 50,000 and viscosity properties defined according to Figure 2 ~( The KLUCEL~ EF is dispersed in the liquid flavor compo-sition o~ Example A with vigorous stirring, thereby result-ing in a viscous liquid. 48.4 Parts by weight of the powder !; 25 flavor composition of Example D is the~ blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.

EXAMPLE XXX
The following mixture is prepared:

Ingredient Parts bv Weight ..
Liquid Flavor Composition.... ~................................ 48.4 35 of Example B
; RLUCEL~ LF (brand of foodstuff hydroxy ... .3.2 propyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 100,000 and viscosity properties defined accordin~ to Figure ~) _ ,, . 1.

t . ' :

7~ 3 . .

The KLUCEL~ L~ is dispersed in the liquid flavor compo-sition of Example A with vigorous stirring~ ~hereby result-lng in a viscous liquid. 48.4 Par~s by weight of the powder flavor composition of Example D is then blended into the ; 5 said viscous liquid, with stirring at 25C for a period ; of 3Q minutes, resulting in a thixotropic sustained release ` flavor paste.

EXAMPLE XXXI
The following mixture is prepared:

Ingredient Parts by Weight Liquid Flavor Composition................ 48 4 of Example B
KLUCEL~ JF (brand of foodgrade............ 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, -Delaware having a molecular weight of ~ 12OJOOO and viscosity properties 2~ defined according to Figure 2) THE KLUCEL~ JF is dispersed in the liquid flavor compo-sition of Example A with vigorous stirring, thereby result- ~5 ing in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirring at 25C for a period o 30 minutes, resulting in a thixotropic sustained release flavor paste.

EXAMPLE XXXII
The following mixture is prepared.
. . , . I
Ingredient Parts by Weight Liquid Flavor Composition.......... -.-.-.48.4 of Example B
; RLUCEL~ GF (brand of foodgrade............ 3.2 ,. ¦
of hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 300,000 and viscosity properties defined accordinq to Fiqure 2) ~ . :

., .

The KLUCEL~ GF is dispersed in the liquid flavor composition of ExampIe A with vigorous stirring, thereby resulting in a viscous liquid. 4'8.4 Par'ts'by we'ight of the powder flavor composition of Example D is then biended in~o the said'viscous liquid, wi~h stirring at 25~C for a period of~30 minutes,~resulting in 'a~thixotropic sustained release flavor paste.
, E~AMPLE XXXIII
The following mixture is prepared:
-: .
-~redi-ent - ---~ rts--by-Weight -Liquid Flavor Composition......... ~... ..... 48.4 of Example B
KLUCEL~ MF (brand of foodgrade.u....... ..... . 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, ' Delaware having~a molecular weight of -700,000 and viscosity properties ~0 -de~~~ined-~accordrng to-Figure-2~--- ------------------------The KLUCEL~ MF is dispersed in the liquid flavor compos1tion of Example A with vlgorous stirring, thereby ^resulting in a vlscous liquid. 48.4 Par'ts by weight of 25- the powder flavor composition of Example D i's th'en' blended into the said viscous liquid, with stirring at 25DC for a period of 30 minutesd' resulting in~a' thixotropic sustained release flavor paste.

EXA~PLE XXXIV
The following mixture''is prepared:
Ingredient __ _ __ _ __ _ Parts by Weight -Liquid Flavor Composition............... 48.4 of Example B
KLUCEL~ HF (brand of foodgrade........... 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington Delaware having a mo!ecular weight of 800,000 and viscosi~y properties deined accordin~ tv Figure 2) ' ~ .
, a~9 3 -~6-The KLUCEL~ HF is dispersed in the liquid flavor composi~ion of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirring at 25~C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.
,~ .
EXAMPLE XXXV
;~ 10 The following mixture is prepared:

-Inqredient Parts by Weight . _ .
Liquid Flavor Composition................. 48.4 of Example C
KLUCEL~ EF ~brand of foodgrade........ O.0O 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 500,000 and viscosity properties defined according to Figure 2) ; ( - - .
The KLUCEL~ EF is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirrins at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.

EXAMPLE XXXVI
The following mixture is prepared:
Inq~redient ~ Parts by Weight .
Liquid Flavor Composition... ~..... ~....................... 4~.4 of Example C
KLUCEL~ L~ (brand of foodgrade............ ..3.2 hydroxypropy~ cellulose manufactured by }lercules Corporation o Wilmington, Delaware having a molecular weight of 100,000 and ~iscosity properties defined accordinq to Fiqure 2) ' :
.

!

~7 The RLUCEL~ LF is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby -~ resulting in a viscous liquid. 48~4 Parts by weight of the powder flavor composltion of Example D is then blended into the said viscous liquid, with stirring at 25~C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste~ ' .
E KA~: 'L-- :~ X:(VI I
The following mixture is prepared:
!
Ingredient Par~s by Weight Liquid Flavor composition....O...~..OO.~.48.4 of Example C
KLUCEL~ JF (brand of foodgrade............ 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, ~ Delaware having a molecular weiaht of ! 120,000 and viscosity properties defined according to Figure 2) ( ~0 The KLUCEL~ JF is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirrin~ at 2S 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.
~. , ;~ EXAMPLE XXXVI I I
The following mixture is prepared:
Ingredient Parts by Weight Liquid Flavor Composition.............. ~4~.4 ~ of Example C
- KLUCEL~ GF ~brand of foodgrade.~....... ..3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, ~-Delaware having a molecular weight of 300,000 and viscosity properties defined accordin~ to Fi~ure 2) ;
' , ;

~he KL~CEL~ GF is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then iblended into the said viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.

( EXAMPLE XXXIX
The following mixture is prepared:

.
Inqredient Parts by Weight _ .
Liquid Flavor Composition................ 4804 of Example C
KLUCEL~ MF (brand of foodgrade........ c.. .3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of ; 700,000 and viscosity properties defined according to Figure 2) ( The KLUCEL~ MF is dispersed in the liquid flavor compGsition of Example A with vigorous stirring~ thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the saild viscous liquid, with stirring at 25C for a period of~30 minutes, resulting in a thixotropic sustained release flavor paste.

EXAMPLE XL
The following mixture is prepared:
Inqredient Parts by Weight _ Liquid Flavor Composition............ ...48.4 of Example C
RLUCEL~ HF (br~nd of foodgrade....... ~,. 3.2 ,-hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 800,000 and viscosity properties defined according to Figure ? ) il - - ' ~

-8g- 1 .. , The RWCEL~ HF i5 dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of ; the powder flavor composition of Example D is then blended into the ~aid viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.
r ' , . , , ~, EXAMPLE XLI
: The following mixture is prepared.
Ingredient Parts by Weight Liquid Flavor Composition....... 0............. 4804 ~-of ~xample D
KLUCEL~ ~F (brand of foodgrade.......... ..... l 3.2 hydroxypropyl cellulose manufactured by Hercules Corporation of Wilmington, Delaware having a molecular weight of 50,000 and viscosity properties defined according to Figure 2) ( The KLUCEL~ EF is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Examplé D is then blended into the said viscous liquid, with stirring at ` 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.
, , ~
~` ~ EXAMPLE XLII
The following mixture is prepared:
Ingredient Parts by Weight 5 Li~uid Flavor Composition....... ,....... ,.48~4 of Example D
KL~CEL~ LF (brand of foodgrade.......... ...3.2 ~ ~
hydroxypropyl cellulose manufactured ~! ¦
by Hercules Corporation of Wilmington, !.
Delaware having a molecular weight of 100,000 and viscosity properties defined accordin~ to Fi~ure 2) .. . .
:
.
"
1, 3'~ 3 g - , :
. . .

The KL~C~L~ LF iS dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example D is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes, resulting in a thixotropic sustained release flavor paste.
I

~r '~ ' ' ' ~
, ;' .

, -91-- . , , EXAMPLE XLI I I
A tobacco blend is made up by mixing the following materials:
In~redient Parts by Weight . Bright 40.1 Burley 24.9 Maryland 1.1 Turkish 11.6 -~ Stem (flue cured) 14~2 Glycerine 2.8 Water 5.3 : ~he above tobacco is used in produced cigarettei ~ :
.` and a formulation produced according to Example I
incorporated into each of these cigarettes.
Ingredient Parts by Weight ^ Ethyl butyrate .05 Ethyl valerate .05 ( Maltol 2.00 .` 20 Cocoa extract 26.00 Coffee extract 10.00 . Ethyl alcohol 20.00 Water 41.90 . ` The above flavor is incorporated into model '~filter"
cigarettes at the rate of 0.1% One-third of these mvdel cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced accord-ing to Example I at 100 ppm per cigarette. Another third of these cigarettes are treated in the ilter with the :-. 30 mixture of free and entrapped flavor produced according to Example I at the rate of 2 x 10 5 gm and ~ x 10 5 gm.
When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor ~ to have a cherry flavor and aroma nuance in the mainstream : and in the sidestream on smoking and, ~n addition, prior to smoking.

,. . .

, ~

~ '7~

EXAMPLE XLIII-A
.~.
.. A tobacco blend is made up by mixing the followi~
materials:
In~redient ~ i3~t Bright 40~1 ~ Burley 24~
;.~ Maryland . 1~1 . Turkish 1~6 ... Stem (flue cured~. . 14.2 ; 10 Glycexine 2,8 . . W~ter 5'3 ~l The above to.bacco is used in produced cigarettes . and a formulation produced according to ExamPle XI-A
incorporated into each of these ci~arettes.
.'' .................
: Ingredient Parts ~by ~eight :~ Ethyl butyrate ~Q5 .~ ~thyl valerate ~~Q5 Maltol - 2~.QQ
C~coa extract 26Ø0 Coffee extract . lQ~0.0 . ~thyl alcohql .. ^ ~~Q
. ~ater 4~Q -- .

The above flavor i~ incorporated into model "filte~'l . cigarettes at the rate of 0.1%. One-third of these-model .. ci~arettes are treated in the t~b~cco section with the mixture of free fl~vor and entrapped flavor produced .~ according to Example XI-~ at la0 ppm per cigarette.
Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor . 30 produced according to Example XI-A at the r~te of ~ x 10 ; gm and 3 x 10 ~m. When evaluated by paired comparison, .
: the cigarettes treated both in the tobacco and in the : ilter with the mixture of entrapped and free flavor . taken further together with suspension agent (silica) are .~ ound, in smoking ~lav~r to have a clove--like flavor and aroma nuance in the main stream and in the side stream ~; smoking and, in addition, prior to smoking~
,,: ' ,~ , ~
., , 7~

!

EXAMPLE XLIV
A tobacco blend is made up by mixing the following materials:
~Lredient Parts_~y Weight I

Brigh~ 40~1 j Burley 24.9 Maryland 1.1 Turkish 11.6 Stem (flue cured)14.2 ~ Glycerine 2.8 Water 5.3 . . . ..
The above tobacco is used in produced cigarettes and a formulation produced according to Example II
- incorporated into each of these cigarettes.

IngredientParts by Weight .~
Ethyl butyrate 005 , Ethyl valerate .05 0 Maltol 20 00 Cocoa extract 26000 Coffee extract 10.00 Ethyl alcohol -20.00 Water 41.gO
;~ , . .
' ~ The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture o free flavor and entrapped flavor produced according to Example II at 100 ppm per cigarette.
~nother third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example II at the rate of 2 x 10 5gm and 3 x 10 5 gm. When evaluated by paired comparison, , the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on ~moking and, in addition, prior to smoklng.

, 7~
- 9 ~

EXAMPL~ XLV
A tobacco blend is made up by mixing the following - materialso Inqredient Parts by Wei~ht S Bright 40.1 Burley 24~9 Maryland lql ~urkish 11.6 ( Stem (flue cured) 14~2 Glycerine 2u8 Water 5O3 ' The above tobacco is used in produced cigarettes and a formulation produced according to Example III
incorporated into each of these cigarettes.
1 5 ' ,, Ingredient Parts by Weight ._ , Ethyl butyrate ,05 Ethyl valerate .05 Maltol 2.30 2~ Cocoa extract -26.00 Coffee extract 10.00 Ethyl alcohol 20~00 Water 41.90 ,,.:, The above flavor is incorporated into model "filter';
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example III at 100 ppm per cigarette.
Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example III at the rate of 2 x 10 5gm 7 and 3 x 10 5 gm. When evaluated by paired comparison, 5 the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a peppermint flavor 7, and aroma nuance in the mainstream and in the sidestream ,~
on smoking and, in addition, prior to smoking, t i 9 5 EXAMPLE XLVI
A tobacco blend is made up by mixing the following materials~
In~redient Parts_by Weight 5 Bright 40~1 Burley 24.9 Maryland 1.1 r Turkish 11.6 : Stem (flue cured) 14.2 : 10 Glycerine 2.8 ~ ~ Water 5~3 .~ .... ;
The above tobacco is used in produced cigarettes ~ ' and a formulation produced according to Example IV
;~ -incorporated into each of these cigarettes.

IngredientParts b~ Weight Ethyl butyrate l05 ( . Ethyl valerate .05 `. Maltol 2.00 Cocoa extract . 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 Water 41.90 :..
. The above flavor is incorporated into model "filter"
; 25 cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced.
according to Example IV at 100 ppm per cigarette. Another - third of these cigarettes are treated in the Eilter with the mixture of free and entrapped flavor produced accord.ing to Example IV at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both ~n the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent ~ 35 (silica) are found, in smoking flavor to have a peppermint flavor and aroma nuance in the mainstream and in the sidestream ~ on smoking and, in addition, prior to smoking, .

~6 ` ' .. , - EXAMPLE XLVII
A tobacco blend is made up by mixing the following : materials: i Ingredient Par~s by Weight ~right .40.1 Burley 24.9 Maryland 1.1 Turkish 11.6 ~tem (flue cured) 14.2 Glycerine 2.8 Water 5,3 :
The above ~obacco is used in produced cigarettes and a formulation produced according to Example V incorporated ` into each of these cigarettesO
In~redientParts by Weight , . Ethyl butyrate . O0 .~1 Ethyl valerate .05 ~( ~ Maltol 2.00 Cocoa extract 26.00 Coffee extract 18.00 .Ethyl alcohol . ~o.oo Water 41.90 The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example V at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example V at the rate of 2 x 10 5 gm and 3 x 10 5 gm.~ When evaluated by paired comparison, the cigarettes treated both in the i'~
tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent -(silica) are found, in smoking flavor to have a lemon ~lavor and aroma nuance in the mainstream and in the sidestream on smoking andO in additionO prior to smokingO

.
q.

;, . .

; ~97-.~ , .
EXAMPLE XLVIII
A tobacco blend is made up by mixing the following ~ materials:
- Ingre ient Parts_by Weight Bright 40.1 ~ Burley 24.9 - Maryland l.l Turkish 11.6 f Stem (flue cured) 14.2 ` 1~ Glycerine 20 8 Water 5.3 .. ~ . . .
' The above tobacco is used in produced cigarettes and a formulation produced according to Example VI incorporated into each of these cigarettes.
`` 15 Ingredient Parts by Weight . ; . .. .
Ethyl butyrate .05 ~`~ Ethyl valerate .05 ~g - Maltol 20 00 ', 20 Cocoa extract 26.00 Coffee extract 10~00 ,~ Ethyl alcohol 20.00 ; Water 41.90 ; The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according ,.... .
~o Example VI at 100 ppm per cigarette. Another third of --- these cigarettes are treated in the filter with the mixture-of free and entrapped flavor produced according to Example VI at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a lime flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.

. .

;
-98- ~

XAMPLE XLIX
A tobacco blend is made up ~y mixing ~he following materials:
Ingredient Parts b~_Weight , Bright 40.1 Burley 24.g Maryland 1.1 Turkish ~ 11.6 il Stem (flue cured~ 14.2 i 10 Glycerine 2.8 ~ ~ater 5.3 : ., The above tobacco is used in produced cigarettes and a . formulation produced according to Example VII incorporated into each of these cigarettes.
.
Inqredient Parts by Weight . Ethyl b~tyrate O05 Ethyl valerate .05 ( ~altol 2.00 Cocoa extract 26.00 Coffee extract 10.00 . ; Ethyl alcohol 20~00 : Water 41.~0 ,, .
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of ree flavor and entrapped flavor produced according to Example VII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example VII at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated ; by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a wintergreen 1avor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.

' EXAMPLE L
A tobacco blend is made up by mixing the following materials~
Ingredient Parts by Weight Bright 40~1 j Burley 240 9 Maryland 1.1 ( Turkish 11.6 i Stem (flue cured)14.2 Glycerine 2.8 Water 5.3 .-~ . ' !
The above tobacco is used in produced cigarettes and a , formulation produced according to Example VIII incorporated into each of these cigarettes.

Parts by Weight Ethyl butyrate .05 Ethyl valerate 05 ( Maltol 2.00 Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 - Water 41.90 The above flavor is incorporated into model "f ilter"
cigarettes at the rate of 0~1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example VIII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture - 30 of free and entrapped flavor produced according to Example VIII at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent 3S (~ilica) are found, in smo~ing 1avor to have a cherry flavor and aroma nuance in the mai~stream and in the sidestream on smoking and, in addition, prior to smoking.
?

9~3 ' ~ 10~-.
.; -EXAMPLE LI
` A tobacco blend is made up by mixing the following ; materials:
` Ingredient Parts by Wei~ht B~;ght -40.1 -l Burley 24.9 Maryland lol Turkish llo 6 ( Stem (flue cured~ 14O2 Glycerine 2.8 Water 5~3 ;: ,. i The above tobacco is used in produced cigarettes and a formulation produced according to Example IX incorporated into each of these cigarettes.
Ingredient Parts by Weight ` Ethyl butyrate .05 Ethyl valerate .05 ( Maltol . 2.00 Cocoa extract 26.00 ' Coffee extract 10~00 `~ Ethyl alcohol 20 00 ~ Water 41.90 ~~~
, . ~.
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example IX at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of frei~ and entrapped flavor produced according to Example IX at tne rate of 2 x 10 5 gm and 3 x 10 5 gmD When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on ; smoking and, in addition, prior to smoking.

.

7~3 .:
, .
i~, EXAMPLE LI I
., ; A tobacco blend is made up by mixing the following materials:
I_~redient Parts by Weight ; 5 Bright 40.1 Burley 24.9 ~ aryland lc '` Turkish 11~6 Stem (flue cured) 14.2 Glycerine 2.8 Water 5~3 The above tobacco is used in produced cigarettes and a r,' formulation produced according to Example X incorporated into each of these cigarettes.
". 15 Ingredient Parts by Weight , Ethyl butyrate .05 Ethyl valerate O05 ~`( Maltol 2.00 Cocoa extract 26~00 ' Coffee extract 10.00 Ethyl alcohol 20.00 - Water 41.90 .;: ' , .
The above flavor is incorporated into model 'ifilter"
cigarettes at the rate of 0.1~. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped 1avor produced according to Example X at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to ~xample X at the rate of 2 Y 10 gm and 3 x 10 gm. When evaluated by paired comparison, the cigarettes treated both in the ~! ' tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent lsilica) are found, in smoking flavor to have a lime flavor and aroma nuance in the main5tream and in the sidestream on ~moking and, in addition, prior to smoking.

:' '.

-102~

.
EXAMPLE LI I I
. .
A to~acco blend is made up by mixing the following ,~ materialso In~redientParts by Weight : 5 Bright 40.1 Burley 24.9 Maryland 1.1 ~ Turkish 11.6 .~ Stem ~flue cured)1~.2 Glycerine 2.8 . Water 5.3 :
~ The above tobacco is used in produced cigarettes and a ;: formulation produced according to Example XI incorporated . into each of these cigarettes~
: .
In~redient Parts by Weight Ethyl butyrate .Q5 :~ Ethyl valerate .05 Maltol 2.00 Cocoa extract 26.00 ~ 20 Coffee extract 10.00 . Ethyl alcohol . 20.00 Water 41.90 ~~
The above flavor is incorporated into model "fil er"
~ cigarettes at the rate of 0.1%. One-third of these model ~5 cigarettes are treated in the tobacco section with the : mixture of free flavor and entrapped flavor produced according to Example XI at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XI at the rate of 2 x 10 5 ym and 3 x 10 5 ~. When evaluated by paired comparison, the cigarettes treated both in the ¦
tobacco and in the filter with the mixture of entrapped and '' free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a orange flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.

~.

'; -103-'-;
~ EXAMPLE LIV
'; A tobacco blend is made up by mixing the following materials:
' Ingredient Parts by Weight ': S Bright 40.1 . Burley 24~9 Maryland l~
~urkish 11.6 :' . Stem (flue cured)14.2 ~ lO Glycerine 2.8 '' . . Water 5.3 - .. .
The above tobacco is used in produced cigarettes and a : formulation produced according to Example XII incorporated `~ ~ into each of these cigarettes.

'~ 15 . Ingredient Parts by Welght ''. Ethyl butyrate 005 Ethyl valerate .05 { ' Maltol 20 00 ~. Cocoa extract 26000 ':~ 20 Coffee extract 'lO.OO
~ ~Ethyl alcohol 20.00 ; Water 41.90 . ~ ,--. .
e above flavor is incorporated into model "filter" ~ :
` cigarettes at the rate of Ool~ One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XII at lOO ppm per cigarette~ Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XII at the rate of 2 x lO gm and 3 x lO 5 g~. When evaluated by paired comparison, the cigarettes treated both in the ! tobacco and in the' filter with the mixture of entrapped and ~` free flavor taken further together with suspension agent ~silica) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking, , , :
,~
' 9 , I -~, . .

63~7~
10 4 ~- !
. ` . , .'1 .
EXAMPLE LV
tobacco blend is made up by mixing the following materials:
In~redient Parts by Weight ~right ~ 40.1 Burley 247 9 ~aryland 1.1 .~ . .
Turkish 11.6 Stem (flue cured) 14.2 Glycerine ~8 Water S.3 The above tobacco is used in produced cigarettes and a ormulation produced according to Example XIII incorporated ~" into each of these cigarettes.
.- , lS IngredientParts by Welght Ethyl butyrateO05 Ethyl valerate.05 ~- Maltol ~.00 Cocoa extract26.00 Coffee extract10.00 ` Ethyl alcohol-20~00 Water 41~90 ~ ;
~ ' ' .
; , The above flavor is incorporated into model "filter"
cigarettes at the rate of 0O1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XIII at 100 ppm per cigarette~ Another third of ' these cigarettes are treated in the filter with the mixture o~ free and entrapped flavor produced according to Example XIII at the rate of 2 x 10 5 gm and 3 x 10 5 g~. When evaluated by paired comparison, the cigarettes treated both c in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent ~silica) are found, in smoking flavor to have a cherry flavor 3S and aroma nuance in the mainstream and in the sidestream on ~ smoking and, in addition, prior to smoking.

i, ' ' ' ~

, ~105~

:; .
EXAMPLE LVI
A tobacco blend is made up by mixing the following ` materials:
Inaredient Parts by Wei~ht .
; Bright 40.1 Burley 24.9 Maryland 1.1 Turkish 11.6 Stem (flue cured) 1402 Glycerine 2.8 Water 5~3 ~' .
The above tobacco is used in produced cigarettes and a formulation produced according to Example XIV incorporated into each of these c garettes.
. _ In~redient Parts by Weight Ethyl butyrate c05 Ethyl valerate .05 ( Maltol 2.00 Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 Water 41.90 ~ -, The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1~. One-third of these model 2~ cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XIV at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced accordin~ to Example XIV at the rate of 2 x 10 5 gm and 3 x 10 5 ~m. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent ~si}ica) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking~

.
~.; ' 7~
--106~

EXP,MPLE LVI I
~ A tobacco blend is made up by mixing the following ;~ materials:
IngredientParts by Weight Br ight 40 .1 Burley 24.9 Maryland 1.1 Turkish 11. 6 Stem ~flue cured)14.2 Glycerine 2.8 : Water 5O3 The above tobacco is used in produced cigarettes and a formulation produced according to Example XV incorporated into each of these cigarettes.
.~ .
15 IngredientParts by Weight -Ethyl butyrate .05 Ethyl valerate O05 Maltol 2.00 Cocoa extract 26.00 20 Coffee extract 10.00 Ethyl alcohol . ^2d. oo Water 41.90 The above flavor is incorporated into model "filter"
- cigarettes at the rate of 0~1%o One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XV at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XV at the rate of 2 x 10 5 ~m and 3 x 10 5 ~m. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a lime flavor and aroma nuance in the mainstream and in the sidestream on ~moking and, in addition, prior to smoking.

', ! . . .
, ., , 7~ ;
I -107- , .
EXAMPLE LVIII
.
A tobacco blend is made up by mixing the following materials Ingredient Parts by Weight Bright 40.1 Burley 24.9 Maryland l.l Turkish 11.6 ~( Stem (flue cured) 14.2 : 10 Glycerine 2.8 Water 5 3 ,` , , .
;; The above tobacco is used in produced cigarettes and a formulation produced according to Example XVI incorporated ; into each of these cigarettes. i .
' .
Ingredient Parts by Weight Ethyl butyrate .05 Ethyl valerate .05 t Maltol ~ 2.00 Cocoa extract 26.00 Coffee extract 10~00 Ethyl alcohol 20.00 Water 41.90 ~~:~~
~ . .
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model . 25 cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XVI at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter w~th the mixture of free ~nd entrapped flavor produced according to Example XVI at the rate of 2 x 10 gm and 3 x 10 5 ~m. When evaluated by paired comparison, the cigarettes treated both in the I q tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a peppermint flavor and aroma nuance in the mainstream and in the sidestream on smokin~ and, in addition, prior to smoking.

.

~ 7 93 !
1 0 ~ -, EXAMPLE LIX
A tobacco blend is made up by mlxing the following materials: ¦
In~edient Parts by Weight Bright 40.1 : Burley 24.9 Maryland 1.1 Turkish 11.6 Stem (flue cured) 14.2 Glycerine 2.8 Water 5.3 The above tobacco is used in produced cigarettes and a formulation produced according to Example XVII incorporated into each of these cigarettes.

Ingredient Parts by Weight j Ethyl butyrate .05 . Ethyl valerate .05 , Maltol ~.oo ; Cocoa extract 26.00 Coffee extract -10.00 Ethyl alcohol 20.00 ~ Water 41~90 ,.
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1~. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XVII at 100 ppm per cigaretteO Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XVII at the rate of 2 x 10 5 gm and 3 x 10 5 gm~ When evaluated by paired comparison, the cigarettes treated both : in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent - ! (silica) are ound, in smoking flavor to have a peppermint flavor and aroma n~ance in the mainstream and in ~h~ sidestream on smoking and, in addition, prior to smoking.

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EXAMPLE LX
A tobacco blend is made up by mixing the following materialss - ;
~ Inaredient Pa ts_by Weight Bright 40.1 Burley 24.9 ; !i Maryland 1.1 Turkish 11.6 ,~( i Stem ~flue cured) 14.2 ~lycerine 2.8 Water 5.3 .~ ,The above tobacco is used in produced cigarettes and a ; formulation produced according to Example XVIII incorporated into each of these cigarettesO

Ingredient Parts by Weight . _ Ethyl butyrate .05 ' Ethyl valerate .05 ;r , Maltol 2.00 ,~ Cocoa extract 26.00 Coffee extract 10.00 ",' Ethyl alcohol 20.00 ~ ater 41r 90 .
-~ I
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0~1~. One-third of these model cigarettes are treated in the tobacco section with the ' mixture of free flavor and entrapped flavor produced according to Example XVIII at 100 ppm per cigarette. Another third of these cigarettes are treated ,in the filter with the mixture of free and entrapped flavor produced according to Example ;~ 30 XVIII at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent ~silica) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on I smoking and, in addition~ prior to smoking.

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., EXAMPLE LXI
A tobacco blend is made up by mixing the following materials:
~ Parts b~ Weight ~ .
; Bright 40.1 - Burley 240 9 Maryland 1~1 j Turkish 11. 6 Stem (flue cured)14.2 Glycerine 2.8 Water 5~3 The above tobacco is used in produced cigarettes and a formulation produced according to Example XIX incorporated - into each of these cigarettes.

Ingredient Parts by Weight Ethyl butyrate .05 Ethyl valerate ~.05 ;~ Maltol 2~00 ; Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol -20~00 Water 41.90 .
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XIX at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XIX at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the ~e tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica~ are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, P~ior to smoking~

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EXAMPLE LXII
A tobacco blend is made up by mixing ~he following materialsO
~ IngredientParts by Weight :~ 5 B~ight 40.1 ; Burley 24~9 Maryland 1.1 Turkish 11.6 Stem ~flue cured)14.2 Glycerine 2.8 Water ~5.3 The above tobacco is used in produced cigarettes and a ~ formulation produced according to Example XX incorporated ; into each of these cigarettes.
~ ' . . '. ' IngredientParts by Weight Ethyl butyrate .05 Ethyl valerate .05 . Maltol 2.00 Cocoa extract 26.00 Coffee extract 10.00 ~thyl alcohol ~0.00 `
Water 41.90 The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1~. One-third of these model `~ ~
cigarettes are treated in the tobasco section with the s ,~ mixture of free flavor and entrapped flavor produced according ;~ to Example XX at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XX at the rate of 2 ~ 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in ~he , tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (silica) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking~

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E:XAMPLE LXIII
A tobacco blend is made up by mixing the following ~ materials:
In~redi~ent~Parts-by Weight Br;ight 4U~l : Burley 24.9 ~ Ma ryland 1.1 : Turkish 11.6 ( Stém (flue cùred) 14.2 Glycerine -2.8 Water ` 5~3 The above tobacco is ùsed in produced cigàrettes and a formulàtion produced according to Exampie XXI incorporated into each of these cigarettes.

in~redi~ent -~art-s-by-Wëight Ethyl butyrate .05 - -Ethyl valerate .0~5 ( Maltol . 2.00 Cocoa ëxtract 26.00 -20 Coffëe ëxtract -10.00 Ethyl alcohol -20.00 Water 4i.90 -.. .. . . . ... . . ..
: The àbove flavor is incorporated into model "filter"
cigarettes at the rate of 0.i~. One-third of these model 2S cigarettes are trëated in the tobacco section with the m^ixture of free flavor and entrapped flavor produced according to Example XXI at 100 ppm per cigarette~ Another third of these cigarettes are treated in the filter with the mixture .
of free and entrapped fLavor produced according to Example XXI at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent ~hydroxypropyl cellulose) are found, in smoking flavor to I have a lime flavor and aroma nuance in the mainstream and in the sldestream on smoking and, in addition, prior to smoking, . .

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EXAMPLE LXIV
A tobacco blend is made up by mixing the following materials-Parts by Weight S Bright - 40.l Burley 24~9 1 :
. Maryland 1.1 Turkish 11. 6 I Stem (flue cured~ 1~.2 10 Glycerine 2~8 Water 5.3 ~ he above tobacco is used in produced cigarettes and a formulation produced according to Example XX~I incorporated into each of these cigarettes. I

Ingredient Parts by Weight Ethyl butyrate .05 Ethyl valerate .05 ~ ¦
:¦ Maltol ~ 2.0 Cocoa extract 26.00 Coffee extract 10.00 : .Ethyl alcohol 20~00 Water 41.90 --~~-,, ` The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model 2~ cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according - to Example XXII at 100 ppm per cigaretteq Another third of these cigarettes are treated in the filter with the mixture.
: of free and entrapped flavor produced according to Example XXII at the rate of ~ x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and ree flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, pr~or to smoking.

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EXAMPLE LXV
A tobacco blend i5 made up by mixing the following materials:
Ingredient Parts bv W
Bright 40~1 Burley -24.9 ; Maryland l~l - ~urkish 11.6 Stem ~flue cured) 14.2 Glycerine 2.8 Water 5.3 The above tobacco is used in produced cigarettes and a formulation produced according to ~xample XXIII incorporated into each of these cigarettes.

Ingredient Parts by Weight Ethyl butyrate O05 ; Ethyl valerate O05 ( Maltol 2~00 Cocoa extract 26.Q0 2~ Coffee extract 10.00 Ethyl alcohol ` 20.00 ~ - Water 41.90 : ' ; -The above flavor is incorporated into model "filter"
`i cigarettes at the rate of 0.1~. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XXIII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped ~lavor produced according to Example 3~ XXIII at the rate of 2 x 10 5 gm and 3 x 10 5 ~m. When ; evaluated by paired comparison, the cigarettes treated both : in the tobacco and in the filter with the mixture o entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose~ are found, in smoking flavor to :~ 35 have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to ~; s~oking.
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EXAMPLE LXVI
: A tobacco blend is made up by mixing the following materials:
~ Parts by Weight Bright 40.1 Burley 29.9 Maryland 1.1 ;~ . Turkish 11~6 . Stem (flue cured) 14.2 Glycerine 2.8 ~ ~ater 5.3 ; The above tobacco is used in produced cigarettes and a .
formulation produced according to Example XXIV incorporated in~o each of these cigarettes.
~.
: 15 Ingredient Parts by Weight Ethyl butyrate .05 . Ethyl valerate .05 Maltol 2.00 : Cocoa extract 26.00 2~ - Coffee extract 10.00 - - Ethyl alcohol 20.00 Water 41.90 The above flavor is incorporated into ~odel "filter"
cigare~tes at the rate of 0.1~. One-third of these model cigarettes are treated in the tobacco section with the . mixture of free flavor and entrapped flavor produced according to Example XXIV at 100 ppm per cigarette~ Another third of -: these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example 3Q XXIV at the rate of 2 x 10 5 gm and 3 x 10 5 gm, When . evaluated by paired comparison, the cigarettes treated both ~ in the tobacco and in the filter with the mixture of entrapped : and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in additionl prior to smoking.

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~ '7~33 -~16-., EXAMPLE LXVII
. A tobacco blend is made up by mixing the following . materials In~redient ~ =
Bright 40.1 Burley 24.9 Maryland 1.1 ~urkish 11.6 Stem (flue cured~14~2 ~lycerine 2~8 Water 5~3 ; . ..
. The above tobacco is used in produced cigarettes and a ... formulation produced according to Example XXV incorporated . `~ into each of these cigarettes.

Ingredient Parts by Weight Ethyl butyrate O05 . Ethyl valerate O05 ' Maltol 2.00 .. ~
; Cocoa extract 26.00 ~ .
~ Coffee extract .10.00 Ethyl alcohol -20.00 :~ ~ater 41.90 ~!
:: .~
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model . ~5 cigarettes are treated in the tobacco section with the :` mixture o~ free flavor and entrapped flavor produced according . to Example XXV at 100 ppm per cigarette. Another third of ~ these cigarettes are treated in the filter with the mlxture : of free and entrapped flavor produced according to Example ~ XXV at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated .' by paired comparison, the cigarettes treated both in the ,~
. tobacco and in the filter with the mixture of entrapped and ~.
,..... .... ~ .
free flavor taken further together with suspension agent . (hydroxypropyl cellulose) are found, in smoking flavor to : ~5 have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to , ~mo~ing.
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. ~ 3 : -117- , . EX~MPLE LXVIII
_~_ A tobacco blend is made up by mixing the following materials:
: Ingredient Parts by Weight Bright 40.1 Burley ?4- 9 Maryland 1.1 Turkish 11.6 Stem (flue cured) 1402 ~ a~ Glycerine 20 8 ` Water 503 The above tobacco is used in produced cigarettes and a .
j : formulation produced according to Example XXVI incorporated ..
. ~ into each of these cigarettesO

: 15 Ingredlent Parts by Weight Ethyl butyrate 005 Ethyl valerate .05 : ~ Maltol 2.00 Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 Water 410 90 . . . ; .
: The above flavor is incorporated into model "filter'l : cigarettes at the rate of 0.1~. One-third of these model ~S cigarettes are treated in the tobacco section with the . mixture of free flavor and entrapped flavor produced according : to Example XXVI at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture .: of free and entrapped flavor produced according to Example . 10 XXVI at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both : in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent . thydroxypropyl cellulose) are found, in smoking flavor to . have a cherry flavor and aroma nuance in the mainstream and ln the sides~ream on smoking and, in addition, prior to smoking.

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, -118- .
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EX MPLE LXIX
; A tobacco blend is made up by mixing the following materials: ~

5 - Bright 40~1 !
Burley 24.9 : Maryland 1.1 ~ Turkish 11.6 :( Stem (flue cured)14~2 lycerine 2.8 Water 5.3 .
. The above tobacco is used in produced cigarettes and a : formulation produced according to ~xample XXVII incorporated : into each of these cigarettes.

In~edientParts by Weight Ethyl butyrate .05 . Ethyl valerate O05 Maltol 2.00 Cocoa extract 26.00 . 20 Coffee extract 10.00 Ethyl alcohol . 20~00 ` Water 41.90 The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1~. One-third of th2se model cigarettes are treated in the tobacco section with the .
: mixture of free flavor and entrapped flavor produced according to Example XXVII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to ExampIe XXVII at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both .
in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to ~moking.

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$~3~33 EX LXX
A to~acco blend is made up by mixing the following materials: -In~redient S Bright 40.1 Burley 24~9 Maryland 1.1 Turkish 11.6 Stem (flue cured314~2 1~ Glycerine 20 8 Water 5~3 The above tobacco is used in produced cigarettes and a formulation produced according to Example XXVIII incorporated into each of these cigarettes.

IngredientParts by Weight Ethyl butyrate ,05 Ethyl valerate .05 ( Maltol . 2.00 Cocoa extract 26.00 Coffee extract10,00 Ethyl alcohol 20.00 . i . . .
~, Water 41.90 ., .
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the `~ mixture of free flavor and entrapped flavor produced according to Example XXVIII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XXVIII at the rate of 2 x 10 5 gm and 3 x 10 5 gm.
When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of -entrapped and free flavor-taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream , and in the sidestrearn on smoking and~ in addition, prior to moking.

7~33 -120- ;
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EXAMPLE LXXI
A tobacco blend is made up by mixing the following materials: i Ingredient P _ b ~ i ~ . , Bright 40.1 Burley 24.~ ¦
Maryland 1~1 Turkish 11.6 Stem (flue cured) 14.2 Glycerine 2.8 ~ Water 5,3 :;~ ' . .
The above tobacco is used in produced cigarettes and a formulation produced according to Example XXIX incorporated into each of these cigarettes.
~,, . .
Ingredient Parts~y Weight -Ethyl butyrate O05 Ethyl valerate 05 Maltol 20 00 Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 ~` ~ater 41.90 :: . .
The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture o free flavor and entrapped flavor produced according to Example XXIX at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XXIX at the rate of ~ x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both - in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstre~m and t in the sidestream on smoking and, in addition, prior to smoking.

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: -121~ `
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- EXAMPLE LX
A tobacco blend is made up by mixing the following . ~aterials r : In~redienti Parts by Weight ~ ~right 40.1 : Burley 24.9 Maryland 1.1 Turkish 11~6 Stem (flue cured) 14.2 Glycerine 2.8 - Water 5.3 .
The above tobacco is used in produced cigarettes and a formulation produced according to Example XXX incorporated into each of these cigarettesO
... . ..
. ~5 Ingredlent Parts by Welght . Ethyl butyrate .o~
Ethyl valerate .05 Maltol 2~00 Cocoa extract 26.00 Coffee extract lO.OO
Ethyl alcohol 20000 Water 410 90 . .
, ~ he above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XXX at 100 ppm per cigarette. Another third of . these cigarettes are treated in the filter with the mixture . of free and entrapped flavor produced according to Example . ~ XXX at the rate of 2 x lO 5 gm and 3 x lO 5 gm. When evaluated .~ by paired comparison, the cigarettes treated both in the . q : tobacco and in thb filtier with the mixt~re of entrapped and free flavor taken further together with suspension agent ~hydroxypropyl cellulose) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and . in the sidestiream on smokin~ and, in addition, prior to ~moking.

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-~ l . ~ 7 -122-. 1 ~' rY~ XYI 11 , A tobacco blend is made up by mixing the following materials:
Parts ~y Wei~ht ~, ~ Bright - ` 40.I `
. Burley 24.9 Maryland 1~1 ; Turkish 11.6 - ~ Stem (flue cured)14,2 Glycerine 2.8 : Water 5.3 .
The above tobacco is used in produced cigarettes and a formulation produced according to Example X~XI incorporated .' ~ into each of these cigarettes.

a5 Ingredient P_ t3 b~ 9 ;` Ethyl butyrate .05 Ethyl valerate O05 l ( Maltol 2.00 5 7 ~ Cocoa extract 26.00 .~; 20 Coffee extractlOo 00 ~,` Ethyl alcohol^20.00 Water 41.90 ;~
- -he above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%~ One-third of these model . 25 cigarettes are treated in the tobacco section with the .~ mixture of free flavor and entrapped flavor produced according . to Example XXXI at 100 ppm per cigarette~ Another third of these cigarettes are treated in the filter with the mixture o free and entrapped flavor produced according to Example 3~ XXXI at the rate of 2 x 10 5 gm and 3 x 10 5 gm, When , evaluated by paired comparison, the cigarettes treated both '~
I in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent , (hydroxypropyl cellulose) are found, in smoking flavor to ! have a lemon flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to j smoking.
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EXAMPLE LXXIV
A tobacco ~lend is made up by mixing the following materials:
IngredientParts by Welght Bright 40Ol . Burley 24.9 : Maryland 1.1 Turkish 11.6 : ~ . Stem [flue cured)14.2 . S0 ~lycerine 2.8 Water 5.3 ~' ; The above tobacco is used in produced cigarettes and a ~l formulation produced according to Example XXXII incorporated : into each of these cigarettes.

. lS Ingredientarts by Weight Ethyl butyrate .05 . Ethyl valerate O0~
~ ~ . Maltol 2 00 Cocoa extract 26.00 n Coffee extract 10.00 . Ethyl alcohol 20.00 i Water 41.90 . The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes a~e treated in the tobacco section with the . mixture of free flavor and entrapped flavor produced according to Example XXXII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture . ~-f free and entrapped flavor produced according to Example . 30 XXXII at the rate of 2 x 10 5 gm and 3 x 10 5 gm When evaluated by paired comparison, the cigarettes treated both . in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.
, ., ~ O ' ~ 3~ ~ 3 EXAMPLE LXXV
A tobacco blend is made up by mixing the following materials:
Ingredient Parts by Wei~t ; 5 Bright 40~1 , Burley 24~9 Maryland 1~1 Turkish llo 6 ;~ Stem (flue cured) 14.2 ~ 10 ' Glycerine 2.8 ,~ Water 5~3 The above tobacco is used in produced cigarettes and a `, formulation produced according to Example XXXIII incorporated into each of these cigarettes.

Ingredient Parts by Weight ,, ;
Ethyl butyrate ,05 Ethyl valerate L 05 '~ Maltol 2.00 Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 ~ater - 41.9 . ~ . A
. . . ~ :
i'~ The above flavor is incorporated into modeI "filter"
cigarettes at the rate of 0.1~. One-third of these model cigarettes are treated in the tobacco section with the mîxture o~ ree flavor and entrapped flavor produced according to ~xample XXXIII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to ~ Example XXXIII at the rate of 2 x 10 5 gm and 3 x 10 5 gm.
When eval~ated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent ~hydroxypropyl cellulose) are found9 in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on smoking and~ in addition, prior to ~moking.
' ' ~; -7~3 ~ 125-- 1 .
EXAMPLE LXXVI
~ A tobacco blend is made up by mixing the following ; materials:
ln~redient P~rts by Weight Bright 40.1 ~urley 24.9 MaryIand 1.1 i Turkish 11.6 em (flue cured) 14~2 .
Glycerine 2.8 , .
` Water 5.3 The àbove tobacco is used in produced cigarettes and a ; formulation produced according to Example XXXIV incorporated ; into each of these cigarettes.
,, lS ~ Pà-r-t-s-byTWelght - Ethyl butyrate .05 Et~yl valerate .05 Maltol 2.00 i _ r .
: Cocoa extract 26.00 Coffee extract 10,00 Ethyl alcohol 20.00 . Wàter ~1~90 ~~~~~
, Thé abovè flavor is incorporated into model "filter"
cigarettes at the rate of 0Ol~ One-third of these model cigarettes are treated in the tobacco section with the I mixture of free flavor and entrapped flavor prcduced according to Example XXXIV at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free a~nd entrapped flavor produced according to Example 3~ XXXIV at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigare~tes treated both in the tobacco and in the f ilter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a lemon flavor and aroma nuance in the mainstream and in the sidestream on ~moking and, in addition, prior to smoking.

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EXAMPLE LXXVII
A tobacco blend is made up by mixing the Eollowing materials: !
~ Parts by Weight S Bright 40.1 ; Burley 24.9 Maryland 1.1 Turkish 1106 Stem (fl~e cured) 14O2 Glycerine 2.8 Water 5~3 .
` The above tobacco is used in produced cigarettes and a formulation produced according to Example XXXV incorporated ` I into each of these cigarettes.

Ingredient Parts b~ Weight Ethyl butyrate O05 Ethyl valerate ~05 Maltol 2.00 , Cocoa extract 2~.00 Coffee extract 10.00 Ethyl alcohol 20.00 Water 41.90 -~
- .
~he above flavor is incorporated into model "filter" ~i cigarettes at the rate of 0.1~. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XXXV at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XXXV at the rate o~ 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both q in the tobacco and in the filter with the mixture o entrapped and free flavor taken further together with suspension agent ~hydroxypropyl cellulose) are found, in smoking flavor to have a lime 1avor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.

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, o l ~7~_ 1 EXAMPLE LXXVIII
A tobacco blend i5 made up by mixing the following ' materials:
- Ingredl nt Parts by Wei~ht . , . I
:~ 5 Bright 40Ol .. ~ Burley ~.9 Maryland 1.1 :~ Turkish 11.6 .( Stem (flue cured) 14.2 Glycerine 2.8 .~ Water 5O3 .
The above tobacco is used in produced cigarettes and a -~
~: formulation produced according to Example XXXVI incorporated ~ into each of these cigarettes.

A'" 15 Ingredient Parts by Weight ~, ~
~-: Ethyl butyrate .05 .
Ethyl valerate .05 . Maltol 2~00 Cocoa extract 26~00 . ~ j . 20 Coffee extract 10.00 ~¦
'~1'! Ethyl alcohol 20~00 ~ Water 41.90 ..
: The above flavor is incorporated into model "filter" r cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the ~.
~; mixt~re of free flavor and entrapped flavor produced according to Example XXXVI at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture .
of ree and entrapped flavor produced according to Example . 30 XXXVI at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both ~.
in the tobacco and in the filter with the mixture of entrapped : and free flavor taken further together with suspension agent ~hydroxypropyl cellulose) are found~ in smoking flavor to have a lime flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.

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, -128- j .
EXAMPLE LXXIX
A tobacco blend is made up by mixing the ollowing materials:
Ingredient ~a-t- b~ 39h5 Bri~ht - 40.1 Burley 24.9 Maryland 1~1 i ~urkish 11.6 Stem (flue cured) 14.2 Glycerine 2.8 ~ater 5.3 The above tobacco is used in produced cigarettes and a formulation produced according to Example XXXVII incorporated into each of these cigarettes.
, Ingredient Parts by Weight Ethyl butyrate .05 Ethyl valerate .05 Maltol 2.00 Cocoa extract 26.00 ~ Coffee extract lOo 00 Ethyl alcohol 20.00 Water 41.90 -~

The above flavor is incorporated into model "filter"
cigarettes at the rate of 0~1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XXXVII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free-and entrapped flavor produced.according to Example XXXVII at the rate of 2 x 10 5 gm and 3 x 10 5 gm.
When evaluated by paired comparison, the cigarettes treated ; ~-- both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a lime flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to ~moking.

. -123 EXAMPL~ LXXV
A tobacco blend is made up by mixing the ollowing ; materials:
~ Parts by Weight Bright 40n 1 : Burley . 24~9 Maryland lol ' Turkish 11.6 `~ Stem.(flue cured)14.2 10 Glycerine 2.8 Water 5~3 The above tobacco is used in produced cigarettes and a " formulation produced according to Example XXXVII~
. incorporated into each of these cigarettes. ~ .
.
lS IngredientParts by Weight Ethyl butyrate .05 Ethyl valerate .05 ( Maltol 2.00 Cocoa extract 26~00 Coffee extract 10.00 .Ethyl alcohol 20.00 , ~; . Water 41.90 -, ; .
The above flavor is incorporated into model "filter" ~ :
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XXXVIII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example XXXVIII at the rate of 2 x 10 5 gm and 3 x 10 5 gm.
i When evaluated by paired comparison, the cigarettes treated 't both in the tobacco and in the filter with the mixture of ~ entrapped and free flavor taken further to9ether with suspension ¦ agent thydroxypropyl cellulose) are found, in smoking flavor I 35 to have a lime flavor and aroma nuance in the mainstream and ¦ ln the sidestream on smoking and, in addition, prior to j smoking.
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dJ ~ 3 i --131)- -`:;
:
EXAMPLE LXXXI
. A tobacco blend is made up by mixing the following : materials: :
. ' Ingredient Parts b~ Wel~ht . Bright 40.1 - i -Burley 24.9 Maryland 1.1 Turkish 11.6 ~' Stem ~1ue cured) 14.2 Glycerine 2.8 : . Water 5,3 ~ The above tobacco is used in produced cigarettes and a -~ formulation produced according to Example XXXIX incorporated . .
into each of these cigarettes.
.~ ...
In~redient Parts by Welght Ethyl butyrate .05 Ethyl valerate .05 ( Maltol 2.00 Cocoa extract 26.00 Cofee extract 10~00 ~ .Ethyl alcohol 20~00 : Water 41D 90 , The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1~. One third of these model cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XXXIX at 100 ppm per cigarette. Another third of ~hese cigarettes are treated in the filter with the mixture ; of free and entrapped flavor produced according to Example XXXIX at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When `~ evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a lime flavor and aroma nuance in the mainstream and in the aidestream on smoking and, in addition, prior to smoking.

, .
~: , ,;

7~3 i 13~
.
EXAMPLE LXXXII
A tobacco blend is made up by mixing the following materials:

Bright 40.1 Burley ~4O9 Maryland 1.1 Turkish 11.6 Stem (flue cured) 14.2 Glycerine 2.
Water 5~3 The above tobacco is used in produced cigaret~es and a formulation produced according to Example XL incorporated ~` into each of these cigarettes.

~ I r _ Ethyl butyrate.05 Ethyl valerateO05 ~i Maltol 2.00 Cocoa extract26.00 ; 20 Coffee extract10.00 , Ethyl alcohol20~00 ~ater - 41.90 The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1~. One-third of these model ~5 cigarettes are treated in the tobacco section with the mixture of free flavor and entrapped flavor produced according to Example XI, at 100 ppm per cigarette. Another third of these cigarettes are treated in the ilter with the mixture of free and entrapped flavor produced according to Example 3~ XL at the rate of 2 x 10 5 gm and 3 x 10 5 g~. When evaluated ; by paired comparison, the cigarettes treated both in the tobacco and in the ~ilter with the mixture of entrapped and free flavor ~aken further together with suspension agent (hydroxypropyl cell~lose) are found, in smoking flavor to 3S have A lime flavor and aroma nuance in the mainstream and in th~- sidestream on smoking and, in additio~, prior to smoking.

, -l32U_ :
: T EXAMPLE LXXXIII
i A tobacco ~lend is made up by mixing the following material5: i ~ P ts by Wei~ht S Bright 40.1 .
Burley 24.9 .I Maryland 1.1 Turkish 11.6 Stem (flue cured)1402 ¦~ ~ Glycerine 2a 8 . Water 503 The above tobacco is used in produced cigarettes and a . formulation produced according to Example XLI incorporated ~ into each of these cigarettes.
.` ' , IngredientParts by Weight i Ethyl butyrate.05 ; Ethyl valerate.05 Maltol 2.00 ~ . Cocoa extract26.00 ~, : 20 Cofee extract. 10.00 Ethyl alcohol20.0 Water 41.90 .
~ ' , , .
- The above flavor is incorporated into model "filter"
; cigarett~s at the rate of 0.1~. One third of these model cigarettes are treated in the tobacco section with the ..
mixture of free flavor and entrapped flavor produced according to Example XLI at 100 ppm per cigarette. Another third of ;` these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example 3~ XLI at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated;
by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and . free flavor taken further together with suspension agent ; ~hydroxypropyl cellulose) are found, in smoking flavor to ~S have a cherry flavor and aroma nuance in the mainstr~am and ~n the sidestream on smo~ing and, in addition~ prior to smoking.

, , 7~
--13~---EXAMPLE LXXXIV
A tobacco blend is made up by mixing the following ma~erials:
Xn~redient Par~s by Wei~t Bright 40.1 Burley ~4.9 ~aryland 1.1 Turkish 11.6 f Stem ~flue cured)14.2 ; 10 Glycerine 2~8 Water 5.3 The above tobacco is used in produced cigarettes and a formulation produced according to Example XLII incorporated `~ into each of these cigarettes.

~ Parts by Weight Ethyl butyrate .05 ~thyl valerate .05 ( Maltol 2.00 Cocoa extract 26.00 Coffee extract 10.00 Ethyl alcohol 20.00 Water 41.90 The above flavor is incorporated into model "filter"
cigarettes at the rate of 0.1%. One-third of these model cigarettes are treated in the tobacco section wi~h the mixture of free flavor and entrapped flavor produced according to Example XLII at 100 ppm per cigarette. Another third of these cigarettes are treated in the filter with the mixture of free and entrapped flavor produced according to Example 3Q XLII at the rate of 2 x 10 5 gm and 3 x 10 5 gm. When evaluated by paired comparison, the cigarettes treated both in the tobacco and in the filter with the mixture of entrapped and free flavor taken further together with suspension agent (hydroxypropyl cellulose) are found, in smoking flavor to have a cherry flavor and aroma nuance in the mainstream and in the sidestream on smoking and, in addition, prior to smoking.

li !

9. 7~
-1 3 ~ - `

EXAMPLE LXXXV
-- - - ..- _ V.6 ml of an aqueous emulsion containing 37.5 mg per liter of the mixture of free flavor and entrapped 1avor S with suspension agent produced according to Example II
; are added to the contents of an infusion of tea of approx- ¦
imately 10 liters prepared by the decoction of 250 g of tea leaves followed by vigorous stirring. The tea has a solid content of 3 9 per liter which means that it con-tains 0.75 ppm of aromatizing substance. The tea thus treated is then submitted to a jury of tasters and amateurs who~ after blindfolding, have to indicate their preference between the aroma*ized tea and a non-aromatized reference tea of the same kind. 8 tasters out of 8 preferred the lS aromatized tea describing it as generally lemon-like.
By way of comparison, similar aromatization in the quantity of O.S ppm produced the tea which is preferred by 4 tasters out of 5 and which was described as having a lemony note while aromatization in a quantity of 3.5 ppm in the unan-imous opinion of the tasters gave the tea a strong aroma hut still pleasant note~

, EXAMPLE LXXXVI `~
0.6 ml of an aqueous emulsion containing 37.5 mg - per liter of the mixture of free flavor and entrapped flavor with suspension agent produced IV to Example II
are added to the contents of an infusion of tea of approximately 10 liters prepared by the decoction of 250 g of tea leaves followed by vigorous stirring. The tea has a solid content of 3 g per liter which means that it contains 0.75 ppm of aromatizing substance.
The tea thus treated is then submitted to a jury of tasters and amateurs who, after blindfolding, have to indicate their preference between the aromatized tea -and a non-aromatized reference tea of the-same kind. 8 tasters out of 8 preferred the aromatized tea describing .
.
~, .
.

7~ 3 ~13~-it as generally peppermint-likeO By way of comparison, similar aromatization in a quantity of 0.5 ppm produced the tea which is preferred by 4 tasters out of 5 and which I was described as having a peppermint note while aromatiza~
tion in a quantity of 3O5 ppm in the unanimous opinion of the tasters gave the tea a strong peppermint aroma but still pleasant note.
EXAMPLE LXXXVII
The following mixture is prepared:

0 Ingredient Parts by Weight . ~
Liquid Flavor Composition~.. O...... ~.. O~.O.48.4 of Example B
I KLUCEL~ HF (Brand of hydroxypropyl.. ~ O.... 6.4 i cellulose manufactured by Hercules l 15 Corporation of Wilmington, Delaware t having a molecular weight of 800,000 -l and viscosity properties as defined 1 according to Figure 2 (see note l) ~, .
The KL~CEL~ HF is dispersed in the liquid flavor ~ 2Q composition of Example A with vigorous stirring thereby ¦ resulting in a viscous liquid. 48.4 Parts by weight of il the powder flavor composition of Example D is then 1 blended into said viscous liquid with stirring at 25C
¦ for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.
NOTE l RLUCEL~ is a brand of hydroxypropyl cellulose manufactured by the Rercules Corporation of Wilmington, Delaware having the structure:

OCH CHCH, OH
: CH, ~1 OCH,C11CH, .. ~ ~
H OCH,CH HI C~
: OHOCH~ f HCH, C~cH~ciHcH~
S~
3S having a particle size such that 95% of the particles are passed through 30 mesh screens and 99% of the material is passed through 20 mesh screens.

~, .

3~- 1 .
!
EXAMPLE LXXXVI I I
0.6 ml of an aqueous emulsion containing 37.5 mg per liter of the mixture of free flavor and entrapped flavor with suspension agent prod~ced according to Example LXXXVII are added to the contents of an infusion -` of tea of approximately 10 liters prepared by the decoction of 250 9 of tea leaves followed by vigorous stirring. The tea has a solid conten~ of 3 g per liter which means that it contains 0.7~ ppm of aromatizing substance. The tea thus treated is then submitted to a jury of tasters and amateurs who, after blindfolding, have to indicate their preference between the aromatized tea and a non-aromatized reference tea of the same kindO 8 tasters out of 8 preferred the aromatized tea lS describing it as generally lemon-like. By way of comparison, similar aromatization in the quantity of 0.5 ppm produced the tea which is preferred by 4 tasters out of 5 and which was described as having a lemony ;~ note while aromatization in a quantity of 3.5 ppm in the unanimous opinion of the tasters gave ~he tea a strong a~oma but still pleasant note.

~, . . .

. .

, , '~ l 137~

.1 EXAMPLE LXXXIX

The following mixture is prepared:

Ingredient ~ ___ __ _Parts by Weight . ~ . . _ _ .
~ Liquid 1avor composition of o~ o48~4 Example XA
; KLUCEL~ JF (brand of foodgrade....... O.. O 3~2 hydroxypropyl cellulose by Hercules Corporation of Wilmington, Delaware having a molecular weight of 120,000 and viscosity properties defined according to Figu_e 2) _ .
The KL~CEL~ JF is dispersed in the liquid flavor compo-sition of Example XA with vigorous stirring thereby result-ing in a viscous liq~lid. 48.4 Parts by weight of a powder flavor composition prepared as follows~

20 Grams of the flavor composition produced accord ing to Example XA is emulsified in a solution ( containing 300 grams of gum acacia and 700 grams of water. The emulsion is spray-dried with a Bowen Lab Model Dryer utilizing 260 cfm of air ! ' with an inlet temperature o 500F an outlet temperature of 200F ,and a wheel speed of 50,000 rpm, is then blended into said viscous li~uid with stirring Z5 at ~5C for a period of 30 minutes resulting in a dry, free-flowing sustained release flavor powder having an excellent coffee flavor.

~ -13~3- 1 ~ , The resulting flavor powder i5 then added at the rate of 2~ to Nescafe~ brand o~ instan~ coffee manufactured by the Nestle Corpora~ion of Basle, Switzerland. The result-lng mix~ure is then added to boiling water at the rate , of one teaspoon per standard cup of water~ The resulting coffee flavor beverage is allowed to oool to 70F. The resulting coffee has an excelle~t long lasting aroma of constant strength and an excellent long lasting taste of ^~ ! constant strength over a period of 15 minutes.

~ EXAMPLE XC
~, The following mixture is prepared: ¦

Ingredient Parts by Weight Peppermint Oil~ o47~25 Propylene glycol......................... 0.50 ¦ KLUCEL~ JF(brand of hydroxypropyl....~.. 5.00 cellulose manufactured by the ¦ Hercules Corporation of Wi]nington~ I
Delaware having a molecular welght of about 120,000 and a viscosity defined I according to Figure 2.) ¦ ;

; The KLUCEL~ JF is dispersed in the peppermint oil wi~h vigorous stirring, thereby resulting in a viscous ~; liquid. 47.25 Parts by weight of the powder flavor com-position of Example K is then blended into the said visco~s ~;; liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

,, , I
. !

1, '~ 7 ~139-:

EXAMPLE XCI

The following mixture is prepared:

Ingredient _ _ ~arts by Weight Peppermint oil.. O......... O.......... O... 20 Propylene glycolO... ,....... ~ ........... 1.00 KLUCEL~ GF(brand of hydroxypropyl........ 9 0O
cellulose manufactured by Hercules Corp. of Wilmington, Delaware having a ~olecular weight of about 300,000 and a viscosity defined according to Fiqure 2.~
. . _ . . _ - . ._. . __ The KLUCEL~ GF is dispersed in the peppermint oil with vigorous stirring, thereby resulting in a viscous liquid. 71 Parts by weight of the powder Elavor composition of Example L is then blended into the said viscous liquid, with stirring at 25C for a period of 3Q minutes resulting in a dry, free flowing sustained release flavor powder.
. .
EXAMPLE XCII
. . . ' .... ..
The following mixture is prepared:

Ingredient Parts by Weight Liquid flavor composition of...... O..... O.. 20 Example B
Propylene glycol... ,.. ,....... O.,... ,... ,.. 1.00 KLVCEL~ MF~brand of hydroxypropyl.......... 9.00 cellulose produced by the Hercules Corp~ of Wilmington, Delaware having a molecular weight of about 700,000 and a vlscosity defined according to 11 . 1 ' . . . .
.' .~

-~40-The KLUCEL ~ is dispersed in the liquid flavor composition of Example B with vigorous stirring, ~hexeby resulting in a viscous liquid. 65 Parts by weight o~
the powder flavor composition of Example E is then blended into the said viscous liquid, with stirring at 25C for-a period of 30 minutes resulting in a dry, free flowing sustained release flavor powder.
., ..
EXAMPLE XCIII
. ' , ~ ,~
; The following mixture is prepared:
, . . .. ... . , ._ , Ingredient Parts by Weight .~ . _ ~ ~ ~
Liquid flavor composition of..... O.... ~.O.48.4 Example C
Ethyl Cellulose.................. OO.. 3.2 KLUCEL~ type HF (brand of hydroxy~ O~ 2.0 propyl cellulose manufactured by the Hercules Corporation of Wilmington, Delware having a molecular weight of about 800,000 and a vlscosity defined according to Figure 2) _ _ _ _ __ i:
The ethyl cellulose and hydroxypropyl cellulose are intimately admixed. The intimate admixture o~ ethyl cel-lulose a~nd hydroxypropyl cellulose is dispersed in the - liquid flavor composition of Example C with vigorous stir-ring thereby resulting in a viscous liquid~. 48.4 Parts - by weight of the powder flavor compos~tion of Example F
.! iS then blended into the said viscous liquid, with stir-ring at 25C for a period of 30 minutes resulting in a thixotrop sustai~d rele-se flavo peste.

I
.' .

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-~

EXAMPLE XCIV

The following Mixture is prepared: .

~ In~redient Parts by Weight .~ Oil of wintergreen... O... ~ ........ O.~D.O47~25 Propylene glycol.................. ...... O. 0.50 KLUCEL~ HF (brand of hydroxy- .............. ~. 5.00 propyl cellulose produced by the ~ercules Corporation of Wilmington Delaware having a molecular weight of about 800,000 and a viscosity .~ defined according to Figure 2) . ~

The KLUCEL~ HF i5 dispersed in the oil of wintergreen ; with vigorous stirring, thereby resulting in a viscous liquid. 47.25 Parts by weight of the powder flavor com-position of Example M is then blended into the said vis-cous liquid, with stirring at 25C for a period of 30 min-~ utes resulting in a thixotropic sustained release flavor '~ paste. . . ~
~ .'. ~ .
. . EXAMPLE XC`V
, , . . . '. ....... ..
The following mixture is prepared:.
. ...
. Ingredient Parts bv Weight . ...~
: Liquid flavor composltion of~...... ~.. ~..... 26 . Example A ~
: . Propylene glycol........ ~..... ~.. ~.. ~..... .1 KLUCEL HF ~brand of hydroxy~ ~O~ 9 .~ propyl cellulose produced by the . Hercules Corporation of Wilmington, .: , Delaware having a molecular weight .~ of about 800,000 and a viscosity ------~ 30 defined accordinq to Figure 2) .' .
.~
., . ~ .
.

'7~ ~
-1~2-The KL~CEL is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 65 Parts by weight of .
the powdered flavor composition of Example N i.s then blended into the said viscous liquid, with stirring at 2SC for a period of 30 minutes resulting in a dry, free flowing sust~ined release flavor powder.
..
EX~MPLE XCVI

The following mixture is prepared:
.' . ' ~
Ingredient _ Parts by Weight . Liquid flavor composition of............... 48.4 : , Example B
Propylene glycol..... /............... O............................ .2 KLUCEL HF (brand of hydroxy~ O~ 3.4 : propyl cellulose produced by the . - Hercules Corporation of ~ilmington, Delaware having a molecular weight ` of about 800,000 and a v:iscosity defined_according to Figure 2) The KI.UCEL~ HF is dispersed in the liquid flavor com-position of Example B with vigorous stirring, thereby re- -. sulting in a viscous liquid. 48.4 Parts by weight of the . powder flavor composition of Example O is then blended .
into the said viscous liquid9 with stirriny at 25C for a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

30 ~
,, ' ', l .

-~ ~ 3 -143~
.~
EXAMPLE_XCVII

The ollowing mixture is prepared:

Ingredient Parts by Welght Liquid flavor composition of~.O.OO~oo.-..4~-4 Example C
Propylene Glycol...~.O.~. L ~ ~ ~ O ~ O O O D ~ ~ 0 5 Ethyl CelluloseO.... O... ~.......... O...... ..4.1 KLUCE~ type MF (brand of hydroxy- ....... ~. 0.S
propyl cellulose produced by the ~ Herc~les Corporation of Wilmington, Delaware havins a molecular weight of about 700,000 and a viscosity defined . accordinq to Figure 2) ~' .. ~ .

An intimate admixture is made of the ethyl cellulose and hydroxypropyl cellulose. The mixture of ethyl cellu-lose and hydroxypropyl cellulose is dispersed in the liquid flavor composition of Example C with vigorous stirring thereby resul~ing in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example P is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropic s~stained release flavor paste.

E~r~PL~ XCVIII ~~
`; " . ' ' . , The following mixture is prepared:
;.: _ Ingredient Parts by Weight .- . , _ ........... . ~, .. .,_ .
Orange oil..... O.. ~,......... O.......... 48.4 RLUCEL~ GF (brand of hydroxy- ..... ~..................... ~ 3.2 propyl cellulose produced by the ~` 30 Hercules Corporation of Wilmington, - Delaware having a molecular weight of about 300,000 and a viscosity defined a~cordina to Fiqure 2) i' ~. ' . . I

.
.

--The KL~CEL GF is dispersed in the orange oil with vigorous stirring, thereby resulting in a viscous liquid.
48 . 4 Parts by weight of the powder f lavox composition of Example Q is then blended into the said viscous liquid, with stirring at 25C ~or a period of 30 minutes resulting in a thixotropic sustained release flavor paste.

EXAMPLE XCIX
,. .

The following mixture is prepared:
., , .
Ingredient_ Parts by Weight ...._ ..
Liquid flavor composition of.... ~.O. no~ 20 Example A
Propylene glycol... ~............ ~..... O.~........ 2 , RLUCEL~ GF (brand of hydroxy-........ ~..... 4.2 propyl cellulose produced by the Hercules Corporation of Wilmington, Delaware having a molecular weight of about 300,000 and a viscosity defined according to Figure 2) Ethyl cellulose.... O....................... O..... 1.0 ':: .' ~ '''' ' ~' ' ' ........................... ~ .
~ The KLUCEL~ GF and ethyl cellulose is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 70 Parts by weight of the powder flavor composition of Example R
- ~ is then blended into the said viscous li~uid, with stir-ring at 25C for a period of 30 minut~s resulting i~ a dry, fre lowing sustalned ~elease flavor powder.

' . . ~

.

; ~ 793 The KLUCEL GF and ethyl cellulose is disp~rsed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 70 Parts by weight of the powder flavor composition of Example R is then blended into said viscous liquid, with stirring at 25C ~or a period of 30 minutes resulting in a dry, free flowing sustained release flavor powder.
.~
EX~MPLE C (100) ..... ,:.. ,.,,.. ~; . -. The following mixture is prepared-. .. . ... .. _. . ..... . .. :.. .
Ingredient Parts by Weight Liauid flavor composition of....... .~....... O20 Example A
Propylene glycol............... ~... cO... O.... ..1 KLUCEL GF tbrand of hydroxy- ...... ..... ~.... ..3 propyl cellulose produced by the - Hercules Corporation of Wilmington, Delaware having a molecular weight of about 300,000 and a viscosity Ethyl cellulose........... ~............ ~..... ..3 The KLUCEL~ GF and ethyl cellulose are dispersed in the liquid flavor composition of Example A with vigorous J : stirring, thereby resulting in a viscous liquid. 65 Parts .
by weight of the powder flavor composition of Example R
is then blended into the said viscous liquid with stirring at 25C for a period o 30 minutes resulting in a dry, free flowing sustained release flavor powder.
~ , . .

,~
,, ~ , :
! .

~1~6-EXAMPLE CI

The following mixture is prepared:

Ingredient _ _ Parts by Weight _ . ~ .
Liquid flavor composition of......... .,.O.. 48.4 Example B
Propylene glycol... O........ O........ -.O~.. .2 RLUCEL~ GF (brand of hydroxy-.~...... O0. 3.2 . propyl cellulose produced by the :~ Hercules Corporation of Wilmington, Delaware having a molecular weight of about 300,000 and a viscosity . defined according to Figure 2) ~yl cellulose.............. ......... ~ 1.5 _ ~ - The KLUCEL~ GF and ethyl cellulose is dispersed in .~ the liquid flavor composition of Example B with vigorous stirring, thereby resulting in a viscous liquid. 48.4 :~ ~Parts by weight of the powder flavor composition of Example :; ~ S is then blended into the said viscous liquid, with stir-~: ring at 25C for a period of 30 minutes resulting in a ; 20 thixotropic sustained release flavor paste.
~ -. . ...................... . ., . .. . ........... ~ .. ,, .
. - ' . .
. E~PLE CI~ - . .
~ ~ . ~ ' .
The following mixture is prepared: ~ .
,: -----~
Ingredient _ _- Parts by Weight Liquid flavor composition of.... ~.... ~..... l8 .
. Example C
:: Propylen glycol............................ .1 .
KLUCLL~ GF (brand of hydroxy~ O~ 3 , . propyl cellulose produced by the Hercules Corporation of Wilmington, .
Delaware having a molecular weight of about 300,000 and a viscosity . defined accordin~ to Figure 2) ~147-The KLUCEL R GF and ethyl cellulose is dispersed in the liquid flavor composition of Example C with vigorous stirring, thereby resulting in a viscous liquid. 62 Parts by weight of the powder flavor composition o~ Example ~
is ~hen blended into the said viscous liquid, with stir-ring at 25C for a period of 30 minutes resulting in a dry, free flowing sustained release ~lavor powderc EX~MPLE CIII
,, ,,,~,, ,~, ~ .... .. ~
The following mixture is prepared:

Ingredient Parts by Weisht _._ Peppermint oil.......................... 48.4 Propylene glycol.... ~............ O.. O... .2 KLUCEL GF ~brand of hydroxy ............ .3.8 propyl cellulose produced by ~he ~ Hercules Corporation of Wilmington, ; Delaware having a molecular weight of about 300,000 and a viscosity defined according to Figure 2) The KLUC~L GF is dispersed in the peppermint oil with vigorous stirring, thereby resulting in a v~scous liquid. 48.4 Parts by weight of the powder flavor comp-osition in Example U is then blended-into the said viscous ;~ liquid, with stirring at 25C for a period of 30 minutes ~ resulting in a thixotropic ~ustained ~elease flavor paste.
'~,'' ~
EXAMPLE CIV
, =.. . __ The following mixture is prepared:

Ingredient Parts b Weight ~ Y _ Peppermint oil.................. ,..... ~.. 21 1 Propylene glycol...................... ... .1.0 KLUCEL~ GF (brand of hydroxy- ........ ... .2.0 propyl cellu~ose produced by the Hercules Corporation of Wilmington, Delaware having a molecular weight of about 300,000 and a ~iscosity defined according to Figure 2) Ethyl cellulose......... ~........ _... ,O. ~.2 _ _ -R
The KLUCEL GF and ethyl cellulose is dispersed in the peppermint oil with vigorous stirring, thereby resulting in a viscous liquid. 65 Parts by weight of the powder flavor composition of Example W is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes in a dry, free flowing sustained release flavor powder.

EXA~IPLE CV
. .~ ~ . , . ,,, .. ~.. ~ ,~ ~.. ,, .
The ollowing mixture is prepared:

Ingredient Parts bv Weight Liquid flavor composition of.......... O... 52 Example B
Propylene glycol... O.............. O... OOO. 1 KLUC~L~ GF (bra~d of hydroxy-......... O... .3.8 propyl cellulose produced by the --Hercules Corporation of Wilmington, Delaware having a molecular weight of about 300,000 and a viscosity defined according to Figure 2) Ethyl cellulose........................... .2~2 '~ .
:. ~
The KLUCEL GF and ethyl cellulose is dispersed in the liquid flavor composition of Example B with vigorous stirring, thereby resulting in a viscous liquid. 44 Parts by weight of the powder flavor composition of .
Example Y is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a thixotropi sustained release flavor paste.

' . ~ ~c -: . ,~ .
.
. ~ . .
,. .

.. ~ 9t~

.' -149-.` .
EXAM:PLE CVI
. . ~.........
The following mixture is prepared:

Ingredient __ _ _ ___ Parts by Weight Liquid flavor composition of.......... ..~ 8.4 Example A
Propylene glycolO...... O..... O........ O.~.OO 3 KLUCEL~ GF (brand of hydroxy-...~...~a.... 5.2 propyl cellulose produced by the Hercules Corporation of Wilmington, ~elaware having a molecular weight of about 300,000 and a viscosity defined according to Figure 2) __ _ .~, .
The RLUCEL~ GF and is dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 48.4 Parts by weight of the powder flavor composition of Example G is then blended into the said viscous liquid, with stirring at 25C for a period of SO minutes resulting in a thixotropic sustained release flavor paste.
., .. 1, . . ~ :
EX~MPLE CVII

The following mixture is prepared:
;l . .
Ingredient Parts by Weight __ . _ _ _ _ Liquid flavor composition of........ ,.,... 25 Exa~ple B ~
Propylene glycol.O.-~....--O-..-O~--O---.. 2 KLUCEL GF (brand of hydroxy-.~.O. 3 ~ O ~ 10 propyl cellulose produced by the Hercules Corpora'ion of Wilmington, Delaware having a molecular weight of about 300,000 and a viscosity defined according to Figure 2) EthYl cellulose... ~l...................... .4 _ I
, . ' . ' .

.. :
:

~ V~

R
The KLUCEL GF and e~hyl cellulose is dispersed in the liquid flavor composition of ~xample B with vigorous stirring, thereby resulting in a viscous liquid~ 65 Parts by weight of the powder flavor composition of Example H is then blended into the said viscous liquid, with stirring at 40C for a period of 100 minutes resulting in a dry, free flowing sustained release !~ flavor paste.
:' EXAMPLE CVIII
.
, 10 The following mixture is prepared~
.
Ingredient _ Parts by Weight Liquid flavor composition of... O......... ~25 . Example C
:~ Propylene glycol............... r........ O. 1 : KLUCEL~ GF (brand of hydroxy-........... ... 3 propyl cellulose produced by the Hercules Corporation of Wilmington, Delaware having a molecu:Lar weight of about 300,0Q0 and a viscosity .defined according to Figure 2) Ethyl cellulose......... ,................................ _._........ 8. __ The KLUCEL~ GF and ethyl cellulose is dispersed in the liquid flavor composition of Example C with vigorous - stirring, thereby resulting in a viscous liquid. 65 Parts .
.~ by weight of the powder flavor composition of Example J
is then blended into the said viscous liquid, with stir-ring at 25C for a ~eriod of 30 minutes resulting in a .~ . dry~free flowing sustained release flavor paste.
. .
~ : `
. ..

1~ ~Ug7~3 1 -151-~
,~' EX~PLE_CIX
CHEWING GUM

100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example XXIII. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Company.
, ~ he resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
~; The strips are cut into lengths of 3 inches eachO On chewing, the chewing gum has a pleasant long lasting cherry flavor.
.~ 'i ' EXAMPLE CX
~ CHEWING GUM
.' . ....... ____ 100 Parts by weight of chicle are mixed with 18 - parts by weight of the flavor prepared in accordance with Example XXIV. 300 Parts ol sucrose and 100 parts of corn syrup are then added. Mixing is effected in a ribbon blender with jacketed sicle walls of the type manufactured by the Baker Perkins Company. ----. . .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness~
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting cherry f'avor.

.~

, ' . , . .

9'793 ` -152 EXAMPLE CXI
_HEI~ING GVl~l ;~ 100 Parts by weight of chicle are mixed with 4 - parts by weight of the flavor prepared in accordance with Example XC. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.

The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting peppermint flavor.
~, .
EX~MPLE CXII
CHEWING GUM
.~
~; 100 Parts by weight of chicle are mixed with 18 ; parts by weight of.the flavor pxepared in accordance with Example XCI. 300 Parts of sucrose and 100 parts ` of corn syrup are then added. ~5ixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co. ~~
, .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant lc~ lasting peppermint flavor.

9'79 EX~5PLE CXIII
CHEWING GU~
'~
l00 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example XCII~ 300 Parts of sucrose and l00 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.

The resultant chewing gum blend is then manufactured into strips l inch in width and 0.l inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting lemon flavor.
;,, EXAMPLE CXIV
; C~lEWING GUM

l00 Parts by weight of chicle are mixed with l~
parts by weight of the flavor prepared in accordance with Example XCIII. 300 Parts of sucrose and l00 parts of corn syrup are then added. Mixing is effected in a ribbon blender w-th jacketed side walls of the type manufactured by the Baker Perkins Co. --The resultant chewing gum blend is then manufactured into strips l inch in width and 0.l inches in thicknessO
The strips are cut into lengths of 3 inches each. On ; chewing, the chewing gum has a pleasant long lasting lime flavor.
. ~
, .
.

~.

',:
EX~MPLE CXV
CHE WING GUM

100 Parts by weight of chicle are mixed wi-th 4 parts by weight of the flavor prepared in accordance with Example XCIV. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type ' manufactured by the Baker Perkins Co.
.
The resultant chewing gum blend i5 then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting . wintergreen flavor~
,. , EXAMPLE CXVI
CHEWING GUM

100 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance with Example XCV. 300 Parts of sucrose and 100 parts of corn syrup are then added. Mixing is effected in a ribbon blender with jacketed side walls o~ the type manufactured by the Baker Perkins Co.
' ..................................................................... . ~
The resultant chewing gum blend is then manufactured into strips l inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing yum has a pleasant long lasting ¦¦cherry flavor J , '', .
' ,' .
~ .

~:

.
E ~IPLE CXVII
.` CHEWING GUM

100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example XCVI. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is ef~ected in a ribbon blénder with jacketed side walls of the type manufactured by the Baker Perkins Co.
.~
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, thé chewing gum has a pleasant long lasting lemon flavor.
; . ' EXAMPLE CXVIII
CHEWING GUM

l00 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance with Example XCVII. 300 Parts of sucrose and 100 parts o~ corn syrup are then added. Mixing is effected in a ribbon blender with ~acketed side walls of the type - manufactured by the Bakër Perkins Co. - -'' ., . . .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into Iengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting lime ilavor.

., , . , ,.

.

$~

., EXAMPLE CXIX
..
CHEWING GU~
~ .

100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example XCVIII. 300 Parts of sucrose and 10U
parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed s,ide walls of the type manufactured by the Baker Perkins Co.
,~ ~ .
The resultant chewing gum blend is then manufactured into strips l inch in wid~h and 0.1 inches in thickness.
O .The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting orange flavor.

EX~IPLE_CXX
' CHEWING GUM

100 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance with Example XCIX. 300 Parts of sucrose and 100 p,arts of corn syrup are then added. Mixing is effected in a 20` ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co. ...
, . .
The resultant chewing gum blend is then manufactured into strips l inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum as a pleasant long lasting cherry flavor.
.. ...
.

J

~$~
`-157-.
E ~lPLE CXXI
..~
CHEWING GUM
.~
lG0 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example C (100). 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with iacketed side walls of the type manufacture~ by thé Bàker Perkins Co.

~he resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches eachO On chewing, the chéwing gum has a pleasant long lasting cherry flavor.

EXAMPLE CXXII
eHEWING GUM
... ..
lG0 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance ; with Example ~I~ 300 Parts of sucrose and 100 parts ; of corn syrup are thén added. Mixing is effected in a ~ibbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.
. . .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing g~m has a pleasant long lasting -lemon flavor.
.
' ~
., ~

~158-:
EXI~lPLE CXX I I I
. __ CHEWING GUM
.~
100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with ExampLe CII. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.

The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting / lime flavor.
~.

CHEWING GUM
..
100 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance with Example CIII. 300 Parts of sucrose and 100 parts of corn syrup are then added. Mixing is effected in a ribbon blender with jacketed side walls ~f the type manufactured by the Baker Perkins Co. ---.
The resultant chewing gum blend is then manufactured ; into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting peppermint flavor.

3a . , ~ c`

g~93 - . ~15~-, EXAMPLE CXXV
CE:EWING GUM
.
100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example CIV. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type ;manufactured by the Baker Perkins Co.
., . . .
The xesultant chewing gum blend is then manufactured into strips l inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting peppermint flavor.
. , ' EXAMPLE CXXVI ~ -` CHEWING GUM

100 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance with Example CV. 300 Parts of sucrose and 100 parts of corn syrup are then added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.
'.` . , .
, The resultant chewing gum blend is then manufactured into strips l inch in width and 0.1 inches in thickness.
~ The strips are cut into lengths of 3 inches each. On ; chewing, the chewing gum has a pleasant long lasting lemon flavor.
.

. , ' ~, EXAMPLE CXXVII
C~EWING GUM
'.
100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example CVI. 300 Parks of sucrose and 100 parts o corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.
.`
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting cherry flavor.

EX~IPLE CXXVI I I
CEIEWING GUM
.
100 Parts by weight of chicle are mixed with 18 parts by wei~ht of the flavor prepared in accordance with Example CVII. 300 Parts of sucrose and 100 parts of corn syrup are then added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.
, . .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting lemon flavor.
. , ~ _, .

., ' . . ~

~ 7~3 .~
EXAMPLE CXXIX
CHEWING GUM
~ ' .
100 Parts by weight of chicle are mixed with 4 parts by weight of the flavor prepared in accordance with Example XXI. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.
': ' ' . , .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into lengths of 3 inches each. On chewing, the chewing gum has a pleasant long lasting lime flavor.
. ` . , .
. ' * * * * * , .

A taste test is made to compare the chewing gum products of this invention of Example CIX-CXXIX inclusive ; - with (i) standard chewing gum containing the same total amount of flavor in unfixed form and (ii) chewing gum containing the same total amount: of flavor without the hydroxypropyl cellulose and with each flavor ingredient (fixed and unfixed) added to the chicle separately rather than in a blend. During the test, 1.0 inch x 3.0 inch x 0~1 inch slabs of each gum are separately chewed and the following noted: Time and intensity of initial flavor, extent of flavor burst, duration of interesting flavor level, and approximate total time during which flavor is available. In these tests, the ratlng o~ flavor intensity is measured by the person chewing, on a scale ranging from 0 to 10, the level of 1 indicating threshold flavor intensity just discernible to the taste, and a level of 10 indicatlng a maximum intensity above which the sensation c originating in flavor is unpleasant.

, W162-The commercially available s~andard (i) containing unfixed flavor in chicle i5 characterized by initial indi cation of flavor at a level of 1 after about 7~8 seconds.
Intensity rises to 3 at about 15 seconds, and thereafter at a slower rate to a level of 6 at about 60 seconds.
At this point, flavor intensity drops off to 3 after about ~0 seconds. At about 2 minutes, the flavor intensity is at the uninteresting low level of 1.5. After 4 minutes of chewing, the flavor drops below the threshold value of 1, and the standard gum (i) is flat and lifelessq ., . .
: ~ . The standard (ii) containing flavor in both fixed and unfixed form but without the hydroxypropyl cellulose and with each flavor ingredient (fixed and unfixed) added : to the chicle se~arate rather than in a blend, is chara-cterized by initial indication of flavor at a level of 3 after 7 8 seconds with intensity rising to 6 at about 20 seconds and thereafter a slower rate at a level of ?
at about 60 seconds. At that polnt, the flavor intensity i drops ofE to about 5 after about 90 seconds. At about 4 minutes, the flavor intensity is at the uninteresting level of 1.5. After 8 minutes of chewing; the flavor drops below the threshold value of 1 and the standard gum (ii) is fla~ and ifeless.

. ~ ' , .' ' . ' , .

r ~ 3 L ~ 9 3 Samples prepared in accordance with the invention as set orth in Examples CIX-CXXI~, supra, are found to have an initial flavor liberation which occurs substan~ially : immediately ~at about 0.25 seconds~ i.e. more ~uickly than does that of the standard or ~i) or (ii), and which is at a higher level than that of either standardO .The flavor or intensity of the chewing gum product of this invention continuously rises to a high level which is four fold that of the maximum level reached by the standard (i) and twice that of the maximum level reached by the standard (ii) and it remains at this high level for a total period of time which is four fold the total flavor perception time : of the standard (i) and twice the total flavor perception .~ time of the standard (ii). Under preferred conditions, : flavor l.iberation is apparent for a time-which approaches 20 minutes. During the entire chewing period, which is ~. typically 2-4 times as long as the chewinperiod of either : standard chewing gum, the flavor of the product of this invention may be found to be rich, full-bodied and substan-tially true in characterO

It will be apparent to the person making the.chewing test that the chewing gum samples prepared in accordance with this invention are eminently superior to the samples containing the same amount of flavoring oil in unfixed form alone or the chewing gum containing the same total .
amount of flavor without the hydroxypropyl cellulose and with each flavor ingredient (fixed a~d unfixed) added to the chicle separately rather than in a blend. The extended flavor perception time, early flavor release,.true flavor character, and high degree of released flavor make this new product superior~
. . . ,. . , . .

~-.
'79 3 EXAMPLE CXXX
_ _ .
TOOTEIPASTE FO~ULATION

The following separate groups of ingredients are pre~
pared:

Parts by Weight Ingredient , .... ~
Group "A"
30.200 Glycerin 15.325 Distilled Water ,100 Sodium Benzoate .125 Saccharin Sodium .400 Stannous Flouride ; G~oup "B"
12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) Group lC"
2.000 n-Lauroyl Sarcosinate ~foaming agent) ~ ' Gro up " D "
1. 200 Flavor Material of Example XXIII

100.00 (Total) PROCEDURE
1. The ingredients in Group "A" are stirred and heated in a 5~eam jacketed kettle to 160F.
2. Stirring is continued for an additional three to f ive minutes to form a homogeneous gelO
3. The powders of Group "B" are added to the ' gel, while mixing until a homogeneous paste is formed.
4. With stirring, the flavor of "D" is added and lastly the sodium n-lauroyl ~arcosinate.
5. ~ The resultant slurry is then blended for ' one hour. The completed paste is then transferred to a three roller mill and then homoqenized, and finally rubed.
~ .

--~
~ 7~3 .' The xesulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant cherry flavor, of constant strong intensity throughout said procedure (1-1.5 minutes)~ .
.,. .
EXAMPLE CXXXI -;~ TOOTHPASTE FORMULATION
;i,~ . . . , .
;:
:~ The following separate groups of ingredients are pre pared:
Parts by ~eight Ingredient ; 10 Group "A"
30.200 Glycerin 15.~25 Distiiled Water .100 Sodium Benzoate .125 Saccharin Sodium . .400 Stannous Flouride .

Group "B"
: 12.500 Calcium Carbonate ~ 37.200 Dicalcium Phosphate (Dihydrate) .~ ~ - .
Group "C"
2.000 n-hauroyl Sarcosinate ~:. (oaming agent) '.' i ' ' "' ' . , , ' .
~ Group "D"
:~ `. lo 200 Flavor Material of Example XXIV .
., _ ' - .
. 100.00 (Total) .~. PROCEDURE
. 1. The in~redients in Group "A'i are stirred and heated in a steam jacketed kettle to .: 160F.
2. Stirring is continued for an additional three to five minutes to form a homogeneous gel.
The powders of Group "B~ are added to the .
~gel, while mixing until a homogeneous ' paste is formed.
4, With stirringJ the flavor of "D" is added and lastly the sodium n-lauroyl : ~arcosinate. , .
5, ~he resultant slurry is then blended or one hour. The completed paste is then :: transferred to a three roller mill and ; then homogenized, and finally tubed.
~' ~
. , .

9~7 ~166-The resulting toothpaste when used in a normal tooth~
brushing ~rocedure yields a pleasant cherry flavor, of constant strong intensity throughout said procedure (1-1.5 minutes)~

EXAMPLE CXXXII
TOOTHPASTE FGRMULATION

;i The following separate groups of ingredients are pre- paredO

.Parts by Weight Ingredient _ _ 10-Group "A"
: 30.200 Glycerin 15.325 Distilled Water . .100 Sodium Benzoate . .125 Saccharin Sodium 400 Stannous Flouride .
Group "B"
: 12.500 Calcium Carbonate :~ 37.200 Dicalcium Phosphate (Dihydrate) Group "C"
- . 20 2.000 n-Lauroyl Sarcosinate ~foaming agent) .
~ ' , , .
. ~Group " Dr 1~200 . Flavor Material of Example XC
. . . ~
100.00 ~Total) PROCEDURE
1. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to 160F.
2. . Stirring is continued for an additional three to five minutes to form a homoqeneous gel.
3. The powders of Group ~B" are added to the ~: ~ gel, while mixing until a homogeneous paste i5 formed, 4. With stirring, the flavor of "D" is added . and la tly the sodium n-lauroyl sarcosinate.

5. The resultant slurry is then blended for ,: one hour. The completed paste is then : tr~nsferred to A three roller mill and then homogenized, and finally tubed.

~ 7 .. 167-The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant peppermint flavor, o~
constant strong intensity throughout said procedure (1-1.5 minutes).
.
. EXAMPLE CXXXIII . . .
TOOTHPASTE FORMULATION

The ollowing separate groups of ingredients are pre-pared:
..
. Parts by Weight_ Ingredient lQ Group "A"
30.200 Glycerin 153 325 Distilled Water .100 Sodium Benzoate . o125 Saccharin Sodium .. ~400 Stannous Flouride ., , .
.: Group "B"
12~500 Calcium Carbonate .~ 37.200 Dicalcium Phosphate (Dihydrate) .,~ . . .
. Group n Cll - ~
20 2.000 n-~.auroyl Sarcosinate (foaming agent~ -.. Group "D" .
1.200 Flavor Material of Example XCI

100. 00 (Total ) PROC EDURE
. 1. The ingredients in Group "A" are stirred alld heated in a steam jacketed kettle to . 160F. .
2. Stirring is continued or an additional three to ive minutes to form a homo~eneous gel.
.. 3. The powders of Group "B" are added to the. gel, while mixing until a homogeneous : paste is formed.
. 4. WLth stirring, the flavor of ~D" is added.: and lastly the sodium n-lauroyl .~ sarcosinateO .
5. ~he resultant slurry is then blended for one hour. The completed paste i5 then transferred to a three roller mi~l and : then homogenized, and inally tubed.
~ I ~
' I ' , I
.

The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant peppermint flavor, of constant strong intensity throughout said procedure (1-1.5 minutes).

EXAMPL,E 5XXXIV
TOOTHPASTE FORMULAT~ON
The following separate g~oups of ingredients are pre-paredO

Parts by Weight Ingredient Group ~A"
. 30~200 Glycerin ; 15.325 Distilled Water .100 Sodium Benzoa~e o125 Saccharin Sodium - .400 Stannous Flouride Group "B"
12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) Group "C"
2.000 n-Lauroyl Sarcosinate (foaming agent) -Group "D"
- 1.200 Flavor Material of Example XCII
~ , . _ .
100.00 (Total) PROCEDURE ~ .
l. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to 160F.
2. Stirring is continued for an additional 3Q ~ three to five minutes to form a homogeneous gel.
3. The powders of Group "B" are added to the , gel, while mixing until a homogeneous paste is formed.
4. With stirring, the flavor of "D" is added : and lastly the sodium n lauroyl sarcosinate~ , 5. The resultant slurry is then blended for one hour. The completed paste is then transferred to a three roller mill and then homogenlzed, and finally tubed.
',~ ~

:~

The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lemon flavor, of constant strong intensity throughout said procedure (1-1.5 minutes).
.. ...
: EXAMPLE CXXV
TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared:
. .
Parts by Weight Ingredient Group "A"
30.200 Glycerin 15.325 Distilled Water .100 Sodium Benzoate .125 Saccharin Sodium ` .400 Stannous Flouride Group ~B"
12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) .' . , ' ' ' ':
Group "C"
2.000 n-L~uroyl Sarcosinate (foaming agent) ; ' ,.
Group "D"
lo 200 Flavor Material of Example XCITI

100 . 00 ( Total ) -PROCEDURE
lo The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to 160~.
2. Stirring is continued for an additional three to five minutes to form a homogeneous gel.
3. ~he powders of Group "B" are added to the gel, while mixing until a homogeneous paste is formed.
~ith stirring, the flavor of "D" is added and lastly the sodium n-lauroyl sarcosinate.
5. The resultant slurry is then blended for one hour. The completed paste is then trans~erred to a three roller mill and then homogenized, and finally tubedO
. . .

--- ~ 3~

-17~
. ' .
The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lime flavor, of : constant strong intensity throughout said procedure (1-1.5 minutes)O

EXAMPLE CXXXVI .
TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-.:: pared: -. ' ' .
. Parts by Wei~ht Inqredient . ~
Group "A" . . . .
. 30.200 Glycerin . . 150 325 Distilled Water : .100 Sodium Benzoate . .125 Saccharin Sodium ~ . .400 Stannous Flouride -'' ~
Group "B" - ----12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) ~ .
:~ Group "C"
, . 2.000 n-Lauroyl S~rcosinate (foaming agent) .~ .
Group "D~ . .
' ~ . 1.200 Flavor Material of Example~CIV
.

: ~- . ... _ -~ 100.00 (Total) . PROCEDURE ;
.' . . 1. The ingredients in Group "A" are stirred .:~ and heated in a steam jacketed kettle to 160F.
;: 2. Stirring is continued for an additionai .
~ 30 three to five minutes to form a .
: homogeneous gel.
.; 3O The powders of Group "B" are added to the .~ . gel, while mixing until a homogeneous .
.~ paste is formed.
.; 4. With stirring, the flavor of n D~ iS added - and lastly the sodlum n-lauroyl -~arcosinate.

:; 5. The resultant slurry is then blended for .
. one hour. The completed paste is then:~ transferred to a three roller mill and ~ then homogenized, and finally tubed.
"
.
. .

-7'~3 ;171--The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant wintergreen flavor, of constant strong intensity throughout said procedure ( l-lo S
minutes)O

~: EXAMPLE CX~7 TOOTHPASTE FORI~ULATIO~`l The following separate groups of ingredients are pre-pared:
.
. Parts by Weight Ingredient , . .~
10Group "A"
30.200 Glycerin 15.325 Distilled Water ~100 Sodium Benzoate .125 Saccharin Sodium 400 Stannous Flouride Group "Bl' 12.500 Calciurn Carbona~e 37.200 . Dicalcium Phosphate (Dihydra~e) ., Group "C"
. 202.0Q0 n~Lauroyl ',arcosinate : (foaming agent) .
'~ . , .
Group "D" - ---; .: i.200 Flavor Material of Example XCV .
,.~ ~
. 100.00 (Total) ~
: .PROCEDURE
1. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to : 160F.
: 20 Stirring is continued for an additional - three to five minutes to form a homogeneous gel. .
. 3~ ~he powders of Group "B" are added to the gel, while mixing until a homogeneous -~paste is formedO
~, , With stirring, the flavor of ~D" is added : and lastly the sodium n-lauroyl ~arcosinate. .

The resultant slurry is then blended for one hourO The cornpleted paste is then transferred to a three roller mill and then homogenized, and finally tubed.
Il I

The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant cherry flavor, of : constant strong intensity throughout said procedure tl-l.5 minutes).
, .
EXAMPLE CXXX~
TOOTHPASTE FORMULATION
c The following separate groups of ingredients are pre-pared:
.
Parts by Weight Ingredient , Group "~."
30~200 Glycerin . 15~32S Distilled Water olOO Sodium Benzoate :~ ol25 Saccharin Sodium ~ O400 Stannous Flouride ',`
. Group "B"
; 12.500 Calcium Carbonate ~ ~ 37.200 Dicalcium Phosphate (Dihydrate) . .
: : Group "C"
- . 20 2.00U n-Lauroyl ';arcosinate . ~
(foaming agent) . ~ ' , . ~ ~roup "D"
l.200 Flavor Material of Example XC~I .
.- ~ -.
l00.00 (Total) . PROCEDURE
. l. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to . 160F. .
2. Stirring is continued for an additional .
: 30 three to f ive minutes to form a homogeneous gel.
3. The powders of Group "B" are added to the gel, while mixing until a homogeneous .
, paste is formed. .
4. With stirring, the flavor of "D" is added ., and lastly the sodium n-lauroyl sarcosinate.
5. The resultant slurry is then blended for .~ one hour. The completed paste is then ransferred to a three roller mill and then cmoye~ized; and fina11~ tubed, iL9`7~3 `173~
~.~
The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lemon fl~vor, of constant strong in~ensity throughout said procedure (1-l.S
minutes).
. ' , .
EXAMPLE CXXX~
.~ TOO~PASTE FORM~TLATION.
The following separate groups of ingredients are pre-pared:
,~ .
Parts by Weight Ingredient , _ _ .. ~
: ~ lQ Group "A"
30.200 :Glycerin . ~ 15.325 Distilled Water . .100 .Sodium Benzoate : .125 Saccharin Sodium : . .400 Stannous Flouride ~ .
.;, Group 11 B~
. 12.500 Calcium Carbonate .~ : 37.200 Dicalcium Phosphate (Dihydrate) .'.' ' ~; . Group "C" .
.``l - 20 2.000 n-~auroyl Sarcosinate , (foaming agent) ~ -. i ' .
.~ ~ Group.~'D"
200 Flavor Material of Example XCY~I .
,., -., . 100-00 (Total) f .~ PROCEDURE .
1. The ingredients in Group "A" are stirred a~d heated in a steam jacketed kettle tv . . 160F.
,. 20 ~tirring is continued for an additional three to five minutes to form a homogeneous gel.
3. ~he powders of Group "B" are added to the .
. . ~ gel, while mixing until a homogeneous ; paste is formed.
,~ 4. W$th stirring, the flavor of "D" is added and lastly the sodium n-lauroyl ' ~arcosinate. .
5. ~he resultant slurry is then blended for one hour. The completed paste is then transferr2d to a three roller mill and then homogenized, and f-nally tabed, 111~3793 The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lime 1avor9 of constant strong intensity throughout said procedure (1-1.5 minutes).

EXAMPLE CX~X~T:II
TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared:

Parts by ~'eiqht Ingredient 0Group "A"
30.200 Glycerin 15.325 . Distilled Water .100 Sodium Benzoate : .125 Saccharin Sodium .400 Stannous Flouride .` ' ...
Group "B"
12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) Group "C"
2.000 n-Lauroyl ~arcosin~te (foaming agent) ~; ', . ' ' ''''' ' . , ; .Group "D"
-. 1.200 Flavor Material of ~xample XCVXII .

. . l00.00 (Total) ~ .
: PROCEDURE
1. The ingredients in Group "A" are stirred :~ . and heated in a steam jacketed kettle to 160F~ .
2. Stirring is continued for an additional : 30 three to five minutes to form a . homogeneous gel.
3. The powders of Group "Bi' are added to the gel, while mixing until a homogeneous ' - paste is formed.
. ~ith stirring, the flavor of nD" is added and lastly tne sodium n-lauroyl sarcosinate. ~ .
5. The ~esultant slurry i5 then blended for one hour. The completed paste is then transferred to a three roller mill and then homogenized, and finally tubed.
. , ~ .

l~L19793 . ~ _ The resulting toothpaste when used in a normal tooth-brushing ~rocedure yields a pleasant orange flavor, of constant strong intensity throughout said procedure (1-1.5 minutes)O

EXAMPLE CXX~IX
TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared:
. . .
Parts by Weight Ingredient ~ . . .~
Group "A"
30.200 Glycerin 15,325 Distilled Water .100 Sodium Benzoate ~125 Saccharin Sodium .400 Stannous Flouride .
:.~
Group "B"
~ 12.500 Calcium Carbonate ; 37.200 Dicalcium Phosphate (Dihydrate) ... ; . ~ .
;`~ Group "C"
~0 2.000 n-Lauroyl Sarcosinate (foaming agent) .. . . ' ''' Group "D'l . 1,200 Flavor Material of Example XCIX

, 100.00 ~Total3 PRO~EDURE
.. . lo The ingredients in Group "A" are stirred ; and heated in a steam jacketed kettle to 160F.
2. Stirring is continued for an additional three to five minutes to form a homogeneous gel.
3. The powders of Group n B" are added to the gel~ while mixing until a homogeneous paste is formed.
4, With stirring, the flavor of "D" is added and lastly the sodium n~lauroyl sarcosinate. , 5. The resultant slurry is then blended for one hour. The completed paste is then transferred to a three roller mill and , then homogenized, and finally tubed.

The resulting toothpaste when used in a normal tooth-: brushing procedure yields a pleasant cherry flavor, of CQnstant strong intensity throughout said procedure ~1-1.5 minutes)~

EXAMPLE CXL
. TOOTHPASTE FORMULATION
.; The following separate groups of ingredients are pre-. pared:
.

Parts by Weight Ingredient ,~
: 10 Group "A"
.~ . 30.200 Glycerin 15.325 Distilled Water . ~100 Sodium Benzoate : . .125 Saccharin Sodium :
.400 Stannous Flouride Group "B"
12.500 Calcium Carbonate :i~ 37.200 Dicalcium Phosphate (Dihydrate) . Grou~ "C"
. 2Q 2.000 n-Lauroyl ';arcosin~te .~ (foaming aqent) , ' . ;'' .
. ~roup "D"
. : 1.200 Flavor Material of Example C (100) , . .
.. 100.00 (Total) ~ .
. PROCEDURE -. 1. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to . 160F.
2. Stirring is continued for an additional 3Q three to five minutes to form a .
: homogeneous gel.
3. The powders of Group "B" are added to the . gel, ~hile mixing until a homogeneous .
paste is formed.
4. ^ With stirring, the flavor of ~D" is added and lastly the sodium n-lauroyl ~arcosinate.
5, ~he resultant slurry is then blended for .
one hour. The completed paste is then . ~ransferred to a three roller mill and then homogenized, and finally tubed~

~ i : ~
-'7~3 ~77 The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant cherry flavor~ of constant strong intensity throughout said procedure (l-1.5 minutes).
;:
EXAMPLE CXLI
TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared-~ ' Parts by Weight Ingredient 10G~oup "A"
30~200 Glycerin 15.325 Distilled Water l00 Sodium Ben~oate ~ .125 Saccharin Sodium ; O400 5tannous Flouride ., Group "~"
`~ 12.500 Calcium Carbonate 37.205 Dicalcium Phosphate (Dihydrate) ~.
Group "C"
; 202.000 n-Lauroyl Sarcosinate ~ ~foaming agent) ., , .
- Group n D~' .
1.200 Flavor Material of ~xample CI

lQ0.00 (Total) PROCEDURE
1~ The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to 160P.
2~ Stirring is continued or an additional three to five minutes to form a homogeneous gel.
3. The powders of Group "B" are added to the gel, while mixing until a homogeneous 'paste is formed.

4. With stirring, the flavor of "D" is added and lastly the sodium n-lauroyl ~arcos inate.
5. The resultant slurry is then blended for one hour. The completed paste is then transferred to a three roller mill and then homogenized, and finally tubed.

~ t7~
. .
. -178-The resul ting toothpaste when used in a normal tooth brushing procedure yield~ a pleasant lemon flavor~ of ~ ~ constant strong intensity throu~hout said procedure (1-1.5 .. minutes), , .................... . , . ~ EXAMPLE CXLI~
~: TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared:
,,..,~
:~. Parts by Weight Ingredient ,,. . __ . ~.......... _ . ,. _. ~
~: 10Group "A"
: . 30~200 Glycerin ~
. 15.325 Distilled Water ~: .100 Sodium Benzoate : . .125 Saccharin Sodium 400 Stannous Flouride .., Group "B"
12.500 Calcium Carbonate .~ ` 37.200 Dicalcium Phosphate (Dihydrate~
:, : . , ' .
. Group "C" .
2.000 n-Lauroyl Sarcosinate `
' (foaming agent) .
Group "D" ~
1.200 Flavor Material of Example CII .
:.
: 100.00 (Total) PROCEDURE
.~ 1. The ingredients in Group "A" are stirred .~ and heated in a steam jac~eted kettle to .
2. Stirring is continued for an additional three to five minutes to form a homogeneous gel.
3. The powders of Group "B~ are added to the J gel, while mixing until a homogeneous paste is formed.
: 4. With stirring, the flavor of "D" is added a~d lastly the sodium n-lauroyl . 3~ rcosinate. .
5. ~he resultant slurry is then blended for : one hour~ The completed paste is then transferred to a three roller mill and then homogenized, and finally tubed.

~ '7~3 ~179-,.

The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lime flavor, of con~tant strong intensity throughout said procedure (1-1.5 ; minutes)O
.~ . .
XAMPLE CxLII:l:

~r ' The following separate groups of ingredients are pre-pared:
'. , .
Parts by Weight Ingredient -~ ~ 10 Group "A"
30.200 Glycerin 15.325 Distilled Water .100 Sodium Benzoate - ol25 Saccharin Sodium ~400 Stannous Flouride ,, Group ~B~
12.500 Calcium Carbonate 37O200 Dicalcium Phosphate (Dihydrate~
'~' ; ' : Group ~C"
~02.000 n-Lauxo~l Sa~cosina~e ~foaming agent) . , ' ,.
Group n D~
1.200 Flavor Material of Example CIII
: ' 100~00 (Total) PROCEDURE
1. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to , 160F.
2. Stirring is continued for an additional ~0 three ,o five minutes to form a homog~(~20us gel.
3 . The powders of Group "B" are added to the , gel, while mixing until a homogeneous -paste is formed.
4. With stirring, the flavor of "D" is added and lastly the sodium n-lauroyl ~arcosinate.
5. The re5ultant slurry is then blended for , one hour. The completed paste is then transferred to a three roller mill and then homogenized, and flnally tubed.

. . -1~0-..
The resulting toothpas~e when used in a normal too~h-.` brushing procedure yields a pleasant peppermint flavor, of .~ constant strong intensity throughout said procedure (1-1.5 . minutes).
, . ................................ ..
EXAMPLE CXLIl.~
TOOTHPASTE FORMULATION
.~ The following separate g~oups of ingredients are pre-. pared:

.; Parts by Weight Ingredient Group "A"
. . 30.200 Glycerin v~ 15~325 Distilled Water ol00 Sodium Benzoate . .125 Saccharin Sodium .: . .400 Stannous Flouride '.1. ~
; Group "B"
12. 500 Calcium Carbonate . ~ 37O200 Dicalcium Phosphate ~Dihydrate) . Group "C"
20 2.000 n-Lauroyl S~rcosin~te .
~ (foaming agent) , . ,.
. Group "D" -----1.200 Flavor Material of ExampleC
-,' .. _ ._. ' ' 100.00 (Total) . PROCEDURE
: 1. The in~redients in Group "A" are stirred and heated in a steam jacketed kettle to 16OOF.
:- 2, Stirring îs continued for an additional -three to five minutes to form a homogeneous gel.
3 G The powders of Group "B" are added to the gel, while mixing until a homogeneous ^
pa~te is formed.
4. With stirring, the flavor of "D" i5 added and lastly the sodium n-lauroyl sarcosinate.
5. The resultant slurry is then blended for .
one hour. The completed paste is then transferred to a three roller mill and :~ then homogenized, and finally tubed. I

-~ ~ 3 l -181-:' .
rhe resulting toothpas~e when used in a normal tooth~
brushing procedure yields a pleasant peppermin~ flavor, of ; constant strong intenslty throughout said procedure (l-l.S
: minutes).
. .

:, . EXAMPLE CXLV .
` TOOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared:

Parts by Weight Ingredient 10Group "A"
30.200 Glycerin - 15.325 Distilled Water 100 Sodium Benzoate .12~ Saccharin Sodium .400 Stannous Flouride . .
Group "B"
12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) "~ : -Group "C"
202.000 n-Lauroyl Sarcosinate -~
[foaming agent) ~ ' ` Group "D"
1.200 Flavor Material of Example CV .
:~ '` ..
100.00 (Total) PROC EDURE
1. The ingredients in Group "A" are stirred and heated in a steam jacketed ket~le to 160F.
2. Stirring is continued for an additional three to five minutes to for~ a homogeneous gel.
3. The powders of Group "B" are added to the gel, while mixing until a homogeneous ~paste is formed.

- 4. With stirring, the flavor of "D" is added - and lastly the sodium n-lauroyl sarcosinate.
5. The resultant slurry is then blended for one hour. The completed paSte is then transferred to a three roller mill and then homogenized, and finally tubed.
.

:
:~3~7~3 ~ -182-.,.
The resulting toothpaste when used in a normal tooth-brushlng ~rocedure yields a pleasant lemon flavor~ of constant strong intensity throughout said procedure (l-l.S
minutes)O
., . ' ' EXAMPL~ C~:,~7I
TOOTHPASTE FORMULAT~ON
The following separate groups of ingredients are pre-paredO :
'~
. Parts by Weight Ingredient __ .~ . 10 . Group "A"
. 30.200Glycerin 15.325 Distilled Water . .100 Sodium Benzoate .125 Saccharin Sodium . .400 Stannous Flouride ' . Group "Bl' 12.500 Calcium Carbonate 37.200 Dicalcium ~hosphate (Dihydrate) ,. . , - .
~ - Group "C"
; ~0 2.000 n-Lauroyl Sarcosinate (foaming agent) - : Group "D" -1.200 Flavor Material of Example CV~ .
. ' 100.00 (Total) r PROCEDURE
1. ~he ingredients in Group "A" are stirred and heated in a steam jacketed kettle to . 160F.
2. Stirring is continued for an additional three to five minutes to form a :. homogeneous gel.
3~ The powders of Group "B" are added to the .
,gel, while mixing until a homogeneous paste is formed.
4. With stirring, the flavor of "D" is added and lastly the sodium n-lauroyl sarcosinate, , .
5. The resultant slurry is then blended for one hour. The completed paste is then transferred to a three roller mill and .
then homogenized, and finally tubed.
.
, ~ 3 The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasan~ cherry flavor, of constant strong intensity throughout said procedure ~1 1.5 minutes)~
. ., EXAMPLE CXLVII .
. _ ~OOTHPASTE FORMULATION
The following separate groups of ingredients are pre-pared:
. ~ .

Parts by Weight Ingredient Group "A"
30.200 Glycerin 15.325 Distilled ~ater .100 Sodium Benzoate .125 Saccharin Sodium - .400 Stannous Flouride Group IB'' ~~
12.500 Calcium Carbonate 37.200 Dicalcium Phosphate (Dihydrate) Group "Cn 2.000 n-Lauxoyl S~rcosinate --~
(foaming agent) . , ,.'' Group ~D~
1.200 Flavor Material of Example CVII
.."
100.00 (Total~
PROCEDURE
1. The ingredients in Group "A" are stirred and heated in a steam jacketed kettle to 160F.
2. Stirring is continued for an additional three to five minutes to form a homogeneous gel.
3. The powders of Group "E ~! are added to the gel, while mixing until a homogeneous ;
,paste is formed.
4. , With stirring, the flavor of "D" is added and lastly the sodium n-lauroyl sarcosinate.
5. The resultant slurry is then blended for one hour. The completed paste is then transferred to a three roller mill and then homogenized, and finally tubed~
. ..

-~ 7~3 . .
.

~ he resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lemon flavor, of constant strong intensity throughout said procedure (1-1.5 minutes).

. EXAMPLE CXL. __ _ IT
: ~oorll~As~ ~G~ L~l0'.
The following separate groups of ingredients are pre-pared:

Parts by Weight Ingredient . _ . ..... ___ ...
~0Group "A"
~ 30.200 Glycerin : 15.325 Distilled Water .100 Sodium Benzoate .125 Saccharin Sodium .400 Stannous Flouride Group "B"
: 12.500 Calcium Carbonate 37.200 Dicalcium :Phosphate (Dihydrate) Group "C"
202.000 n-~aurayl Sarcosin~te (foaming agent) " .. ' . ~' . , .
Group "D"
1.200 Flavor ~aterial of Example CVIII .

100.00 (Total) PROCEDURE
1. The ingredients in Group "A" are stirred : and heated in a steam jacketed kettle to . 160F. .
: 2. Stirring is continued for an additional .
three to five minutes to form a homogeneous gel.
3. The powders of Group "B" are added to the . ~gel, while mixing until a homogeneous -paste is formed.
: 4~ With stirring, the flavor of "D" is added and lastly the sodium n-lauroyl sarcosinate. ! .
5. The resultant slurry is then blended for one hour. The completed paste is then transferred to a three roller mill and then homogenized, and finally tubed~

,_ ~ L~

The resulting toothpaste when used in a normal tooth-brushing procedure yields a pleasant lime flavor, of constant strong intensity throughout said procedure (1-1.5 minutes).

EXAMPLE CXL I X
C~7EW~BLE VITAMIN TABLETS

The flavor material produced according to the process of Example XXIII is added to a Chewable Vitamin Tablet Formulation at a rate of 4 mg/gm which Chewable Vitamin Tablet Formulation is prepared as follows-. In a Hobart Mixer, the following materials are blended : to homogeneity-: - _Gms/1000 tablets Vitamin C (ascorbic acid) 70.0 : as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1~3~4O0 .; (Hoffmann La Roche) Vitamin B2 (riboflavin) as Rocoat riboflavin 33 1/3~ 5O0 : . Vitamin B6 (pyridoxine hydroch:loride) as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 : . Niacinamide as Rocoat niacinamide 33 1/3% 33.0 . Calcium pantothenate 11.5 : - Vitamin Bl (cyanocobalamin) .
as Merk 0.~ in gelatin ~ 3.5 Vitamin E (dl-alpha tocopheryl acetate) as dry Vitamin E acetate 33 1/3% Roche60 6 d-Biotin 0.044 Certified lake color s.o Flavor of Example XXII~ `~2.0 .
Sweetener sodium saccharin 1.0 Magnesium stearate lubricant lOo O ,, Mannitol q.s. to make _500.0 Preliminary tablets are prepared by slugging with flat-fa~ed punches and grinding the slugs to 14 mesh. 13.5 g dry ~itamin A Acetate and 0.6 g Vitamin D are then added as bead-lets. The entire blend is then compressed using concave .
punches at 0.5 g eachO - .

Chewing of the resultant tablets yields a pleasant, long-lastingl con~istently 5trong cherry flavor for a period of 12 m~nute~ ......... ..

.~ 3'7~3~

EXAMPLE CL
CHEWABLE VITAMIN TABLETS

The flavor material produced according to the process of Example XXIV is added to a Chewable Vitamin Tablet Formulation at a rate of 5 mg/gm which Chewable Vitamin Tablet Formulation is prepared as follows:
In a Hobart Mixer, the following materials are blended to homogeneity:
_ __ ___ Gms/1000 tablets Vitamin C (ascorbic acid) 70.0 as ascorbic acid-sodium ascorbate mi~ture 1:1 Vltamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3~ 4.0 ~Hoffmann La Roche) Vitamin B2 (riboflavin) as Rocoat riboflavin 33 1/3% 5,0 Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 Niacinamide as Rocoat niacinamide 33 1/3~ 33.0 Calcium pantothenate 11.5 Vitamin B (cyanocobalamin) as Merk 01~% in gelatin - 3,5 ; Vitamin E (dl-alpha tocopheryl acetate) - as dry Vitamin E acetate 33 1/3% Roche - 6~6 d-Biotin -0.044 Certified lake color 5.0 ;~ ~ Fl~vor of ~xample XXI~ ~ i 2.5 Sweetener - sodium saccharin 1.0 Magnesium stearate ]ubricant 10.0 Mannitol q.s. to make 500aO
Preliminary tablets are prepared by slugging with flat-faced punches and grinding the slugs to 14 mesh. 13.5 9 dry Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-lets. The entire blend is then compressed using concave punches at 0.5 g each. r .' . ~
Chewing of the resultant tablets yields a pleasant, long-lasting, consistently strong cherry flavor for a period of 12 minutes. , :

,' EX~MPLE CLI
CI~EWABLE VIT~MIN TABLETS
..
The flavor material produced according to the process of Example XC is added to a Chewable Vitamin Tablet Formulation at a rate of 6 mg/gm which Chewable Vitamin Tablet Formulation i5 prepared as follows:
In a Hobart Mixer, the following materials are blended to homogeneity:
Gms/1000 tablets 1 0 . _ ...... _ , ..................... .. _ _ Vitamin C ~ascorbic acid) 70.0 as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3% 4.0 (Hoffmann La Roche) Vitamin B2 (riboflavin) as Rocoat riboflavin 33 1/3% 5~0 Vitamin B6 tpyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3~ 4.0 Niacinamide as Rocoat niacinamide 33 1/3% 33.0 Calcium pantothenate 11.5 Vitamin Bl (cyanocobalamin) as Merk 0.~% in gelatin - 3.5 Vitamin E (dl-alpha tocopheryl acetate) as dry Vitamin E acetate 33 1/3% Roche 6.6 d-Bio~in 0-044 Cértified lake color 5.0 Flavor of Example XC ~ j3 ~
Sweetener - sodium saccharin 1.0 - 30 Magnesium stearate lubricant 10.0 Mannitol q.s. to make 500.0 Preliminary tablets are prepared by slugging with flat-faced punches and grinding the slugs to 14 mesh. 13.5 g dry Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-lets. The entire blend is then sompressed using concave ; punches at 0~5 g each. .
., Chewing of the resultant tablets yields a pleasant, long lasting, consistently strong peppermint flavor for a period of 12 minutes. , ~0 -~ ` ~ 7~3 . -188-, EXZ~MPLE CLI I
CHEW~BLE VITAMIN TABLETS
. ~ .

The flavor material produced according to the ,; process of Example XCI i5 added to a Chewable Vitamin Tablet Formulation at a rate of 7 mg/gm which Chewable ; Vitamin Tablet Formulation is prepared as follows:
In a Hobart Mixer, the following materials are blended to homogeneity.
Gms/lOOO tablets , ~ . -- .... , . . . _ _ .
Vitamin C ~ascorbic acid) 70.0 as ascorbic acid-sodium ascorbate mixture l:l Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 l/3~ 4.0' (Hoffmann La Roche) -Vitamin B2 (riboflavin) , .
as Rocoat riboflavin 33 l/3% 5~0 Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 l/3~ 4.0 Niacinamide as Rocoat niacinamide 33 l/3% 33.0 Calcium pantothenate ll.5 Vitamin Bl (cyano,cobalamin) as Merk 0.1% in gelatin 3.5 Vitamin E (dl-alpha tocopheryl acetate) as dry Vitamin E acetate 33 l/3% Roche , ' 6~6 d-Biotin ' ' 0.044 Certified lake color .S.O
Flavor of Example XCI - i 3.5 .
Sweetener - sodium saccharin l.O
Magnesium stearate lubricant lO.O
Mannitol q.s. to make 500.0 Preliminary tablets are prepared by slugging with flat-faced punches and grinding the slugs to l4 mesh. 13.5 g dry .
Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-lets, The entire blend is then compressed using concave punches at 0.5 g each. - .
.~
Chewing of the resultant tablets yields a pleasant, long lasting, consistently strong peppermint flavor for a period o~ l2 minutes. .
~0 ~ J~ 7~3 . -189 .
........
EXA~lPLE CLIII
,, ,, " . _ ~ .., . , . . _ .
CHEW~BLE VIT~lIN T~BLETS
.`
The flavor ~aterial produced according to the process of Example XCII is added to a Chewable Vitamin Tablet Formul~tion at a rate ~f 7 mgfgm which Chewable Vitamin Tablet Formulation is prepared as ~ollows:
In a Hobart Mixer, the following materials are blended to homogeneity:
Gms/1000 tablets 1 0 ,, ~
Vitamin C (ascorbic acid) 70.0 as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3~ 4.0 tHoffmann La Roche) Vitamin B2 (riboflavin) as Rocoat riboflavin 33 1/3% 5.0 Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 Niacinamide as Rocoat niacinamide 33 1/3% 33.0 Calcium pantothenate 11.5 Vitamin Bl (cyanocobalamin) as Merk 0.~ in gelatin --~ 3.5 Vitamin E (dl-alpha tocopheryl acetate) as dry Vitamin E acetate 33 1/3% Roche - 6~6 d-Biotin -O.04~
Certified lake color ~ 5.0 .
Flavor of Example XCII r i 3 . 5 Sweetener - sodium saccharin 1,0 Magnesium stearate lubricant lQ.0 Mannitol q.s. to make 500.0 :
Preliminary tablets are prepared by slugging with flat-. ~ faced punches and grinding the slugs to 14 mesh. 13.5 g dry : Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-lets. The entire blend is ~hen compressed using concave . punches at 0.5 g each.

; Chewing of the resultant tablets yields a pleasant, long lasting, consistently strong lemon flavor for a period of 12 minutes. , ~0 . . .

i ~ 7~3 EX~lPLE CLIV
CHEWABLE VITAMIN TABLETS

The flavor material produced accor~ing to the process of Example XCIII is added to a Chewable Vitamin . Tablet Formulation at a rate of 8 mg/gm which Chewable : Vitamin Tablet Formulation is prepared as follows: ' In a Hobart Mixer, the following materials are blended to homogeneity:
' Gms/lOOO tablets ., . ~ ~
10 Vitamin C (ascorbic acid) 70.0 as ascorbic acid sodium ascorbate mixture 1:1 . Vitamin Bl (thiamine mononitrate) : as Rocoat thiamine mononitrate 33 1/3% 4.0 ., (Hoffmann La Roche) Vitamin B2 triboflavin~
as Rocoat riboflavin 33 1/3~ 5.0 , Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3~ 4.0 Niacinamide 20 as Rocoat niacinamide 33 1/3% 33.0 '~ Calcium pantothenate 11.5 ' ~ Vitamin Bl ~cyanocobalamin) as ~erk 0.~% in gelatin , ~ 3.5 : Vitamin E tdl-alpha tocopheryl acetate) --. . as dry Vitamin E acetate 33 1/3% Roche,-6.6 ~ d-Biotin 0.044 :~ Certified lake color . 5.0 . .
- Flavor of Example XCIII ,l 4.0 , , Sweetener - sodium saccharin 1.0 30 Magnesium stearate lubricant 10.0 ; . ~annitol q.s. to make 500.0 _ _ . Preliminary tabl_ts are prepared by slugging with flat-.~ f~ced punches and grinding the slugs to 14 mesh. 13.5 g dry .
i Vitamin,A Acetate and 0.6 9 Vitamin D are then added as bead-., lets. The entire blend is then compressed using concave . ,punches at 0.5 g each. , ~ ~, J
Chewing of the resultant table~s yiel~ leasant, long lasting, consistently strong lime flavor for a period of 12 minutes~ , .

EXAMPLE CLV
CHEWABLE VIT~MIN TABLETS
.; - - .

The flavor material produced according to the process of Example XCIV is added to a Chewable Vitamin Tablet Formulation at a rate o 9 mg/gm which Chewable Vitamin Tablet Formulation is prepared as follows:
In a Hobart Mixer, the follo~ing materials are blended to homogeneity: .
_ _ _ ___ _ _Gms/1000 tablets Vitamin C (ascorbic acid) 70~0 as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl ~thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3~ 4.0 (Hoffmann La Roche) Vitamin ~2 ~riboflavin) as Rocoat riboflavin 33 1/3~ .5.0 Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 Niacinamide as Rocoat niacinamide 33 1/3~ 33.0 Calcium pantothenate 11.5 .
Vitamin Bl~ (cyanocobalamin) as MerX O.I~ in gelatin - 3.5 Vitamin E (dl-alpha tocopheryl acetate) .
as dry Vitamin E acetate 33 1/3~ Roche 6.6 d-Biotin 0,044 Certified lake color . 5.0 .
Flavor of Example XCIV ' 4-5 Sweetener - sodi~m saccharin 1.0 Magnesium stearate lubricant 10.0 Mannitol q.s. to make 500.0 - - _ . .
~ . Preliminary tablets are prepared by slugging with flat- .
:: faced punches and grinding the slugs to 14 mesh. 13.5 g dry.
~ Vitamin A Acetate and 0.6 9 Vitamin D are then added as bead-'................ lets. The entire blend is then compressed using concave . punches at 0.5 g each. .
. ~ . .
Chewing of the resultant tablet~ viql~s a Pleasant, long lasting, consistently strong wintergreen oil like .~ 40 flavor for a period o 12 minutes. ! ' .
i' .' ., ~ `7~3 EXP~IPLE CLVI
CHEWABLE VITAr~IN TABLETS
. ~- . . ,_ _, ,~ The flavor material produced according to the . process of Example XCV is added to a Chewable Vitamin : Tablet Formulation at a rate of 10 mg/gm which Chewabl~
Vitamin Tablet Formulation is prepared as follows:
In a ~lobart Mixer, the following materials are blended to homogeneity:
- __ _ _ _ Gms/1000 tablets 10 Vitamin C (ascorbic acid) 70.0 as ascorbic acid-sodium ascorbate mixture lol Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3% 4.0 (Hoffmann La Roche) Vitamin B2 (riboflavin) as Rocoat riboflavin 33 l/3% 5.0 Vitamin B6 (pyridoxine hydrochloride) -as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 ~0 Niacinamide as Rocoat niacinamide 33 1/3% 33~0 . Calcium pantothenate ll.5 . . Vitamin Bl (cyanocobalamin) as Merk 0.~ in gelatin 3.5 Vitamin E (dl-alpha tocopheryl acetate) ~ as dry Vitamin E acetate 33 l/3~ Roche - 6.6 : d Biotin. ~ 0,044 Certified lake color 5.0 Elavor of Example CV 55 0 .
~ Sweetener - sodium saccharin 1.0 3~ Magnesium stearate lubricant 10.0 Mannitol q.s. to make . 500.0 . ~
Preliminary tablets are prepared by slugging with flat-faced punches and grinding the slugs to 14 mesh. 13.5 g dry Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-lets. The entire blend is then compressed using concave punches at 0.5 9 e~ch.
. . . ~

Chewing of the resultan' tablets yields a pleasant, . long lastingl consistently strong orange oil-like flavor ; for a period of 12 minutes.
' .,.
.' . , ~

-~

~193-.
EXAMPLE CLVII
CHEWABLE VITAMIN TABLETS

The flavor material produced according to the ; pxocess of Example XCVI is added to a Chewable Vitamin Tablet Formulation at a rate of 5 mg/gm which Chewable Vitamin Tablet Formulation is prepared as followso In a Hobart Mixer, the following materials are blended to homogeneity:
Gms/1000 tablets . ~
Vitamin C (ascorbic acid) 70.0 as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3% 4~0-~Hoffmann La Roche) Vitamin B2 (riboflavin) as Rocoat riboflavin 33 1/3% 5~0 Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 Niacinamide as Rocoat niacinamide 33 1/3% 33.0 Calcium pantothenate 11.5 ; Vitamin Bl (cyanocobalamin) as Merk 0.~% in gelatin 3.5 Vitamin E (dl-alpha tocopheryl acetate) as dry Vitamin E acetate 33 1/3% Roche 6.6 d Biotin 0.044 Certi~ied lake color 5.0 Flavor of Example XCVI 2.5 Sweetener - sodium saccharin -lo O
`~ - 30 Magnesiu~ stearate lubricant 10.0 Mannitol q.s. to make 500 0 ~ Preliminary tablets are prepared by slugging with flat-; faced punches and grinding the slugs to 14 mesh. 13.5 g dry Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-lets. The entire blend is then compressed using concave punches at 0.5 g e~ch.
. . . . ~
Chewing of the resultant tablets yields a pleasant, ,i long-lasting, con~istently strong cherry f~avor for a period ~ 4~ of 12 minute . ,.

::

- ~ 3t~

; EX~MPLE CLIX
CHEI~BLE VITAMIN T~BLETS

The flavor material produced according to the process of Example XLVII is added to a Chewable Vitamin Table~ Formulation at a rate of 6 mg/gm which Chewable Vitamin Tablet Formulation is prepared as follows~
, .
In a ~obart Mixer, the following materials are blended to homogeneity:
_ __ _ Gms/1000 tablets Vitamin C (ascorbic acid) 70.0 . as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl (thiamine mononitrate) as Rocoat thiamine mononitrate 33 1/3% 4.0 (Hoffmann La Roche) - Vitamin B2 (riboflavin) as Rocoat riboflavin 33 1/3% 5.0 Vitamin B6 (pyridoxine hydrochloride) as Rocoat pyridoxine hydrochloride 33 1/3% 4.0 Niacinamide as ~ocoat niacinamide 33 1/3% 33.0 Calcium pantothenate 11.5 Vitamin Bl (cyanocobalamin) --as Merk 0.~ in gelatin 3.
Vitamin E ~dl-alpha tocopheryl acetate~
as dry Vitamin E acetate 33 1/3~ Roche 6~6 d-Biotin 0,0~4 Certified lake color S.o - ~lavor of Example CVII 3.0 Sweetener - sodium saccharin 1~0 Magnesium stearate lubricant 10~0 Mannitol q.s. to make ___ _ 500.0 Preliminary tablQts are prepared by slugging with flat-faced punches and grinding the slugs to 14 mesh. 13.5 g dry Vitamin A Acetate and 0.6 g Vitamin D are then added as bead-- lets. The entire blend is then compressed using concave punches at 0.5 g each.
.. " J .
Chewing of the resultant tablets yields a pleasant, long-lasting, consistently strong cherry flavor for a period of 12 minutes.
'~~ 40 . ,.
. . .

.; , -lgS- , EXAMPLE CLX
CEIEWABLE VIT~IIN TAB1ETS
. -- -- - - -- - ,.

The flavor material produced according to the process of Example XCVIII is added to a Chewable Vitamin ; Tablet Formulation at a rate of 7.5 mg/gm which Chewable : - Vitamin Tablet Formulation is prepared as follows:
: In a Hobart Mixer, the following materials are blended to homogeneity-Gms/1000 tablets . . . ~
Vitamin C ~ascorbic acid) 70.0 10 . as ascorbic acid-sodium ascorbate mixture 1:1 Vitamin Bl (thiamine mononitrate) -as Rocoat thiamine mononitrate 33 1/3% 4.0 (Hoffmann La Roche) . . Vitamin B~ (riboflavin) . as Rocoat riboflavin 33 1/3~ 5.0 .~ . Vitamin B6 (pyridoxine hydrochloride1 ---as Rocoat pyridoxine hydrochloride 33 1/3~ 4.0 . Niacinamide ~ 20 as Rocoat niacinamide 33 1/3%33.0 `~: Calcium pantothenate 11.5 ~- Vitamin Bl (cyanocobalamin) as Merk 0.~% in gelatin ~ 3.5 : Vitamin E tdl-alpha tocopheryl acetate) -;~ as dry Vitamin E acetate 33 1/3% Roche 6.6 d 8iotin . 0,044 ; Certified lake color 5~0 .
. Flavor of Example XCVIII 3.75 Sweetener - sodium saccharin 1.0 Magnesium stearate lubricant 10.0 . Mannitol q.s. to make 500.0 .. .. . ~.. _ ___ _ _ Preliminary tablets are prepared by slugging with flat-. . faced punches and grinding the slugs to 14 mesh. 13.~ g dry .~ Vitamin A Acetate and 0.6 g Vitamin D are then adde~ as bead-lets. The entire blend is then compressed using oncave punches at 0.5 9 each. .
. ,, Chewing of the resultant tablets yields a pleasant~
long lasting, consistently strong peppermint ~lavor for a period o~ 12 minutes. . .

' .

.. . . .

. . EX~PLE CLXI
.. CMEWING TOB~CCO
..

Onto 100 pounds of tobacco for chewing (85 percent Wisconsin leaf and 15 percent Pennsylvania leaf) the following casing is sprayed at a rate of 30 percent:
.' :: IngrPdients _ - Parts by Weight Corn Syrup . 60 . Licorice 10 Glycerine 20 Fig Juice 4.6 ~Prune Juice 5 Flavor Material of Example XCV 0.4 .
The resultant product is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistent~ long lasting . orange (20 minutes) nuance in conjunction with the main : . fruity tobacco note.
. . , ,_ . E ~PLE CLXII - -CHEWING TOBACCO
, . - .....
Onto 100 pounds of tobacco for chewing (85 .
. percent Wisconsin leaf and 15 percent Pennsylvania . . leaf) the following casing is sprayed at a rate of ~ . 30 percent:

,~ In~redients Parts by Weight .
Corn Syrup 60 _ Licorice 10 Glycerine 20 Fig Juice . ~.6 3Q Prune Juice 5 Flavor Material of Example XI A 3.4 The resultant product is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistent, long lasting clove-like (20 minutes) nuance in conjunction with the main fruity tobacco note~

~.
XAMPLE CLXIII
HEWING TOBACCO

Onto 100 pounds of tobacco for chewing (85 percent Wisconsin leaf and 15 percent Pennsylvania leaf) the Eollowing casing is sprayed at a rate of 30 percent:
' Inqredients _ Parts by Weight Corn Syrup 60 Licorice 10 Glycerine 20 Fig Juice 4O6 Prune Juice Flavor Material of Example XCIX 0.4 .` .~
The resultant pxoduct is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistent, long lasting cherry (20 minutes) nuance in conjunction with the main fruity tobacco note.
,,.- ' .-EXAMPLE CLXIV
, C~EWI~JG TOBACCO
Onto 100 pounds of tobacco for chewing (85 perent Wisconsin leaf and 15 percent ~ennsylvania leaf3 the following casing is sprayed at a rate of 30 percent:

Ingredients Parts by Weight Corn Syrup 60 Licorice 10 Glycerine 20 E`ig Juice 4.6 Prune Juice S , 3~ ~
`:`
; The resultant product is redried to a moisture content .` of 20 percent. On chewing, this tobacco has an excellent substantially consistent, long-lasting cherry (20 minutes) nuance in conjunction with the main fruity tobacco note.
. .

. ~ 3 -1~8-ExAr-~p-LE CLXV
CHEWING TOB~CCO
Onto 100 pounds of tobacco for chewing ~85 percent Wisconsin leaf and 15 percent Pennsylvania leaf) the following casing is sprayed at a rate of 30 percent:

Inqredients Parts by Weight Corn Syrup 60 Licorice 10 Glycerine 20 Fig Juice 4.
Prune Juice 5 Flavor ,~aterial of Example XX~V 0.4 The resultant product is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistentl long-lasting cherry (20 minutes) nuance in conjunction with the main fruity tobacco note.

EXAMPLE- CLX~I
CHEWING TOBACCO
., Onto 100 pounds of tobacco for chewing (85 percent Wisconsin leaf and 15 percent Pennsylvania leaf) the following casing is sprayed at a rate of 30 percent:

Ingredients ~ Parts by Weight . . . ~
Corn Syrup 60 Licorice 10 . Glycer ine - ~0 -. Fig Juice 4.
Prune Juice 5 ~lavor Material of Example XCV 0.4 . ... ._. .... ~ . __ The resultant product is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistent, long-lasting cherry (20 minutes) nuance in conjunction with the main fruity tobacco noteO

.' . . ..

,. -lg9~

EXI~MP L E CLXVI I -CHEWING TOBACCO

Onto 100 pounds of tobacco for chewing (85 percent Wisconsin leaf and 15 percent Pennsylvania leaf) the following casing is sprayed at a rate of 30 percent Ingredients _ _ Parts by Weight Corn Syrup 60 Licorice 10 Glycerine 20 Fig Juice 4O6 Prune Juice ~-~ Flavor Material of ~xample XCIX 0.4 The resultant product is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistent9 long lasting cherry (20 minutes) nuance in conjunction with the main fruity tobacco note.
.. . , .
EXAMPLE CLX~III
CHEWING TOBACCO

~0 Onto 100 pounds of tobacco for chewing (85 percent ~isconsin leaf and 15 percent Pennsylvania leaf) the following casing is sprayed at a r~te of 30 percent Ingredients Parts_by Weight Corn Syrup 60 Licorice l0 , Glycerine 20 ; Fig Juice 4J 6 ~~
Prune Juice 5 Flavor Material of ~xample C ( 100) _ 0.4 _ ,' ~ ' . .
The resultant product is redried to a moisture content of 20 percent. On chewing, this tobacco has an excellent substantially consistent, long-lasting cherry ~20 minutes~
nuance in conjunction with the main fruity tobacco note, .~ ~ ~ 3`7~3 : 200~ ~

. EX~IPI,E CLXIX
CHEWING TOBACCO
. ,, Onto 100 pounds of tobacco for chewing (85 percent Wisconsin leaf and 15 percent Pennsylvania leaf) the following casing is sprayed at a rate of 30 percent:

Ingredients Parts by Weight Corn Syrup 60 Licorice 10 Glycerine 20 : 10 Fig Juice . 4,6 Prune Juice 5 Flavor Material of Example CVI 0 4 : The resultant product is redried to a moisture content .
.~ . of 20 percent. On chewing, this tobacco has an excellent .: substantially consistent, long-lasting cherry (20 minutes) . nuance in conjunction with the main fruity tobacco note~.~ . .

~, ' . ,~

11 ~ I

-`

EXAMPLE CLXX
.,,..... ,,.. ~' The following mixture is prepared:

; Ingredient arts by Weight Orange oil.~ -O----OOO~ o~ o-48-4 Cab-O-Sil~M-5.. Oc......................... ~.OO 3.2 (Brand of Silica produced by the Cabot Corporation of 125 High Street, Boston, Mass. 02110, Physical Propertles:
1~0 Surface Area: 200 m2/gm Nominal Particle Size: 0.012 microns Density: 2. 3 lbs./cu.f~. ) anthan gum.... .O.... O.. ~..... I........... ..Oo 4.2 KLUCEL HF ( Brand of hydroxypropyl........ .....1.0 : . cellulose produced by the Hercules Corporation of Wilmington, Delaware ; having a molecular weight of 800,000 and a viscosity defined according to Figure 2) _ The Cab-O-Sil~ hydroxypropyl cellulose and xanthan gum are intimately ad~.ixed. The resulting mixture of Cab-O-Sil, ,~
xanthan gum and hydroxypropyl cellulose is dispersed in_the orange oil with viyorous stirring, thereby resulting in a vis-cous liquid. 48.4 Parts by weight of the powder flavor com~-osîtion of Example Q is then blended into the said viscous - liquid, with stirring at 25C for a period o~ 30 minutes result-ing in a thixotropic sustained release fl~vor paste.
.", . , ~ .
~ EXAMPLE CL~XI
.' .

The following mixture i5 prepared:
.,~ . .. . .
Ingredient Parts by Weight Liquid flavor composition of............... 20 Example A
Propylene glycol.... ,O.... ~O .l...... ~..... .2 Xanthan gum......... l.. ,............. O..... .8.0 KLUCEL~ EF ~Brand of hydroxypropyl......... .2.0 cellulose produced by the Hercules Corporation of Wilmington, De~aware having a molecular weight of 50,000 and a viscosity defined according to Fiqure 2) , . -202- .

The xanthan gum and hydroxypropyl cellulose are intimatley admixed. The resulting mixture of xanthan gum and hydroxy-propyl cellulose is dispersed in the liquid flavor compo-sition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 70 Parts by weight of the powder flavor composition of Example R is then blended into the said viscous liquid, with stirring at 25C for a period of 30 minutes resulting in a dr~, free flowing sustained release flavor powderO
..
, .10 . EXA~PLE CLXXII
.` .
~ The following mixture is prepared:
,' Ingredient Parts by Weight Liquid flavor composition of.......................... ~.O.... u.20 . Example A
.: Propylene glycol.... O....~ ..... O... ..~.... r. 1 . Xanthan gum......... O....,.......... ..~.... n. 3 Ethyl cellulose.......... ....... .... .~c....... 3 KLUCEL LF (brand of hydroxypropyl.......................... O. 1.0 . cellulose produced by Hercules Corporation of Wilmington, Delaware . ~ having a molecular weight of 100,000 . . and a viscosity defined according to Figure 2)_ _ , .' ---- O
The xanthan gum, ethyl cellulose and hydroxypropyl .
cellulose are intimately admixed. The resulting mixture . of xanthan gum, ethyl cellulose and hydroxypr~pyl cellulose . is then dispersed in the liquid flavor composition of Example A with vigorous stirring, thereby resulting in a viscous liquid. 65 Parts by weight of the powder flavor composition of Example R is then blended into the said viscous liquid, .; with stirring at 25~C for a period of 30 minutes resulting in a dry, free flowing sustained release flavor powder~

l .

- ~ 3 EX~IPLE CLXXIII

100 Parts by weight of chicle are mixed with 4 ~ parts by weight of the flavor prepared in accordance : with Example CLXX. 300 Parts of sucrose and 100 parts of corn syrup are added~ ~ixing is effected in a ribbon ' blender with jacketed side walls of the type manufactured by the Baker Perkins Co.
.
` The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
. The strips are cut into length of 3 inches each. On /~ chewing, the chewing gum has a pleasant long lasting r, orange flavor.
~,~ .
. E ~IPLE CLXXIV
, . . .
CHEWING GUM
,~
100 Parts by weight of chicle are mixed with 18 parts by weight of the flavor prepared in accordance with Example CLXXI. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured '.~! by the Baker Perkins CoO
., ,. . . .
The resultant chewing gum blend is then manufactured into strips 1 inch in width and 0.1 inches in thickness.
The strips are cut into length of 3 inches each. On chewing, the chewing gum has a pleasant long lasting cherry flavor.

' :, ' , ~ `
. .
. ~

-204-~

EX~PLE CLXXV
CHEwING Gur~
~ ., ~
100 Parts by weight of chicle are mixed with 4 ; parts by weight of the flavor prepared in accordance with Example CLXXII. 300 Parts of sucrose and 100 parts of corn syrup are added. Mixing is effected in a ribbon blender with jacketed side walls of the type manufactured by the Baker Perkins Co.

The resultant chewing gum blend is then manufactured - 10 into strips 1 inch in width and 0.1 inches in thickness.
; ~ The strips are cut into length of 3 inches each. On , chewing, the chewing gum has a pleasant long lasting -~ cherry flavor.
';` . ' ,,,,_ .j , . .' ' ' .
.` .
. .:....... . .

. . . . ' ' ,. ' "' ~, '. , ,.............. , . .

'` ~1 I
, ` ? .
. ' . .
. ._ . ,, ' . ~,

Claims

The embodiments of the invention in which an exclusive property or right is claimed are defined as follows:

1. A smoking tobacco or substitute smoking tobacco comprising a composition consisting essentially of:
a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil;
b. From about 3 up to about 7 parts by weight of a hydrolytically releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil;
c. From about 0.1 up to about 1 part by weight of hydroxypropyl cellulose, having a molecular weight of from about 50,000 up to about 800,000, whereby the physically entrapped flavor oil is suspended in the non-confined flavor oil, and shredded tobacco within which the resulting suspension is uniformly distributed whereby as the tobacco is smoked during the smoking activity, the flavor is released at a high flavor intensity substantially evenly and uniformly over an extended smoking activity time.

2. A smoking article comprising tobacco, a wrapper holding the tobacco in place and a filter in contact with said tobacco and said wrapper and in intimate contact with the filter or the wrapper or the tobacco a composition consisting essentially of:

a. From about 3 up to 7 parts by weight of a non-confined hydrophobic flavor oil, b. From about 3 up to 7 parts by weight of a hydrolyti-cally releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil;
c. From about 0.1 up to about 1 part by weight of a solid suspending agent selected from the group consisting of hydroxypropyl cellulose, colloidal silica, xanthan gum and ethyl cellulose, whereby the physically entrapped flavor oil is suspended in the non-confined flavor oil.

3. The smoking article of Claim 2, wherein the solid suspending agent is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000.

4. A process for augmenting or enhancing the aroma or taste of a smoking tobacco comprising the step of adding to smoking tobacco an aroma or taste augmenting or enhancing quantity of a composition consisting essentially of:
a. From about 3 up to 7 parts by weight of a non-confined hydrophobic flavor oil;
b. From about 3 up to about 7 parts by weight of a hydro-lytically releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil;

c. From about 0.1 up to about 1 part by weight of hydroxy-propyl cellulose having a molecular weight of from about 50,000 up to about 800,000, whereby the physically entrapped flavor oil is suspended in the non-confined flavor oil.

5. A composition comprising :
a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil;
b. From about 3 up to about 7 parts by weight of a hydrolytically releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil; and c. From about 0.1 up to about 1 part by weight of a solid.
suspending agent selected from the group consisting of hydroxypropyl cellulose, colloidal silica, xanthan gum and ethyl cellulose.

6. A composition consisting, in intimate admixture, of:
a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil;
b. From about 3 up to about 7 parts by weight of a hydro-lytically releaseable flavor oil physically entrapped in an edible solid material, selected from the group consisting of gum acacia, gelatin, modified food starch and dextrin, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil; and c. From about 0.1 up to about 1 part by weight of a solid suspending agent which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000.

7. A flavored heated beverage wherein the flavor is released at a high flavor intensity substantially evenly and uniformly over an extended period of time comprising an edible liquid capable of remaining in the liquid phase between 0°C and 100°C and intimately admixed therewith a composition consisting essentially of:
a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil;
b. From about 3 up to about 7 parts by weight of a hydrolytically releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil;
c. From about 0.1 up to about 1 part by weight of a solid suspending agent selected from the group consisting of hydroxypropyl cellulose, colloidal silica, xanthan gum and ethyl cellulose.

8. The beverage of Claim 7, wherein the non-confined hydrophobic flavor oil and the entrapped flavor oil are tea flavor or tea leaf extract.

9. The beverage of Claim 7, wherein the non-confined hydrophobic flavor oil and the entrapped flavor oil are lemon flavor oils.

10. The beverage of Claim 7, wherein the non-confined hydrophobic flavor oil and the entrapped flavor oil are coffee flavor or coffee bean extract.

11. The beverage of Claim 7, wherein the edible liquid comprises ethanol and water.

12. The beverage of Claim 11, wherein the ratio of ethanol:water is 1:1.

13. The beverage of Claim 7, wherein the edible liquid is water.

14. The method of preparing a flavoring comprising:
(i) Admixing a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil; and b. From about 0.1 up to about l part by weight of a solid suspending agent which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000 thereby forming a first suspension; and (ii) Admixing said first suspension with from about 3 up to about 7 parts by weight of a hydrolytically releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gum acacia, gelatin, modified food starch and dextrin, said solid material having a particle size of from about 5 microns up to about 400 microns thereby forming a second suspension, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil.

15. The method of preparing a flavoring composition comprising the steps of:
(i) Forming an aqueous solution of a solid flavor entrapment material selected from the group consisting of gum acacia, gelatin, modified food starch and dextrin;
(ii) Mixing therewith a first portion of a volatile, water immiscible first flavor oil thereby forming an emulsion;
(iii) Drying said emulsion thereby forming a solid flavoring agent having a particle size of from about 5 microns up to about 400 microns and containing entrapped hydrolytically releasable flavor oil;
(iv) Admixing a suspension agent which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000 with a portion of a non-confined hydrophobic second flavor oil organoleptically compatible with said first flavor oil thereby forming a first suspension; and (v) Admixing said solid flavoring agent with said first suspension thereby forming a second suspension, the weight ratio of said entrapped flavor oil :suspension agent being from 3:1 up to 7:0.1, and the weight ratio of said entrapped flavor oil:said second flavor oil being from 3:7 up to 7:3.

16. A chewing gum comprising particles of a composition consisting essentially of:
a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil;
b. From about 3 up to about 7 parts by weight of a hydrolytically releaseable flavor oil physically entrapped in an edible solid material selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil, c. From about 0.1 up to about 1 part by weight of a solid suspending agent which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000 and an all-enveloping mass of a chewable gum base within which said particles are substantially uniformly distributed whereby, as the chewing gum is chewed, the flavor is released at high flavor intensity substantially evenly and uniformly over an extended chewing time.

17. The chewing gum of Claim 15, wherein the non-confined hydrophobic flavor oil is selected from the group consisting of cherry flavor oil, lemon flavor oil, lime flavor oil, orange oil, peppermint oil and oil of wintergreen.

18. The chewing gum of Claim 16, wherein the flavor oil physically entrapped in the edible solid material is selected from the group consisting of:
a. Cherry oil physically entrapped in modified food starch;
b. Cherry oil encapsulated in gelatin capsules;
c. Cherry flavor oil entrapped in gum acacia;
d. Lemon oil physically entrapped in modified food starch;
e. Lemon oil encapsulated in gelatin capsules;
f. Lemon flavor oil entrapped in gum acacia;
g. Lime oil physically entrapped in modified food starch;
h. Lime oil encapsulated in gelatin capsules;
i. Lime flavor oil entrapped in gum acacia;
j. Peppermint oil physically entrapped in modified food starch;
k. Peppermint oil encapsulated in gelatin capsules;
l. Peppermint flavor oil entrapped in gum acacia;
m. Oil of wintergreen physically entrapped in modified food starch;
n. Oil of wintergreen encapsulated in gelatin capsules;

o. Flavor oil of wintergreen entrapped in gum acacia;
p. Orange oil physically entrapped in modified food starch;

q. Orange oil encapsulated in gelatin capsules;
r. Orange flavor oil entrapped in gum acacia;
s. Cherry flavor oil entrapped in dextrin;
t. Lemon oil encapsulated in dextrin;
u. Lime flavor oil entrapped in dextrin;
v. Peppermint flavor oil entrapped in dextrin;
w. Oil of wintergreen entrapped in dextrin; and x. Orange flavor oil entrapped in dextrin.

19. The chewing gum of Claim 16, wherein the composition has additionally added thereto from 0.03 up to 0.07 parts by weight of propylene glycol.

20. The method of preparing a chewing gum comprising:
(i) Admixing a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil; and b. From about 0.1 up to about 1 part by weight of a solid suspending agent which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000, thereby forming a first suspension;

(ii) Admixing said first suspension with from about 3 up to about 7 parts by weight of a hydrolytically releaseable flavor oil physically entrapped in an edible solid material, selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about 5 microns up to about 400 microns thereby forming a second suspension, said physically entrapped flavor oil being organoleptically compatible with said non-confined hydrophobic flavor oil; and (iii) Substantially uniformly distributing said second suspension within an all-enveloping mass of a chewable gum base.

21. The method of preparing chewing gum comprising the steps of:
(i) Forming an aqueous solution of a solid flavor entrapment material; selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch;
(ii) Mixing therewith a first portion of a volatile, water immiscible flavor oil thereby forming an emulsion;
(iii) Drying said emulsion thereby forming a solid flavoring agent having a particle size of from about 5 microns up to about 400 microns and containing entrapped hydrolytically releasable flavor oil;
(iv) Admixing a suspension agent therewith which is hydroxy-propyl cellulose having a molecular weight of from about 50,000 up to about 800,000 with a portion of a non-confined hydrophobic second flavor oil organo-leptically compatible with said first flavor oil to form a first suspension;
(v) Admixing said solid flavoring agent with said first suspension thereby forming a second suspension, the weight ratio of said entrapped flavor oil:suspension agent being from 3:1 up to 7:0.1, the weight ratio of said entrapped flavor oil:said second flavor oil being from 3:7 up to 7:3; and (vi) Substantially uniformly distributing said second suspension within an all-enveloping mass of chewing gum base.

22. The method of preparing an orally utilizable composition comprising:
(i) Admixing a. From about 3 up to about 7 parts by weight of a non-confined hydrophobic flavor oil; and b. From about 0.1 up to about 1 part by weight of a solid suspending agent which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000, thereby forming a first suspension;

(ii) Admixing said first suspension with from about 3 up to about 7 parts by weight of hydrolytically releaseable flavor oil physically entrapped in an edible solid material, selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch, said solid material having a particle size of from about; 5 microns up to about 400 microns thereby forming a second suspension, said physically entrapped flavor oil being organo-leptically compatible with said non-confined hydrophobic flavor oil; and (iii) Substantially uniformly distributing said second suspension within a base for said orally utilizable composition.

23. The method of preparing an orally utilizable composition comprising the steps of:
(i) Forming an aqueous solution of a solid flavor entrapment material; selected from the group consisting of gelatin, dextrin, gum acacia and modified food starch;

(ii) Mixing therewith a first portion of a volatile, water immiscible flavoring oil thereby forming an emulsion.

(iii) Drying said emulsion thereby forming a solid flavoring agent having a particle size of from about 5 microns up to about 400 microns and containing entrapped hydrolytically releasable flavor oil;
(iv) Admixing a suspension agent therewith which is hydroxypropyl cellulose having a molecular weight of from about 50,000 up to about 800,000 with a portion of a non-confined hydrophobic second flavor oil organoleptically compatible with said first flavor oil thereby forming a first suspension; and (v) Admixing said solid flavoring agent with said first suspension thereby forming a second suspension, the weight ratio of said entrapped flavor oil:suspension agent being from 3:1 up to 7:0.1, and the weight ratio of said entrapped flavor oil:said second flavor oil being from 3:7 up to 7:3; and (vi) Substantially uniformly distributing said second suspension within a mass of the base for said orally utilizable composition.

24. The process of Claim 22, wherein said orally utilizable composition is a toothpaste.

25. The process of Claim 22, wherein the orally utilizable composition is a chewable vitamin tablet.

26. The process of Claim 22, wherein the orally utilizable composition is a chewing tobacco.

27. The process of Claim 23, wherein the orally utilizable composition is a toothpaste.

28. The process of Claim 23, wherein the orally utilizable composition is a chewing tobacco.

29. The process of Claim 23, wherein the orally utilizable composition is a chewable vitamin tablet.

30. The process of Claim 22 or 23, wherein the base is selected from the group consisting of chewing gum, chewable vitamin tablet base, chewing tobacco and toothpaste base.