CA2479058A1 - Edible films including aspartame and methods of making same - Google Patents

Abstract

Methods of producing edible thin film products and products so produced are provided. The method comprising the steps of: adding to a film formulation a food grade acid; and adding aspartame to the film formulation and acid.

Description

"EDIBIr,» FILMS INCLUDING A,SkARTAME ~I~ Iv~THODS OJF MAY~TNG
~9!
~~A L .
13ACKGROUI~A Op' THE INVENTION
The present invention generally relates to edible film compositions. More specifically, the present invention relates to edible films with inczeased stability_ Aspartame has been used as am artificial, low calorie sweetener in numerous food, cosmetic, a»d pharmaceutical cvznpositions. Aspartame is a very attxaetive sweetener due to xt$ intensity and because very Iow levels can be used tv achieve a high swee~ess perception by the consumer. It is noted for its clean, sweet taste that resembles sucrose. Aspartame has recently become a desirable sweetener to employ iGn edible film products.
Edible I'xlm groducts are designed to adhexe to azxd rapidly dissolve in the mouth of the consumer. Edible films cant provide Ilavor ar~dlor oral care agents, e.g., breath freshening to the consumer. Such films typically include a :film former and flavor or other iz~gredierct. See, for example, U.S. Patent No. 5,948,430 and U.S.
Applicatioia publication No. US2001/Oa22964 AI.
Edible f [~, pxoducts are usually provided to the consumer in sta-ip form. The strips are sized so that they can be placed o~n the tone of a consuiz~er. rn this regard., the edible film strips typically have a size of a postage Stamp yr slightly Iargez. These strips pzeferably hava a supple texture and are non-self adhering.
Ono type of edible film product is distributed by Pfizer Consumer klealtheare under the name ListerineG~ PocketPaksTM. The 1?;hzer edible film product is packaged in a plastic container that includes a top that can open along a hir~gc. A
stack of strips are located in an interior of the paelcage one on lop of aztother. The package is 515485/DlT FNCTO1_ s desig~zed so that the cansurxter can open tlae container azxd remove ozte strip from the stack with his or her fAngeT.
Edible fzim products aze also disclosed izt Assignee's co-pending U.S. parent application "Rolled Edible Thin Film Products and IV~ethods of Making Same,"
Fled on August 27, 2002, bearing x.1.5. Serial No. 101228,742.
Attempting to ixtcorporate aspartame in an edible film results in a less than satisfactory product. The aspartame cant become unstable> yielding an xrrferior, Iess flavorful product. The ~ instability of aspartame is primarily due to tine nature of asparta~cze itself; its erystaIlirte structure and configuration. Aspartame has historically exlxibited difficulty in rs~aintaining its strucrure in complex, heterogeneous environments. In pazticular> aspartame has two major disadvantages. 1~izst>
aspartame becomes unstable under acidic conditions, and extaibits rapid degradation wherx exposed to elevated tezztpEratures. Secozxdly, the peptide nature of aspartazrze makes it susceptible to hydzalysis; this featufe also causes other reactions and microbial degradation.
Aspartame has previously dernoustrated instability izt other products, such as chewing gums. Sugarless chervxztg gums often cozttain flavors aztd hygroscopic compoztents that arc usually saturated with aldel~ydes that contribute to the instability of aspartame. The compozxents of a chewing guzza matrix generally yield a product having a pkZ of about ~.5. At this p~f, aspartame beeome;s unstable.
Similazly, the production of edible films also provide a complex rnatrxx of ingredients and processing parameters that aid in rendering aspartame unstable.
Therefore, there is a need far an edible frlmi product including aspaz~tame that.is stable.
SUMMARY OF THE IN~V~E1V'~'ZON
The present irtvetation provides an edible ,filrxx pz'oduct with increased aspartame stability due to the incorporation of acid into the film far~ulation during processing.
sxsassmrr a=r~c~rm_ 1.t has been surprisingly discovered that by incorporati>3g . aczds into the film coating syrup dt~ning processing and maintaining a pH range o~F about 4.5 to about 6,0, tl~e aspartame will not denature in the final film carnpositiota, despite the high processing temperatures to which the film is exposed. !, In accordance with the present xz~.vention, a variety of methods of foizning a thin edible flm can be used. Ozte rzrethvd includes the st4~ps of. adding filrn_forming materials togethez- with water and agitating sarrae until tlae powder is preferably hydrated and few lumps are present. To this mixture, plasticizers, softening agents, colors, sweeteners, cooling agents, flavors and active ingredients can be blended together to form a homogeneous solution.
It should be ranted that err acid may be added at anytime before aspartame is included into the mixture. Itr a pzefexxed embodiment, the acid is incorporated aver water has been added to the film forming materials to ztaal~e the coating syrup. In an embodiment of the process, a coatinb syrup with acid is then fed into a hopper, and spread onto a maving slebstrate through a drying tmuael in which it is exposed to high processing temperatures a~.~d exits the dzying system as a dried, edible fitF.n. Upon exiting the drying system, the filrrx may be rolled, cut, stamped, etched, etc., to yield the desired film form.
Irl an eznbodimeat of the present invention, at least one food grade acid is added to the coatxzrg syzup.
In an embodiment, the acid is added to the coating syrup before water is added.
1n an embvdirnent, the acid is added to the coatxz~g sy~p after water is added.
In an embodiment, the acid is added to mixing lank before: other ingredients are added.
SF5485/D/1 FNCTOI, In an embodiment of the present invention, the acid is chosen froze the group consisting of phosphoric aczd; citric acid; make acid, acetic, adipxe, benzoic, butyric, formic, furnaric, hexanoic, lactic, propavnic, succinic, tartaric, carbonic, attd sulforic.
In still another embodiment of the pz~esent invention, tl~e acid is encapsulated.
In an errzbodiment, the acid is spray dxied.
In an ernbodizrzent, the pH of the coating syrup is between 4.7 and 5.~
In an embodiment, the pH oFthe coat~g syrup is between 4_5 and 6Ø
In an embodiment of the present invention, the acid maintains the stability of the aspartame in the edible film con3positiozt during processing.
rn arr embodisner~t, the edible film compositiozt comprises at least one polysaccharide.
In anoEhcr cmbodirn~ez~t, the edible film composition comprises at least one filrta-forming agent drat is a water-soluble non-starch polysaccharide.
In an embodiment of the present invention, the film-forming ageztts include a polysaccharide and a softener.
In an ernbodim~ent of the prcsezrt invention, the polysaccharide is pullulan.
lrt another embodiment of the present invention, the hltn product is a vehicle for delivering active agents to a consumer.
In a fiuthe~r eznbodisnent of the present invention, a method for preparing a rolled ~lrn is provided cornprisiag the steps of forming a rnixture of at least one film forming or coatixtg syrup material in powder form with a food grade acid and water;
agitating the mixture preferably unizl the powder is txxostly hydrated and few lumps remain; adding to the mixture at least one ingredient selected from the group Go~5I5tlIig of-. plasticizers, softening agents, colors, sweeteners, cooling agetxts, flavors su4asmn ~cTO~_ and active ingredients; blending the mixture to obtain a homagerteous solution;
spreading the solution onto a moving substrate; drying the solution an the substrate to create a flexible ftlm.; a~,d winding the film onto a take-up roll- .
In an embodiment, a method for preparing a rolled film is pifovided comprising forming a mixture of at least one .film-fvztning material in powder fornn and water, agitating the mixture until the powder is mostly hydrated and few lumps remain, adding to tlxe mixture at least one ingredient selected from plastieizws, solfiening agents, acids, colors, sweeteners, cooling agents, flavors and active ingredielat$, then adding aspartame, blending the mixture to obtain a homogeneous solution, spreading the solulzon vzztv a moving substrate, drying the solution on tk~e substrate to create a flexible film and winding the film onto a tape-up roll.
It is an advantage of the present inverttior~ to pzovide improved edible f lms.
Another advantage of the present aravention is to provide a him corrtpositiott including an acid that maintains the stability of aspartame during pzocessing.
Moreover, an advantage of the preseztt invention is to provide an improved method ofmanufacturxzrg edible film products.
Still, an advantage of the present invention is to provide tua, edible film product including aspartame.
Another advazttage of the pzesezit izzventzort is to enhance the flavor of the edible film_ Additionally, an advantage of the present invention is to provide methods for stabilizing aspartame.
Furthermore, an advantage of the present iztvez~txor~ is that iv can be :implemented by making relatively xniz~or modifications to an Otherwise Conventional process.
515485/D/1 FNCTOi_ Additional features and advantages of the present inventiozl are d~se~bed in.
and will be apparent in, the detailed desc~ption of the presently preferred embodiments.
DETAILEI? ;DIrSCRIPTION OF THIS INVEl~'TION
'flxe present xzlventioa provides stable edible txlzn formulataor~so containing aspartame, through the: addition of acid to the film composition. Moreover, the present invention provides methods for manufacturing edible films eoataining aspartame.
It has been surprisingly found to be advantageous during thin film processing tv add acid to the film formulation. Pursuant to the present inventioxi, aspartame containing stable, flavoz~ul edible thin films can be formed by a variety of difFei-ent processes.
One such process xs as follows: (I) as adueous solution is formEd by blending film-forrzzizlg materials to$othc~r with water and acid arid are agitated until the powdered materials are prefezably mostly hydrated and few lumps are present;

(2) to ttus mixture, plastieizers, softening ageTlts, colors, sweeteners, cooling agents, and active ingredients are blended together to form a horxaogeneous solution; and

(3) this solution is then cast auto a sutable carrier, and dried to fon~n a film. It should be noted that no particular order is placed on inevrporadclg the ingredients into tIze mixture;
howwer, xt,is importarxt that the acid is included izt the solution before the aspartame is added. Tt should also be noted that a wide variety of film formulations or coating 5yriip5 Carl be used.
As part of the process, preferably, a carrier is used to produce edible fihns.
T~xe cannier material should be irctperr~cieable to the ;elm coating, allowing the film coating to disperse evenly oztto the carrier and allowing for the ease of removal of the film from the carrier. hxamples of suitable carriers include plastic or polyester films, polypropylexte, polycarbonate, nva-siticonizcd polyethylene terephthalate Film, .non-smaasrm rrc~'ot_ 6 siliconized Kraft paper, polyethylene irtap~eegnated Kraft paper, metal belts, voltage yr corona treated belts, drum dryers, and polytetxaflurve2hylene-impregnated glass fabric.
A particularly preferred method of casting the fllr'ta on the carrier is tluough a slot die extrusion- By use of mu2tiple .extrudErs and specially constructed dies, it is possible to add nnultiple color stripes to the p~oduCt. It is also possible tv oscillate the dze head tv produce wavy Lines on ttxe product. The resulting films eau be laminated to produce various visual ~ffeets.
The casting of the solution onto a suitable carrier material catr be performed using any conventional coating technique. Examples of coating teclrniques include spraying, dipping, comma coatefis, l~nife over plate, roll aver roll, reverse roll, slot die extrusion, and various extrusion techniques. Fihxr thiclmess can be controlled by adjusting the gap on the coating head, or by applying the desired amount of the solution onto the substratelcarrier. No particular liruitation is placed an the thiclrness of the film layer. The thickness of the hlm may vary, or a mufti-layered film product may be processed, depending o~z the desired speed of dissolution o;f the edible Fim while in the oral cavity.
After coating, the film passes through a dryer for moisture reduction. Drying is carried out through a variety vl"different mesas, such as high velocity turbulent hot air, conduction from steam located slide bed, direct heating or casting o~ film onto a heated drum or belt, hot or cold six xznpingErnent, infrared heating, oz~ any other suitable drying eyupmertt tlxat dues not adversely affect the components of the film.
Once the film exits the drying system, the dried film is either taken-up along with its substrate or peeled i~-om the carrier to form a wide roll. As the film exits the drying system, it can be exposed tv a number of different types of treatments.
If desired, the film may be sprxztlsled with sugar, starch, flavor, color, color enhancers such as glitter, acids, bioadhesives, actives and texturizexs such as candy sprinkles to make specialty edible ftlrz~ products that may be desirable to younger consumers.
sisassran ~vcTOi_ After the palm has bees dried arad treated as desired, it may be cut, stamped, etched, punched, etc" into its final chosen sate and form. For example, the edible filir~
can be a rolled edible filrt~_ Rolled edible films and methods of making the same are disclosed in U.S. Patent Application Serial t~tv. It?/228,742, entitled "Rolled Edible Thin Film Products and Methods of Making the Sajne," filed on August 27,2002, the disclosure which is incorporated herein by reference.
The formulations of the present inventiozz may be used to generate "specialty"
films that can be produced at various poizzts during the f~lzn making process.
For example, those concepts which appeal to younger consumers. Types of specialty filnrt products include, but are not limited to films that are mufti-flavoring, mufti-layering, mufti-coloring, mult~i-shapes or foruzs, texturizing, larninatizrg, printing, graphical designs, "tongue-tattoos°°, oral sensations, varying dissoiuzion pxofiles, bioadhesive components, within the oral mueosa of a consumer; alone or in combinations thez~evf.
The films of the present invention are also suitable for food applications beyond direct consumption.
Any suitable water-soluble, film-formex can be used to produce a rolled edible thin film product, Suitable Flm-formers include, but are not limited tv, water-soluble non-starch polysaccharides such as modified eelIuloses, carboxymethylcellulose (CMC), methylcellulose, hydroxypropylrrmthylcellulose (HI'MC), hydrolyzed gums, xanthan gum, guar gum, locust bean gum, tamarind, agar agar, carrageenau, algins, gum arabic, ghatti gurn, Karaya gum, Oragacanth gum, konjac, arabxzzvgalactan, larch arabinogalactan, beta-glucan, propylene glycol, pullulan, levan, elsinazi, pullulan, pectins, curdlan, chitosatz; native starches such as turn starch, waxy maize starch, high-amylose corn starch, potato, tapioca, rice and wheat starch; modified starches sueb as those that have been acid modified, bleached, oxidized, esterified, ethcrified, crossZxzxked, and treated enzymatically; starch hydz~olyzed products such as maltodextrin: protein such as gelatin, casEin. salts of casein, whey, and protein, derived from soybeans; polymers such as polyvinyl pyrrolidone, methycrylate copolymer, and carboxyvinyl eopolyrz~ers alone or in any combinativzt. Iii an embodiment, the 5154&S!D/1 f'NC'f01_ concentration of the film-forming agent constitutes between approximately 5%
to about 60% by dry weights, or approximately 20% to abut 40% by dz7r weight of the hzral film composition. Further, it slavuld be noted that some ftIm forming agents, such as sodium alginate, will have an impact on the ~H of the edible film composition.
i Fiu ther, any suitable food-grade bulk filler can also be added to the elm.
This cav reduce any "slimy" texture as well as provide structure io the film making it more palatable. In an erabodizactetit, the tiller can constitute approximately I%
to about 30%
by dry weigt3t of the film, ar approximately 5% to about 15% by dry weight of the fzlzzt, The filler can include microcrystalline cellulose, cellulose polymers, such as wood, magnesitun and calcium carbonate, ground limestone, silicates, such as magnesium and alurnitzurn silicate, clay, talc, titanium dioxide, mono-calcium phosphate, di-calcium phosphate, tri-calcium phosphate, other like bulk fillers or combinations thereof_ I,f it is desired to use reduced levels of f Inx forming agents; sofleneTs coat also be employed to ensure the flexibility of the film, thereby reducing b~ttleraess. The softetaers, which are also lrnowrz as plasticizers, may include tallow, hydrogenated tallow, hydrogenated and partially hydrogenated vegetable oils, cocoa butter, sorbitol and other polyols, glycerin, polyethylene gtycoJ, propylene glycol, invert sugars, corn syrup, lecitl~izt, hydrogenated lecithin, mono-, di- and trxglycerides, acetylated monoglycerides, fatty acids (c.g. stearic, palmitic, oleic, and linoleic acids), arid eornbinations thereof. In an embodiment, the so,~er~ex cdrr constitute 0% to about 20%
by dry weight of the film, or approximately 2% to about 10% by dry weight of the Film.
Another means of controlliztg the brittlencss of the frlm as to maintain an adequate moisture level in the hlm. Preferably, moisture levels should range from approximately 5°/q to about 20°/a or approximately 10°/V
to about l5% of brie final him product.
sis4as~Dn ~cTO~_ g Pursuant to the preseztt invention, a variety of acids can be used to maintain the stability of the aspartame during processing or to enhance the flavor of the filrtx. These acids include, but, are not litnitcd to malic, fumarie, adipie, succinc, citric, acetic, lactic, pyruvic, butyric, foz~,ic; xsociiric, Iactocitric, shikirnic, quir>ic, oxalic, glyceric, citraznalie, glyeolic, ghxeuronic, galacturoinc, aspartic, benzoic, lactarimic, cctostearic, allantoic, pyroglutamic, hydrochloric, bexanoic, carbonic, sulfuric, pyrrolidinonecarboxylic, and tartaric. Further, acids may be added to impact the flavor of the producf. For exanxple, malic acid is commonly associated with apples, citric acid with lemons, and tartaric acid with grapes_ However, mixtures of different acids may be used in combination to create a desired taste or flavor. Further, t~tese acids may be encapsulated to control their rate of zelease and interaction witkr the other components of the f lm matrix.
A variety of other suitable ingcdiezits cars be added to the edible flin of the present invention. For example, any suitable r~aedicament for oral clcansirng:
breath Freshening or the like can be added to the .film formulation. The medicaments can xz~ctude, for example, pH control agents, tartar, caries control, whitenatxg agerlts>
enzymes, breath freshening agents, anti,plaque/anti-gingivitis agezats, saliva stimulating agents, pharmaceutical agents, nutxaceutical agents, vitamins, mineral, otlZer like rnedieaments or combinations thereof ' The: edible rIm fortn,ulations or coating syrups o,f the present invention can also include colorants or coloring agearts that can be used in any suitable amount to produce a desired color. Further, the rolled films of the present izzvention, if desired, can include colored stripes and/or other related desigrAS or shapes to produce color contrasts on the edible rolled film. Colaring agents can include, for example, natural.
food colors and dyes suitable for food, drug, and cosmetic applications. The colorants are typically known as FD&C dyes and lakes-1~ variety of flavoring ageztts can also be added to the edible frlms. - Any suitable amount and type of artificial andfoz' ztatural flavoring agents can be used izt any sensorxally acceptable fashion. Far example, the flavor can constitute approximately s~5assmn r-r~cro~_ 10 O.lp/° to about 20% by dry weight of the film, preferably approxircaately 10% to about 15%. T'l~e flavoring agent can include, for example, essential oils, synthetic favors or r~zixtures including but not limited to ails derived from plants and fruits such as citrus oil, fruit essences, peppermint oil, : spearmint oil, other mint oils, clove oils, oil of wintergreen, anise and the like, favor oils with germ killing properties such as rraezzthol, eucalyptol, thyrriol, like flavotzng agents or combinations thereof.
The flavor can be enhanced and distributed evenly throughout the product by emulsi$catiozi, Any suitable amount and type of natural and/or synthetic food-grade emulsifier can be used. JFor example, the emulsifier can include lecithin, :Coed-grade non-ionic emulsifiers, such as fatty acids (C,o C,g), mono and diacyl glyeerides, ox bile extract, polyglycervl esters, polyethylene sorbitan esters, propylene glycol, sorbitan monopalmitate, sorbitan tristerate, other like emulsifiers or combinations thereof:
The flavors can be emulsified by any suitable emulsircatioti process, such as mechanical processing, vigorous stirring, intense pressure fluctuations that occiu- in turbulent flow such as homogenization, sotufieation, colloid milling acid the like.
,~urth~r, flavors may also be encapsulated or spray dried onto the rolled edible f'thn product to enhazice flavor properties or to add texture tv the f lm eomposidon.
Any siutable anriount of sweetening agents may also be employed for the present xzzvention. Sugar sweeteners generally include saechuride-cvzttaining cornpozients including but not li~ziting to, sucrose, dextrose, maltose, dextrin, invert sugar, ficuctvse, levulase, galactose, corn syrup solids, and the like, alone or i~~ any combination. Sugarless sweeteners z~zclude, but are not limited to, sugar aIcohvls such as sorbitol, manztitol, xylitol, isomalt, hydrogenated starch hydrolysates, riialtitol, and the Iike, alone vain any combination. ~Towever, the low weight of the Flan picoducts of tlae present invention generally tender these low intensity sweeteners ineffective for purposes of sweetening although t)xey nnay provide ft~netxvz~al benefits.
I-la~, intensity xrcificial sweeteners arc preferably used. alone or in coriibination with the above. Preferred sweeteners include, but are not li~riited to, sueralose, s~sassmn rrrc~roa_ ~ 1 aspartame, N-substituted AFM derivatives such as neota,ztte, salts of acesulfame, alitamc, saccharin and its salts, cyclamic acid and its salts, glycyrrhizin, dihydrochalones, tlzaumatin, monellin, and the life, alone or in any combination. In order to provide enhanced yr d~:layed swaetncss, or to provide texture to the roaled film i product, it may be desirable tip encapsulate the sweetener. Such teehniclues as wet granulation, wax granulation, spray drying, spray clxilling, fluid bed coating, cvacervation. and fiber extension may be used to achieve the de5xred cl~araeteristies_ Combinations of sugar and/or sugarless sweeteners may be used in the film pzoduct. Additionally, a softening agent may also provide additional sweetness such as with aqueous sugar or alditol solutions.
Cooling agents may also be employed in the present invention, cooling agents include, but are not Iiznited tv> menthol, WS3, WS2~, Utzacool, monomenthyl suceinate, alone or in any combination. Again, tk~ese cooling agents may be encapsulated or spray dried onto the film to enhance a variety of oral sensations.
Depending on the ingredierts being used to make the film pzvduct, preservatives may also be employed to ensure the s~ety and quality of the edzbae thin film. Suitable preservatives include but are not Limited sorbic acid, svdaum, benzoaee, potassiur~z sorbate, methyl p-hydroxyber~zoate, sodium propionate, and propyl p-hydroxybenzoate alone or in any combination. In addition, suitable antioxidants can be used.
It should be appz~eciated Lbat any suitable type, number and arrar~gezrnent of process procedures or sups (e:g. mixing, heating, dryiz~,g, cooling, addition of ingredients), process parameters (e.g: terrapezature, pressure, pFl, process times) yr the like can be utilized to practice the present invention.
~3y way of example and not limitation, exarcaples of tlxe present invention will now be given-s~s4ssrDn rNCTOV_ 12 Edible Filar Prepa>ratiou Method:
1:) Blending:
a a) Powdered materials tsuch as film forming agents) are blended together using a. ribbon blender or equivalent b) Flavors or flavor components/cnhancers are blended together using mecha~ica,1 agitation or equivalent.
2) Mixing:
a) 'fhe mixing tank is turned on and set at desired temperature.
b) To the mixilng Lank the blended powdered materials are added.
c) Water is added to the mixing lank, and begin agitation of the mixing uank.
d) When alI water has been added, the desired acid is added.
e) Once all bleztded powders and acid have been added to the mixing tarok, sweeteners, flaVOrs, cvlvxs, etc. are added as the temperature rises. The blend is maintained ai an even temperature, about 105 to about 115°F.
Tire conditions of the mixing room are maitatained at about 70 to about 80°F, 40 to about 50% RH.
3) Drying:
a) Feed solutivzt into a hopper.
b) Upon entering the drying system; the film solution is coated onto a moving substrate which passes under a coma bar roll to produce a dry thiclrness of about 48 to about 52 microns.
515485/D! I I~CTa 1 c) ,A,djust the beater temperature to achieve ara exit film terzagezatwe of about 215 to about 220°F. This should produce a Flm havir~~ a moisture of about 9 to about 11 %.
d) ( Drying room conditions are about 70 to about 80°F, 40 tv about 50% RH.

4) C~ltting/Slzaping a) The film is removed from the substrate upon exiting the drying system and taken up on a separate roll. Unee the rolled deed Flm cools and sets, it is unwound and cut into its desized final lfvrrn_ Through quality assurance testing, it was discovered that after the edible films ltad been processed, tlae loss of aspartame was in a range of about 20 to about ~0% in the dal product after processuig. Several tests were run, incorporating acid into tfle filu~ composition in order to decrease or stop the losses of aspartarrie in the final film pxoduct. ~'he formulas used and the results from the tests rtxn are as follows:
Fi~zished Wei~Zt rngredieut Cvutroi Coulparative Example x Alginate 32.0 x'7.0 Maltodex?rin J 7.0 17,p Garrageenan 12.0 a 2.0 Cellulose 10.0 10.0 Glyce~"in 8.5 8.S

Aspartame 1.0 1.0 Citric Acid -- 0.15 .Flavor 8.0 8.0 ~.w...

5J5485/Dh FriCT01_ 14 menthol 1.5 1.5 Water 10.0 9.85 2"otul 100.0 ' 100.0 r Test 1:
A syrup holding test was conducted to dernonsrrate aspartame de~adation in the holding tazdt before the solution was processed attd dried to forrrt the final film product. Syrup was made with and without citric acid and placed in an oven at 125 to about 133°k'. Samples of syrup were taken at 0, 2lxr, Shr, 24hr, 4$hr, and 76hr.
Aspareame levels were tested, and the results arc as follows:
Time of SamplingCo~atrol ~:a;arrrrple x (hrs.) (/v Aspartame (lV Aspartame Retalped) Retained) T = 0 I00v/o 100%

T= 1 92.0% d 00.0%

T= 5 87.0% X8.0%

T= 24 G I .U% 92_O%

T= 48 44.0% 8I .0%

'f= 76 34.0/v 73/v The data above demonstrates a significant retention of aspartame while in acidic solution over time. The contzol sample experia~zced a GG% loss of aspartame over a 76 hour period of tine. In contrssC, ~x~unple 1 (contaitun ; citric .acid) experienced only a 27% loss of aspartame over tk~e given period of time.
515485/DI1 F'NC3'oi_ 1$

Test Z
Dried syrup (final Eim product), was also tested for aspartame levels in the fxzushed pzoduct. .Kandom samples were taken off the dried film role in the begizminb, middle, aid end regions of the roll. Aspartame levEls were determined froxu each region, and results ,are as follows:
Sampling region of Control Example 1 the roll (% Asparta~nac (% Aspartame R,etx~iucd) Retained) Begiruiing 76/Q 100%

Middle 66% 1 OU%

End 40% 98%

'flze data above demonstrates a significant loss of aspartame over tizne (approxzzxaately 5 hours to complete the entire processing razz). The control sample experienced a 60% loss of aspartazzze over the five hour period, whereas Example 1 (containing citric acid) onl~r Lost 2% aspartame.
Tlae following examples illustrate some ennbodiments of the invention. Qf course, zrtay others are possible and arc easily Formulated by a skilled technician once ahe fuzadamez~taI concepts of the invention arc grasped.
5154851D1i F'I~tCT01_ 16 (% Finashed'OVt.) Ingredieat ~, Ea.2 Ex.3 Ex.4 Eac.S Ex.6 Ex.7 Corn Starch 24.8 -- -- 30.0 -- --F,lydroxyprvpylatrd- -- .- -- -- 47.35 Starch Carrageenan . 14.0 I2.p 10.0 - 9.0 --Glycerin 10.0 $.0 - 5_0 9.0 7.50 Gelatin - -- 12.0 S.0 -- 2.50 Microcrystalline 3.0 7.0 -- 5.0 8_0 --Cellulose Sodaumc~ A.lginxtc - 25.0 10.0 5_0 30.0 ?2,0 Maltodemrin -- X0.5 -- -- 18.0 -Pallnlan 6.0 -- 39-0 - - --Sorbitol 35_0 - -- 5.0 -- --Liquid Sorbitol -- -- - I O-0 - --tl,cesullamie ~ - -- -- -- -- 1.0 Sacralosr - 1.45 1.U 1.0 -- 1 _25 Aspartame I -50 -- 2.0 -- 2.0 --WS-3 - I.55 - I _0 -- --WS-23 -. -- 2.0 -_ __ -_ Menthol -- 6_0 1.0 -- 3.0 ' 1.0 Spearmint __ -. __ __ 6.0 __ Cherry Flavor 15.0 5.0 -- F2_0 - _ Ptppc~-nniatt~ _ __ __ __ 6.U __ )vwcalyptol - -- -- - -- 6.00 S15a8S1pi1 FriC't'O1_ I7 Methyl Salicylate - 4.$ IO_0 _ _ ._ Citric Acid __ 0.1 -- 5.0 I .0 _.

Adipic .Acid -- __ l ,p __ __ 1.00 ~'l~osphvric 0-2 0.1 - -- _ __ Acid Cvlor ~ 0.50 O.SO -- 0-SO 0.35 0.X0 Water 10.0 8.0 12.0 1S_S 7.65 10.0 Tertal 100.0 100.0 100.0 100-0 100.0 100.0 SISaBSIOI~ FNCTOi_ Ingredient Ea.8 Ea.9 I:a.lO' E~.11 Ea.l2 Fx.l3 I3yd: oxyethylated Starch-- ~i8.0 .- -_ _. __ PURt~-COTE~ >8790* 50.0 -_ _,. __ __ __ Enzyme Flydrotyzed Corn -- -- 22.0 -- - --Stare6 Maltodextrin -- -- 5.0 28.0 -- --Casein -- 2.9 - -- 3.S -~'ullulnn _ __ ._ __ 20.0 35.0 Polyvinyl Pyrollidane -- 11.0 -- -- 6_0 --~

Hydroaypropylmcthylcetlotosc- -- -- -- 30.0 --Xanthan Guut -- -- -- -- -- 6.0 Locust l3aan Cum -- -- -- -- -- 8.0 Glyerin -- -- -- 12.0 9.5 10,5 kolyctl~yteue Glyeot - -- -- -- 6.0 --Propylene Glycol 1.50 -- i 0.0 -- G.0 --Carrageenan - 11.0 - 10.0 -- 24.7 Sodium Alginate -- - -- i3.75 -- -.

Calcium Al~in~atr ~ 22.9 -- -- ~. -- -SilfCa -- -- -- 5.0 -- -Calcium Carbonate - -- 3.0 -- - --~CCtjdt 4,0 - -- _.. - __ l~ccithi~z - 2-0 1-0 1.5 __ _ Saccharin - __ _- .. __ 2.0 A,spartamc 0.25 -- - 1.0 1.5 _..

Sucralosc 1.25 -- -- -- -- --s~sassrn~~ r~~To~_ 19 Neota~ue -- -- 0.50 -- ).S --Encapsulated Acesuif-.~a~e -- -- 1.5 -- 1.0 --K

15_0 Corn Syrup . _- ._ __ _ l '. Guar Gam -- 2.0 -- -- -- --Sorbitan Moaopalsr~itate -- -- -- -- 4.0 --Ultracool - -- -- 1.2 -- 5.0 .

Citrie Acid - -- -- 1.5 -- --Adipic Acid _. _- -_ 1.5 .- .-JV~ethy! Salieylate -. ' __ .. -- _ 1.S

EucaIyptol -- 6.0 -- -- -.. 0.5 iI"Atymol -- _- 2.8 -_ _ 0.5 Encapsulated Peppermint -- -- -- -- 1 i.0 --Mcrrtlaot -- -- 8_0 -- 4_0 I_5 Lert~oa Flavor 10,0 -- -- 8.0 -- --Mixed Berry Flavor -- 5.0 -- 8.0 --Fumaric ,A,cid 1.0 005 - 0.1 -- --Tartaric Acid -- -- 0.1 U.1 -- 0.30 Citric Acid -- -- 0.1 0,1 I.0 --Color 0.05 0-OS 0.50 0.25 -- 0.5 ~Vntcr 9.05 12.0 10.5 8.0 15.0 4.0 'Total 100.0 100,0 100.0 100.0 100,0 100_0 'k PURE-COTE~ B'79fl g Corporation is a produet of the (Gl'C), Grain Processin located is Muscatine, Iowa. PITRE-CVTE~ ash-d7ried rch designed B'79fl ruodilied spacitacally is corn a sta fl for applicotions 1'cyuiriag very low viscosity.

515dR5ipli FNC-fUl_ ~o Irag~r~edient Ex, Ea. Ea. h,~. fix. h~s.X8 ~x.~9 ELK.
13 1~ 15 lb 17 2 Ilydroxypropylccllulosc~S-0 -- , -- - -- -- 18.0 -Waxy Maize Starch - -- -- -- - -- 15.0 --Potstv Starch 2.0 -- 29.5 -- -- .- .. ..

JPuIfulan . 26-0 8.0 -- 55.0 .. .. -.

Microcrystalline Cetlalose- -- I O.U 6.5 -- 8.0 -- G.5 Sorbitaa Fatty Acid -- 1.0 -- -- -- 3.0 --Ester Matiodexiri><a - 19.0 - 2p,0 -- 28-0 -- I9-0 Carrage~nan -- 16.0 -- 10_0 -- 8_0 1.5 10.0 Gclatir~ 7.0 __ __ ._ Z.0 __ .. ._ PolyYinyl Alcoiiot 5.85 -- _. -_ _ _- _ _-Sodium I'olyacryl:dte 5.0 -- - -- -- - ~ -- --Csa~rb4xyrnethylccllulose5_0 -- -- -- -- -- -- -Xantban Cu -- 3.0 -- -- -- -- - --Karsya Gum 3.5 -- -- -- 6-U -- -Glycerin _- __ G.0 -- 4.5 _. 6.0 '1'itaniam Dioxide . -- 2.0 __ ._ .. 2.S __ Sodium Al~inmc - -- -- 25.0 2.0 20.5 13.0 19.0 Sorbitol - -- 1.5 - -- 0.05 -- --Encapsulated Aspartpme -- -- -- -- ~- -- 1.0 --Suc=atone - -- -- -- -- 1.5 1.0 3.0 Corn Syrug _ _- 15.4 _- .- ... .. __ Soybean Oal - - I.0 - __ __ __ _ Lecitbin - -- -- I.5 0.5 0.50 - 1.5 515a8Slplf FNCTOI_ Z1 Dextrv5e __ _ Z.0 .- __ __ _. _ ~ruciose - 9.5 _. __ $.0 .. _. ._ 'WS-3 - 2.9 .. D -0 -- - 4.0 0.5 Clove Oil - -- 1,0 -- 4.5 - -. -_ tYlenthol 8.0 2.U -- 2_0 -- -- 1.0 O,S

Grape Flsvor - -- -- -- -- -- 12_0 5.0 Lemon Blavor - _ __ __ __ 5.0 _- __ Rose Oil __ Z.0 -- - .. __ I,p ._ Pepper - 2.0 -- -_ __ __ _- __ O~'~nge ~'tavor -- -- 3.0 -- -- 4.0 2_0 _.

Peppcra~int OiI .. - -- 9.0 5.0 2.0 -- --Cardamom 8.0 2.0 .. __ _ 1.0 __ __ Crapeseed E:tract - -- -- 5.2 Z.S -- -- -Tea Catecltixts - .. .. __ __ I.0 __ __ Yitattnia C ._ __ 3.0 -- 2_S __ 5.0 9_9 Vitamin .A,B,D,E Comglex. .. __ __ __ .. .. 5.0 Zinc Glucv~ate - - -- -- -- -- 5.0 1.0 Suecinic Acid -- 0.2 - -- -- 1.S -- 0.001 Ts~rtaric Acid 0.15 -- -- 1-0 -- -- -- 3-0 Eacapsutated Citric 0.3 Z,0 - -- 5.0 S.0 --Acid Ecttinacea - - 3.0 -- 2.5 1.0 -- --~

CetyI Pyridinium Cltloside3.0 .. -- -- __ __ _ ._ Encapsulated Caffeine - 5.0 -- -- -. _. __ __ Sodium Bcnzonatc ..- -- 2_0 0.5 -- -- -_ 315485/D/I f'NCTQt_ u.
)<iFiA - -- 0.5 -- 0,0s _. __ Color 0.5 0.1 O.G 0.30 0,5 0,80 0.1 0.1 WRter 7.0 10.0 17.0 10.0 11.5 7.6 ~:9 9.999 Total 100.0 100.0 , 300,0 100,0 100,0 100.0 100.0 100,0 s~saxsmn rNCn'o~_ ~3 It should be appreciated that various changes axtd mod~i~eations of the presently preferred etnbodxmer~ts described herein will be apparent to those skilled in the art_ Such chang4s at~d modifications can be axxadE without departing from the original spirit and scope of the presezct invention without diminishing its intended advantages. It is therefore intended that such changes and modificarions be covered by the apper~de~d clairr~s_ s~sassrnr~ ~cTO~_

Claims (47)

The invention is claimed as follows:

1. A method of producing edible thin film products comprising the steps of:
adding to a film formulation a food grade acid; and adding aspartame to the film formulation and acid.

2. The method of Claim 1 wherein the food grade acid is added to the film formulation before water is added.

3. The method of Claim 1 wherein the food grade acid is added to the film formulation after water is added.

4. The method of Claim 1 wherein the food grade acid is chosen from the group consisting of: phosphoric acid, citric acid, malic acid, acetic, adipic, benzoic, butyric, formic, fumaric, hexanoic, lactic, propionic, succinic, tartaric, carbonic, and sulforic.

5. The method of Claim 1 wherein the food grade acid is encapsulated.

6. The method of Claim 1 wherein the food grade acid is spray dried.

7. The method of Claim 1 wherein the film formulation with acid has a pH
of 4.5 to about 6Ø

8. The method of Claim 1 wherein the film formulation with acid has a pH
of 4.7 to about 5.4.

9. The method of Claim 1 wherein the film formulation includes at least one polysaccharide.

14, The method of Claim 1 wherein the film formulation includes pullulan.

11. The method of Claim 1 comprising the step of casting the film formulation and acid using a coating technique.

12. The method of Claim 11 wherein the coating technique is chosen from the group consisting of: spraying; dipping; comma cutters; knife over plate;
roll over roll; reverse roll; and extrusion.

13. The method of Claim 11 comprising a drying step niter casting.

14. The method of Claim 11 comprising a roll take up step after casting.

15. A method of producing edible thin films comprising the steps of:
producing a coating syrup that does not include aspartame;
adding to the coating syrup an acid;
adding aspartame to the coating syrup and acid; and producing edible film from the coating syrup, aspartame, and acid.

16. The method of Claim 15 wherein the acid is added to the coating syrup before water is added.

17. The method of Claim 15 wherein the acid added to the coating syrup after water is added.

18. The method of Claim 15 wherein the acid is chosen from the group consisting of: phosphoric acid, citric acid, malic acid, acetic, adipic, benzoic, butyric, formic, fumaric, hexanoic, lactic, propionic, succinic, tartaric, carbonic, and sulforic.

19. The method of Claim 15 wherein the acid is encapsulated.

20. The method of Claim 15 wherein the acid is spray dried.

21. The method of Claim 15 wherein the coating syrup with acid has a pH
of 4.7 to about 5.4.

22. The method of Claim 15 wherein the coating syrup includes at least one polysaccharide.

23. A method of Claim 15 wherein the coating syrup includes pullulan.

24. The method of Claim 15 wherein the edible film includes an active agent.

25. The method of Claim 15 wherein the edible film includes a medicament.

26. The method of Claim 15 comprising the step of passing the coating syrup through an extruder.

27. The method of Claim 15 comprising the step of casting the film formulation and acid using a coating technique.

28. The method of Claim 27 wherein the coating technique is chosen from the group consisting of: spraying; dipping; comma cutters; knife over plate;
roll over roll; reverse roll; and extrusion.

29. The method of Claim 27 comprising a drying step after casting.

30. The method of Claim 27 comprising a roll take up step after casting.

31. A, method for preparing a rolled film is provided comprising the steps of:
forming a mixture of at least one film-forming material in powder form with a food grade acid and water;
agitating the mixture;

adding to the mixture at least one ingredient selected from the group consisting of plasticizers, softening agents, colors, sweeteners, cooling agents, flavors and active ingredients, blending the mixture to obtain a homogeneous solution;
spreading the solution onto a moving substrate;
drying the solution on the substrate to create a flexible film; and winding the film onto a take-up roll.

32. The method of Claim 31 wherein the film includes a medicament.

33. The method of Claim 31 wherein the film includes an active agent.

34. The method of Claim 31 wherein the acid is added to the coating syrup before water is added.

35. The method of Claim 31 wherein the acid is added to the coating syrup after water is added.

36. The method of Claim 31 wherein the acid is chosen from the group consisting of: phosphoric acid, citric acid, malic acid, acetic, adipic, benzoic, butyric, formic, fumaric, hexanoic, lactic, propionic, succinic, tartaric, carbonic, and sulforic.

37. The method of Claim 31 wherein the acid is encapsulated.

38. The method of Claim 31 wherein the acid is spray dried.

39. The method of Claim 31 wherein the coating syrup with acid has a pH
of 4.7 to about 5.4.

40. The method of Claim 31 wherein the coating syrup includes at least one polysaccharide.

41. The method of Claim 31 wherein the coating syrup includes pullulan.

42. The method of Claim 31 wherein the edible film includes an active agent.

43. The method of Claim 31 wherein the edible film includes a medicament.

44. The method of Claim 31 wherein an extruder is used.

45. The method of Claim 31 comprising the step of casting the film formulation and acid using a coating technique.

46. The method of Claim 45 wherein the coating technique is chosen from the group consisting of spraying; dipping; comma cutters; knife over plate;
roll over roll; reverse roll; and extrusion.

47. The method of Claim 31 comprising a drying step after casting.