EP0821886A2 - Method of providing aromatic compounds from tobacco - Google Patents
Method of providing aromatic compounds from tobacco Download PDFInfo
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- EP0821886A2 EP0821886A2 EP97113000A EP97113000A EP0821886A2 EP 0821886 A2 EP0821886 A2 EP 0821886A2 EP 97113000 A EP97113000 A EP 97113000A EP 97113000 A EP97113000 A EP 97113000A EP 0821886 A2 EP0821886 A2 EP 0821886A2
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- Prior art keywords
- tobacco
- suspension
- dust
- tobacco material
- process according
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
Definitions
- the present invention relates to methods for providing flavor and aroma substances, i.e. flavor additives, for tobacco materials, cigarettes and other smoking articles.
- Popular smoking articles such as cigarettes, have a substantially cylindrical rod shaped structure and include a charge of smokable material, such as shreds or strands of tobacco material (i.e., in cut filler form), surrounded by a paper wrapper, thereby forming a tobacco rod. It has become desirable to manufacture a cigarette having a cylindrical filter element aligned in an end-to-end relationship with the tobacco rod.
- a filter element includes cellulose acetate tow circumscribed by plug wrap, and is attached to the tobacco rod using a circumscribing tipping material.
- Many cigarettes include processed tobacco materials and/or tobacco extracts in order to provide certain flavorful characteristics to those cigarettes.
- natural tobacco flavors and aromas are important for the taste, aroma, and acceptance of smoking products, including substitute smoking materials.
- search for natural tobacco flavor additives or flavor substances is a continuing task.
- U.S. Patent No. 3,424,171 describes a process for the production of a non-tobacco smokable product having a tobacco taste.
- Tobacco is subjected to a moderate (i.e. below scorching) heat treatment i.e., at from about 175° to 200°C (350° to 400°F), to drive off aromatic components.
- a moderate (i.e. below scorching) heat treatment i.e., at from about 175° to 200°C (350° to 400°F)
- the smokable product disclosed is vegetable matter, treated with the mixture of tobacco aromatic components and the solvent.
- U.S. Patent No. 4,150,677 describes a process for the treatment of tobacco which comprises the steps of: (1) contacting tobacco which contains relatively high quantities of desirable flavorants with a stream of non-reactive gas, under conditions whereby the tobacco is heated in a temperature range from about 140° to 180°C; (2) condensing the volatile constituents of the resulting gaseous stream; and (3) collecting said condensate.
- the condensate may be used subsequently to flavor a smoking material in order to enhance the organoleptic qualities of its smoke.
- British Patent No. 1,383,029 describes a method of obtaining tobacco aroma substances which comprises an extraction treatment wherein the components of the tobacco that are soluble in a suitable solvent are extracted and the residue is obtained after removing the solvent is subjected to heat treatment at a temperature from 30° to 260°C.
- U.S. Patent Nos. 5,038,802 to White et al. and 5,016,654 to Bernasek et al. disclose extraction processes which heat tobacco and then pass an inert atmosphere through the heating chamber to collect volatiles from the tobacco. The volatiles are then fractionated in downstream operations, which include liquid sorbents, cold temperature traps, and filters.
- U.S. Patent No. 5,235,992 to Sensabaugh proposes a process that involves heating tobacco (e.g., in a flowing gas stream) during a first staged heating to a first "toasting" temperature to drive off volatile materials, increasing the toasting temperature during a second staged heating, and separately collecting, as flavor substances, at least portions of the volatile materials driven off at the first and second toasting temperatures.
- U.S. Patent No. 5,121,757 to White et al. proposes a process for altering the chemical nature of a tobacco extract, in which tobacco material is extracted with a chemical solvent, the extract is contacted with an ammonia compound, and the ammonia-treated extract is subjected to heat treatment in a pressure-controlled environment (e.g., in a Parr bomb).
- flavorful and aromatic substances can be produced from tobacco materials previously thought to have little commercial value, for example, tobacco dust from the cigarette manufacturing process, without having to first perform extraction procedures on the materials.
- Other sources of tobacco dust can be used, such as finely ground tobacco leaves and stems.
- the flavorful and aromatic substances produced by the invention described herein possess aromatic qualities, total volatile profiles and individual volatile component profiles that are comparable to flavorful and aromatic substances obtained from the more time-consuming and resource-intensive extraction/heat treatment methods of the prior art.
- the present invention generally relates to a process for the production of natural tobacco flavor substances useful in tobacco smoking products as flavor substances, and in tobacco substitute materials as a source of tobacco smoke flavor and/or aroma.
- the process of this invention produces suspensions having a complex mixture of volatile, semi-volatile, and non-volatile aroma/flavor components that are products of the Maillard reactions.
- tobacco in the form of finely divided particles is produced from tobacco material and is mixed with an aqueous liquid to produce a tobacco suspension.
- This suspension is subjected to heat treatment in a pressure controlled environment (e.g., a Parr bomb) under conditions sufficient to alter the chemical nature (e.g., the flavor and aroma characteristics) of the finely ground tobacco material.
- a pressure controlled environment e.g., a Parr bomb
- the tobacco suspension is exposed to a temperature sufficiently high and for a period of time sufficiently long so as to provide an increase in aroma/flavor compounds.
- it is preferable that the tobacco suspension not be exposed to such a high temperature for a sufficiently long period of time so as to provide an aroma/flavor which exhibits a burnt or tarry aroma/flavor.
- the finely ground tobacco material can be contacted with an aqueous liquid to comprise a tobacco suspension.
- the tobacco suspension should have sufficient aqueous liquid such that a liquid phase is present in the suspension.
- the tobacco suspension can be 80% or less solids. More preferably, the suspension contains less than 50% solids and most preferably contains between 10% and 25% solids.
- a tobacco suspension can include tobacco material in a dust or powder form contacted with an aqueous liquid further comprising additives (e.g., amino acids, amino acid analogs or amino acid sources or other nitrogen sources, and/or sugar or sugar sources).
- the present invention more particularly relates to a process of producing a natural tobacco flavor or aroma by first contacting finely ground tobacco material with an aqueous liquid to provide an aqueous ground tobacco material suspension, which suspension is then subjected to heat treatment at a temperature above about 100°C in a pressure controlled environment.
- the ground tobacco material suspension has a tobacco content of at least about 5 percent by weight, preferably at least about 10 percent by weight, and more preferably at least about 25 percent by weight, when the suspension is exposed to the moderately high temperature treatment.
- the pressure experienced by the ground tobacco material suspension is greater than ambient (i.e., atmospheric) pressure.
- tobacco content relates to the weight of the finely ground tobacco material within the ground tobacco material suspension relative to the total weight of the tobacco suspension.
- the ground tobacco material suspension normally is subjected to such treatment in order that the entire suspension is exposed to a temperature above about 100°C for at least about 10 minutes.
- flavorful and aromatic compositions are useful as casing or top dressing components for tobacco laminae and cut filler, as well as for other smokable material.
- flavorful and aromatic compositions are useful in those types of smoking articles described in U.S. Patent Nos. 4,708,151 to Shelar; 4,714,082 to Banerjee et al.; 4,756,318 to Clearman et al.; and 4,793,365 to Sensabaugh; as well as European Patent Publication Nos. 212,234 and 277,519.
- the flavorful and aromatic compositions are also useful as cigarette filter additives.
- the flavorful and aromatic compositions can be incorporated into low density polyethylenes and formed into strands, and then incorporated into cigarette filters as described in U.S. Patent Nos. 4,281,671 to Byrne et al. and 4,862,905 to Green, Jr. et al.
- the flavorful and aromatic compositions are also useful as cigarette wrapper additives; or as additives to the inner regions of cigarette packages (e.g. within a paper/foil laminate of a cigarette package or within a low density polyethylene film which is placed within a cigarette package) in order to provide a desirable cigarette aroma and "pack aroma.”
- Flavor compounds produced by the methods of the present invention have organoleptic qualities and volatile content qualities that are comparable to those compounds produced by solvent extraction of natural compounds and heat treatments thereof.
- tobacco materials formerly discarded as waste products of the manufacturing process may be used as starting materials in the process of the present invention to yield flavorful aromatic substances that are also comparative in concentration and desirable organoleptic qualities as other tobacco starting materials.
- Tobacco dust represents a significant portion of tobacco material lost during the manufacture of cigarettes.
- the present invention provides a heretofore unknown use for tobacco material as a source for aroma and flavor components for the manufacture of smoking articles and the like.
- FIG. 1 is a schematic diagram of process steps representative of an embodiment of the present invention.
- tobacco material 10 is subjected to grinding 15 to produce a finely ground tobacco material dust or powder 20 .
- finely ground material refers to materials composed of particles that are less than 10 mesh, preferably less than 20 mesh, and most preferably are less than 40 mesh (standard sieve size).
- the tobacco material may already be in dust form such that additional grinding is not necessary (i.e., the starting tobacco material is already finely ground).
- the preferred tobacco material is a dust or powder, other types of tobacco can be used, such as cut filler, strips, stems or leaves.
- the finely ground tobacco material is then contacted 55 with an aqueous liquid (e.g., water) 60 to provide an aqueous tobacco suspension 70 .
- aqueous liquid e.g., water
- This aqueous tobacco suspension is then placed in a pressure controlled environment 30 , subjected to heat treatment 35 , and cooled 40 .
- the treated tobacco suspension is then collected 50 for use.
- the tobacco materials useful herein can vary. Tobacco materials which are used are of a form such that upon grinding, the resulting ground material is in the form of finely divided particles. Examples of suitable tobaccos include Burley, Flue-Cured, Vietnamese, Latakia, Maryland Cigar, as well as the rare or specialty tobaccos, or blends thereof. Unaged, uncured, mature or immature tobaccos may also be employed. Tobacco waste materials such as fines, dust, scrap, stem, and stalk can be employed. In one preferred embodiment of the present invention, the tobacco material comprises a cigarette manufacturing by-product known to the skilled practitioner as cigarette dust. The aforementioned tobacco materials may be processed separately, or as blends thereof.
- the tobacco material may be subjected to various means to reduce its size, such as grinding, such that the resulting tobacco material is in finely ground or powder form.
- various grinding techniques will be apparent to one skilled in the art, and may include the use of e.g., ball mills or hammer mills.
- the grinding may also be carried out under vibrating or agitating conditions, the selection of said conditions being within the skill of one in the art.
- the tobacco suspension may be provided in a number of ways.
- the finely ground tobacco material may be contacted with a liquid having an aqueous character, thus providing an aqueous ground tobacco material suspension.
- a liquid having an aqueous character consists primarily of water, normally greater than about 90 weight percent water, and can be essentially pure water in certain circumstances.
- a liquid having an aqueous character can be distilled water, tap water, or the like.
- a liquid having an aqueous character can include water having substances such as pH buffers, pH adjusters, organic and inorganic acids, bases and salts, or sugars, amino acids or surfactants incorporated therein.
- the liquid also can be a mixture of water and minor amounts of one or more solvents which are miscible therewith (e.g., various alcohols, polyols or humectants such as glycerin or polypropylene glycol).
- solvents e.g., various alcohols, polyols or humectants such as glycerin or polypropylene glycol.
- the tobacco content of the suspension may be at least about 5 percent of the total suspension by weight, preferably at least about 10 percent by weight, and more preferably at least about 25 percent by weight.
- the tobacco suspension can also be contacted with at least one amino acid, amino acid analog or amino acid source (e.g., glutamine, asparagine, proline, alanine, cystine, aspartic acid, phenylalanine, glutamic acid) and at least one sugar or sugar source (e.g., fructose, sucrose, glucose, maltose).
- amino acid, amino acid analog or amino acid source e.g., glutamine, asparagine, proline, alanine, cystine, aspartic acid, phenylalanine, glutamic acid
- sugar or sugar source e.g., fructose, sucrose, glucose, maltose
- flavoring agents e.g., cocoa, licorice, St. John's bread, spices, herbs, and the like
- the tobacco suspension is subjected to moderately high temperature treatment such as described in U.S. Patent No. 5,060,669 to White et al., the disclosure of which is incorporated herein by reference in its entirety.
- moderately high temperature treatment involves exposing the tobacco suspension to a temperature above about 100°C, preferably above about 110°C, and more preferably above about 120°C.
- the moderately high temperature treatment of the tobacco suspension can be performed under an inert atmosphere.
- nitrogen and argon gas can be employed in order to provide an inert atmosphere.
- the heat treatment can be conducted under ambient atmosphere (i.e., air).
- the moderately high temperature treatment is performed in a pressure controlled environment.
- a pressure controlled environment is provided by enclosing the tobacco suspension in an air sealed vessel or chamber.
- a pressure controlled environment is provided using a pressure vessel or chamber which is capable of withstanding relatively high pressures.
- Such vessels or chambers (i) provide enclosure or concealment of the tobacco suspension such that volatile flavor components of the tobacco suspension are not lost or do not otherwise escape during the moderately high temperature treatment step, and (ii) provide for treatment of the tobacco suspension at a temperature significantly above about 100°C.
- Preferred pressure vessels are equipped with an external heating source. Examples of vessels which provide a pressure controlled environment include a high pressure autoclave from Berghof/America Inc. of Concord, California, and Parr Reactor Model Nos.
- Typical pressures experienced by the tobacco suspension during the process of the present invention in such vessels range from about 10 psig to about 1,000 psig, normally from about 20 psig to about 500 psig.
- the amount of time that the tobacco suspension is subjected to the moderately high temperature treatment can vary. Normally, the time period is sufficient to heat an entire tobacco suspension at the desired temperature for a period of at least about 10 minutes, preferably at least about 20 minutes. Normally, the time period is less than about 3 hours, preferably less than about 1 hour, and most preferably about 30 minutes.
- Conditions provided during the process of the present invention most desirably are such that certain components of the tobacco suspension (e.g., free amino acid pools and naturally occurring sugars) undergo the Maillard Reactions.
- the Maillard Reactions or "browning reactions” are reactions between (i) the amino substituents of amino acids, peptides, proteins or other nitrogen-containing compounds, and (ii) the carbonyl group of a sugar in the reducing form or other carboxyl-containing compounds which are indigenous or added to the tobacco suspension.
- Such reactions result in a significant darkening of the tobacco suspension, typically to an extremely dark brown color. See, Maillard, Ana. Chim. , Vol. 9, pp. 5 and 258 (1916); Hodge, J. Agric. Food Chem ., Vol. 1, p. 928 (1953); Nursten, Food Chem ., Vol. 6, p. 263 (1981) and Waller et al, ACS Symp. Ser . (1983).
- the treated tobacco suspension is useful in the manufacture of smoking articles. They may be added to conventional cigarettes or other smoking articles as a top dressing, or casing, or in any convenient mode selected by the manufacturer.
- the amount of the treated tobacco suspension employed per cigarette or smoking article can vary. For example, in a typical cigarette having about 0.6 to about 1 g per rod of smoking material, about 10 to about 100 ppm of the compound can be used as a top dressing or casing.
- the treated tobacco suspension may be used as a filter flavor material for a cigarette.
- the suspension may be used to provide flavor/aroma to any of the forms of material that are used in the manufacture of tobacco products such as cigars, cigarettes, smoking tobacco or snuffs.
- mg means milligram
- ⁇ g means micrograms
- g means grams
- L means liters
- mL means milliliters
- min means minutes
- mm millimeters
- Tobacco in the form of cigarette dust was ground on a SWECO vibrating ball mill (SWECO Inc., Los Angeles, CA USA) until it was reduced to a very fine powder.
- SWECO Inc. Los Angeles, CA USA
- 150 g of the ground cigarette dust was mixed with 1350 g of water. This suspension was reacted in a sealed Parr bomb at 175°C for 30 minutes. After a rapid cooling to ambient temperature, the remaining pressurized volatiles were released and the liquid was removed from the Parr bomb. A very aromatic aroma was observed coming from the liquid. This procedure was repeated with the starting materials of Burley tobacco dust, flue-cured tobacco dust, and Turkish tobacco dust.
- Tobacco in the form of cigarette dust was ground as described in Example 1. 375 g of the ground tobacco material was mixed with 1125 g of water to provide a suspension. This suspension was reacted in a Parr bomb at 175°C for 30 minutes. After cooling and venting as described above, a very powerful aroma was noted. This procedure was repeated with the starting materials of Burley tobacco dust, flue-cured tobacco dust, and Turkish tobacco dust.
- the samples were each preheated at 70°C for 5 minutes prior to being swept for 10 minutes with a stream of helium at 40 mL/min.
- the sample temperature was held at 70°C.
- the volatiles were trapped on a Tenax (TEKMAR) trap and were then thermally desorbed onto the GC column set at 10°C by heating at 180°C for 5 minutes.
- the TEKMAR headspace system was directly interfaced with to a Hewlett-Packard 5880 gas chromatograph (GC) equipped with a DB 1701 fused silica column (J&W Scientific, Folsom, CA) 30 meters long, 0.32 mm inner diameter, and 1 micron film thickness.
- GC Hewlett-Packard 5880 gas chromatograph
- the outlet of the column was split between a flame ionization detector (FID) and a mass selective detector (MSD) operating in the electron impact mode at 70 V.
- FID flame ionization detector
- MSD mass selective detector
- the GC injection port, the MSD interface, and the FID detector were set at 250°C.
- the column oven was programmed from 10°C to 47°C at 2°C per minute followed by 10°C per minute to 240°C.
- the FID area counts for cyclohexanone were employed in the calculation of the amount of each identified volatile component.
- the volatile components were identified from both mass spectral library search routines and GC retention time databases.
- each identified volatile components from the cigarette dust, Burley tobacco dust, flue-cured tobacco dust, and Vietnamese tobacco dust is presented as an average concentration of the component over five samples, in ⁇ g/mL.
- each identified volatile component from the four kinds of dust used is presented as an average percentage distribution of the component over five samples.
- C2 pyrazines mean pyrazines with 2 carbons attached (e.g., dimethylpyrazine);
- C3 pyrazines mean pyrazines with 3 carbons attached (e.g., ethylmethylpyrazines);
- C4 pyrazines mean pyrazines with 4 carbons attached (e.g., ethyldimethylpyrazines).
- a tobacco blend was prepared containing about 20 parts Burley tobacco, 55 parts flue-cured tobacco, and 25 parts Oriental tobacco, in the form of tobacco strips.
- the strip blend dry weight was approximately 2400 gm.
- a suspension of heat-treated tobacco dust was added to this blend of tobacco strips.
- the suspension contained 10% tobacco dust and 90% water by weight (about 150 grams of tobacco dust and 1350 gm of water).
- the tobacco strips' final weight was about 2550 gm and contained 150 gm of the heat-treated tobacco suspension (approximately 5.8% by weight of the strip blend.)
- the strip blend was cut at 32 cuts per inch at a moisture of approximately 18%.
- the cut filler was dried to approximately 13% in a heated pill coater drum.
- 2040 gm (40 parts) of expanded flue-cured tobacco cut filler and 510 gm (10 parts) of cut-rolled expanded stems were added to this blend of cut filler material.
- the final blend was top-dressed with 1.5% by weight of glycerine containing a small amount of flavoring.
- the tobacco cut filler was used to prepare cigarettes that were 88 mm in length (57 mm tobacco rod wrapped with RJR Ref. 456 paper (Ecusta Corp., Pisgah Forest, NC, USA) and a 27 mm shaped acetate filter from Filtron International Ltd. (Great Britain, code SAF).
- the cigarettes were ventilated at approximately 13 mm from the mouth-end. The average ventilation was about 55%.
- a total of five cigarettes were prepared in this manner, as follows:
Abstract
Processes for producing flavorful and
aromatic compounds from tobacco material are provided.
The processes involve subjecting finely ground tobacco
material to heat treatment at a temperature above
100°C, while the finely ground tobacco material is
enclosed in a pressure controlled environment.
Preferably, the finely ground tobacco material is
provided as an aqueous tobacco suspension, which
suspension is then heat-treated in a pressure
controlled environment.
Description
The present invention relates to methods for
providing flavor and aroma substances, i.e. flavor
additives, for tobacco materials, cigarettes and other
smoking articles.
Popular smoking articles, such as cigarettes,
have a substantially cylindrical rod shaped structure
and include a charge of smokable material, such as
shreds or strands of tobacco material (i.e., in cut
filler form), surrounded by a paper wrapper, thereby
forming a tobacco rod. It has become desirable to
manufacture a cigarette having a cylindrical filter
element aligned in an end-to-end relationship with the
tobacco rod. Typically, a filter element includes
cellulose acetate tow circumscribed by plug wrap, and
is attached to the tobacco rod using a circumscribing
tipping material. Many cigarettes include processed
tobacco materials and/or tobacco extracts in order to
provide certain flavorful characteristics to those
cigarettes.
Many types of smoking products and improved
smoking articles have been proposed through the years
as improvements upon, or as alternatives to, the
popular smoking articles. Recently, U.S. Patent Nos.
4,708,151 to Shelar; 4,771,795 to White et al;
4,714,082 to Banerjee et al; 4,756,318 to Clearman et
al; and 4,793,365 to Sensabaugh, Jr. et al; and
European Patent Publication Nos. 212,234 and 277,519
propose cigarettes and pipes which comprise a fuel
element, an aerosol generating means physically
separate from the fuel element, and a separate mouth
end piece. Such types of smoking articles provide
natural tobacco flavors to the smoker thereof by
heating, rather than burning, tobacco in various forms.
Generally, natural tobacco flavors and aromas
are important for the taste, aroma, and acceptance of
smoking products, including substitute smoking
materials. Thus, the search for natural tobacco flavor
additives or flavor substances is a continuing task.
For example, U.S. Patent No. 3,424,171
describes a process for the production of a non-tobacco
smokable product having a tobacco taste. Tobacco is
subjected to a moderate (i.e. below scorching) heat
treatment i.e., at from about 175° to 200°C (350° to
400°F), to drive off aromatic components. These
components are trapped on adsorbent charcoal, and
removed from the charcoal by solvent extraction. The
smokable product disclosed is vegetable matter, treated
with the mixture of tobacco aromatic components and the
solvent.
Similarly, U.S. Patent No. 4,150,677
describes a process for the treatment of tobacco which
comprises the steps of: (1) contacting tobacco which
contains relatively high quantities of desirable
flavorants with a stream of non-reactive gas, under
conditions whereby the tobacco is heated in a
temperature range from about 140° to 180°C; (2)
condensing the volatile constituents of the resulting
gaseous stream; and (3) collecting said condensate.
The condensate may be used subsequently to flavor a
smoking material in order to enhance the organoleptic
qualities of its smoke.
British Patent No. 1,383,029 describes a
method of obtaining tobacco aroma substances which
comprises an extraction treatment wherein the
components of the tobacco that are soluble in a
suitable solvent are extracted and the residue is
obtained after removing the solvent is subjected to
heat treatment at a temperature from 30° to 260°C.
U.S. Patent Nos. 5,038,802 to White et al.
and 5,016,654 to Bernasek et al. disclose extraction
processes which heat tobacco and then pass an inert
atmosphere through the heating chamber to collect
volatiles from the tobacco. The volatiles are then
fractionated in downstream operations, which include
liquid sorbents, cold temperature traps, and filters.
U.S. Patent No. 5,235,992 to Sensabaugh
proposes a process that involves heating tobacco (e.g.,
in a flowing gas stream) during a first staged heating
to a first "toasting" temperature to drive off volatile
materials, increasing the toasting temperature during a
second staged heating, and separately collecting, as
flavor substances, at least portions of the volatile
materials driven off at the first and second toasting
temperatures.
U.S. Patent No. 5,121,757 to White et al.
proposes a process for altering the chemical nature of
a tobacco extract, in which tobacco material is
extracted with a chemical solvent, the extract is
contacted with an ammonia compound, and the ammonia-treated
extract is subjected to heat treatment in a
pressure-controlled environment (e.g., in a Parr bomb).
While these processes have produced flavor
substances acceptable for use in many smoking articles,
they have either not been suitable for some smoking
articles, or have necessarily required the forming of a
tobacco extract prior to the obtaining of the desired
compound. Additionally, many of these processes
necessarily required expensive or inabundant starting
materials. It would be highly desirable to provide a
process for efficiently and effectively producing
flavorful and aromatic compounds useful in the
manufacture of smoking articles, which processes in
particular could utilize more abundant starting
materials and which would not require the additional
steps necessary to form tobacco extractions.
It has now been discovered that flavorful and
aromatic substances can be produced from tobacco
materials previously thought to have little commercial
value, for example, tobacco dust from the cigarette
manufacturing process, without having to first perform
extraction procedures on the materials. Other sources
of tobacco dust can be used, such as finely ground
tobacco leaves and stems. The flavorful and aromatic
substances produced by the invention described herein
possess aromatic qualities, total volatile profiles and
individual volatile component profiles that are
comparable to flavorful and aromatic substances
obtained from the more time-consuming and resource-intensive
extraction/heat treatment methods of the
prior art.
The present invention generally relates to a
process for the production of natural tobacco flavor
substances useful in tobacco smoking products as flavor
substances, and in tobacco substitute materials as a
source of tobacco smoke flavor and/or aroma. The
process of this invention produces suspensions having a
complex mixture of volatile, semi-volatile, and non-volatile
aroma/flavor components that are products of
the Maillard reactions.
In particular, tobacco in the form of finely
divided particles (finely ground tobacco material) is
produced from tobacco material and is mixed with an
aqueous liquid to produce a tobacco suspension. This
suspension is subjected to heat treatment in a pressure
controlled environment (e.g., a Parr bomb) under
conditions sufficient to alter the chemical nature
(e.g., the flavor and aroma characteristics) of the
finely ground tobacco material. Normally, the tobacco
suspension is exposed to a temperature sufficiently
high and for a period of time sufficiently long so as
to provide an increase in aroma/flavor compounds.
However, it is preferable that the tobacco suspension
not be exposed to such a high temperature for a
sufficiently long period of time so as to provide an
aroma/flavor which exhibits a burnt or tarry
aroma/flavor.
The finely ground tobacco material can be
contacted with an aqueous liquid to comprise a tobacco
suspension. The tobacco suspension should have
sufficient aqueous liquid such that a liquid phase is
present in the suspension. Typically the tobacco
suspension can be 80% or less solids. More preferably,
the suspension contains less than 50% solids and most
preferably contains between 10% and 25% solids. Thus,
for the purposes of this invention, it is convenient to
refer to the heat treatment, or the moderately high
temperature treatment, of a tobacco suspension. For
the purposes of the invention, a tobacco suspension can
include tobacco material in a dust or powder form
contacted with an aqueous liquid further comprising
additives (e.g., amino acids, amino acid analogs or
amino acid sources or other nitrogen sources, and/or
sugar or sugar sources).
Accordingly, the present invention more
particularly relates to a process of producing a
natural tobacco flavor or aroma by first contacting
finely ground tobacco material with an aqueous liquid
to provide an aqueous ground tobacco material
suspension, which suspension is then subjected to heat
treatment at a temperature above about 100°C in a
pressure controlled environment. The ground tobacco
material suspension has a tobacco content of at least
about 5 percent by weight, preferably at least about 10
percent by weight, and more preferably at least about
25 percent by weight, when the suspension is exposed to
the moderately high temperature treatment. In general,
the pressure experienced by the ground tobacco material
suspension is greater than ambient (i.e., atmospheric)
pressure. For purposes of this invention, the term
"tobacco content" relates to the weight of the finely
ground tobacco material within the ground tobacco
material suspension relative to the total weight of the
tobacco suspension. The ground tobacco material
suspension normally is subjected to such treatment in
order that the entire suspension is exposed to a
temperature above about 100°C for at least about 10
minutes.
The resulting flavorful and aromatic
compositions are useful as casing or top dressing
components for tobacco laminae and cut filler, as well
as for other smokable material. Alternatively, such
flavorful and aromatic compositions are useful in those
types of smoking articles described in U.S. Patent Nos.
4,708,151 to Shelar; 4,714,082 to Banerjee et al.;
4,756,318 to Clearman et al.; and 4,793,365 to
Sensabaugh; as well as European Patent Publication Nos.
212,234 and 277,519.
The flavorful and aromatic compositions are
also useful as cigarette filter additives. For
example, the flavorful and aromatic compositions can be
incorporated into low density polyethylenes and formed
into strands, and then incorporated into cigarette
filters as described in U.S. Patent Nos. 4,281,671 to
Byrne et al. and 4,862,905 to Green, Jr. et al. The
flavorful and aromatic compositions are also useful as
cigarette wrapper additives; or as additives to the
inner regions of cigarette packages (e.g. within a
paper/foil laminate of a cigarette package or within a
low density polyethylene film which is placed within a
cigarette package) in order to provide a desirable
cigarette aroma and "pack aroma."
Flavor compounds produced by the methods of
the present invention have organoleptic qualities and
volatile content qualities that are comparable to those
compounds produced by solvent extraction of natural
compounds and heat treatments thereof.
Additionally, it has been found that tobacco
materials formerly discarded as waste products of the
manufacturing process may be used as starting materials
in the process of the present invention to yield
flavorful aromatic substances that are also comparative
in concentration and desirable organoleptic qualities
as other tobacco starting materials. Tobacco dust
represents a significant portion of tobacco material
lost during the manufacture of cigarettes. The present
invention provides a heretofore unknown use for tobacco
material as a source for aroma and flavor components
for the manufacture of smoking articles and the like.
These and other advantages of the present
invention are more completely illustrated in view of
the accompanying drawings and detailed description of
the invention which follows.
FIG. 1 is a schematic diagram of process
steps representative of an embodiment of the present
invention.
Referring now to FIG. 1, tobacco material 10
is subjected to grinding 15 to produce a finely ground
tobacco material dust or powder 20. As used herein,
the term "finely ground material" refers to materials
composed of particles that are less than 10 mesh,
preferably less than 20 mesh, and most preferably are
less than 40 mesh (standard sieve size).
Alternatively, the tobacco material may already be in
dust form such that additional grinding is not
necessary (i.e., the starting tobacco material is
already finely ground). Although the preferred tobacco
material is a dust or powder, other types of tobacco
can be used, such as cut filler, strips, stems or
leaves.
The finely ground tobacco material is then
contacted 55 with an aqueous liquid (e.g., water) 60 to
provide an aqueous tobacco suspension 70. This aqueous
tobacco suspension is then placed in a pressure
controlled environment 30, subjected to heat treatment
35, and cooled 40. The treated tobacco suspension is
then collected 50 for use.
The tobacco materials useful herein can vary.
Tobacco materials which are used are of a form such
that upon grinding, the resulting ground material is in
the form of finely divided particles. Examples of
suitable tobaccos include Burley, Flue-Cured, Turkish,
Latakia, Maryland Cigar, as well as the rare or
specialty tobaccos, or blends thereof. Unaged,
uncured, mature or immature tobaccos may also be
employed. Tobacco waste materials such as fines, dust,
scrap, stem, and stalk can be employed. In one
preferred embodiment of the present invention, the
tobacco material comprises a cigarette manufacturing
by-product known to the skilled practitioner as
cigarette dust. The aforementioned tobacco materials
may be processed separately, or as blends thereof.
The tobacco material may be subjected to
various means to reduce its size, such as grinding,
such that the resulting tobacco material is in finely
ground or powder form. Various grinding techniques
will be apparent to one skilled in the art, and may
include the use of e.g., ball mills or hammer mills.
The grinding may also be carried out under vibrating or
agitating conditions, the selection of said conditions
being within the skill of one in the art.
The tobacco suspension may be provided in a
number of ways. In particular, the finely ground
tobacco material may be contacted with a liquid having
an aqueous character, thus providing an aqueous ground
tobacco material suspension. Such a liquid consists
primarily of water, normally greater than about 90
weight percent water, and can be essentially pure water
in certain circumstances. For example, a liquid having
an aqueous character can be distilled water, tap water,
or the like. However, a liquid having an aqueous
character can include water having substances such as
pH buffers, pH adjusters, organic and inorganic acids,
bases and salts, or sugars, amino acids or surfactants
incorporated therein. The liquid also can be a mixture
of water and minor amounts of one or more solvents
which are miscible therewith (e.g., various alcohols,
polyols or humectants such as glycerin or polypropylene
glycol). When the finely ground tobacco material is
provided as a suspension in an aqueous liquid, the
tobacco content of the suspension may be at least about
5 percent of the total suspension by weight, preferably
at least about 10 percent by weight, and more
preferably at least about 25 percent by weight.
The tobacco suspension can also be contacted
with at least one amino acid, amino acid analog or
amino acid source (e.g., glutamine, asparagine,
proline, alanine, cystine, aspartic acid,
phenylalanine, glutamic acid) and at least one sugar or
sugar source (e.g., fructose, sucrose, glucose,
maltose).
If desired, flavoring agents (e.g., cocoa,
licorice, St. John's bread, spices, herbs, and the
like) can also be added to the tobacco suspension.
The tobacco suspension is subjected to
moderately high temperature treatment such as described
in U.S. Patent No. 5,060,669 to White et al., the
disclosure of which is incorporated herein by reference
in its entirety. Typically, such treatment involves
exposing the tobacco suspension to a temperature above
about 100°C, preferably above about 110°C, and more
preferably above about 120°C. However, it is desirable
to subject the tobacco suspension to a temperature
below about 250°C, more desirably below about 200°C, and
most preferably about 175°C, in order to avoid an
undesirable formation of components which are
deleterious to the taste characteristics of the tobacco
composition.
The moderately high temperature treatment of
the tobacco suspension can be performed under an inert
atmosphere. For example, nitrogen and argon gas can be
employed in order to provide an inert atmosphere.
However, the heat treatment can be conducted under
ambient atmosphere (i.e., air).
The moderately high temperature treatment is
performed in a pressure controlled environment. Such
an environment is provided by enclosing the tobacco
suspension in an air sealed vessel or chamber.
Typically, a pressure controlled environment is
provided using a pressure vessel or chamber which is
capable of withstanding relatively high pressures.
Such vessels or chambers (i) provide enclosure or
concealment of the tobacco suspension such that
volatile flavor components of the tobacco suspension
are not lost or do not otherwise escape during the
moderately high temperature treatment step, and (ii)
provide for treatment of the tobacco suspension at a
temperature significantly above about 100°C. Preferred
pressure vessels are equipped with an external heating
source. Examples of vessels which provide a pressure
controlled environment include a high pressure
autoclave from Berghof/America Inc. of Concord,
California, and Parr Reactor Model Nos. 4522 and 4552
available from The Parr Instrument Co. and described in
U.S. Patent No. 4,882,128 to Hukvari et al. Operation
of such exemplary vessels will be apparent to the
skilled artisan. Typical pressures experienced by the
tobacco suspension during the process of the present
invention in such vessels range from about 10 psig to
about 1,000 psig, normally from about 20 psig to about
500 psig.
The amount of time that the tobacco
suspension is subjected to the moderately high
temperature treatment can vary. Normally, the time
period is sufficient to heat an entire tobacco
suspension at the desired temperature for a period of
at least about 10 minutes, preferably at least about 20
minutes. Normally, the time period is less than about
3 hours, preferably less than about 1 hour, and most
preferably about 30 minutes. However, it is desirable
to control the time/temperature profile of tobacco
suspensions subjected to heat treatment so that each
tobacco suspension is not subjected to a particularly
high temperature for a lengthy period of time. It is
highly desirable to employ a pressure vessel design or
a vessel equipped with an agitation mechanism such that
the tobacco suspension experiences a relatively uniform
temperature throughout the treatment period. In
particular, it is highly desirable for the entire
tobacco suspension to be heated uniformly throughout as
much as possible at the maximum temperature to which
the tobacco suspension is subjected.
Conditions provided during the process of the
present invention most desirably are such that certain
components of the tobacco suspension (e.g., free amino
acid pools and naturally occurring sugars) undergo the
Maillard Reactions. The Maillard Reactions or
"browning reactions" are reactions between (i) the
amino substituents of amino acids, peptides, proteins
or other nitrogen-containing compounds, and (ii) the
carbonyl group of a sugar in the reducing form or other
carboxyl-containing compounds which are indigenous or
added to the tobacco suspension. Such reactions result
in a significant darkening of the tobacco suspension,
typically to an extremely dark brown color. See,
Maillard, Ana. Chim., Vol. 9, pp. 5 and 258 (1916);
Hodge, J. Agric. Food Chem., Vol. 1, p. 928 (1953);
Nursten, Food Chem., Vol. 6, p. 263 (1981) and Waller
et al, ACS Symp. Ser. (1983).
The treated tobacco suspension is useful in
the manufacture of smoking articles. They may be added
to conventional cigarettes or other smoking articles as
a top dressing, or casing, or in any convenient mode
selected by the manufacturer. The amount of the
treated tobacco suspension employed per cigarette or
smoking article can vary. For example, in a typical
cigarette having about 0.6 to about 1 g per rod of
smoking material, about 10 to about 100 ppm of the
compound can be used as a top dressing or casing.
Moreover, the treated tobacco suspension may
be used as a filter flavor material for a cigarette.
The suspension may be used to provide flavor/aroma to
any of the forms of material that are used in the
manufacture of tobacco products such as cigars,
cigarettes, smoking tobacco or snuffs.
The present invention is more fully
illustrated by the following examples, which are set
forth to illustrate the present invention and are not
to be construed as limiting thereof. In the following
examples, mg means milligram, µg means micrograms, g
means grams, L means liters, mL means milliliters, min
means minutes, and mm means millimeters.
Tobacco in the form of cigarette dust was
ground on a SWECO vibrating ball mill (SWECO Inc., Los
Angeles, CA USA) until it was reduced to a very fine
powder. 150 g of the ground cigarette dust was mixed
with 1350 g of water. This suspension was reacted in a
sealed Parr bomb at 175°C for 30 minutes. After a
rapid cooling to ambient temperature, the remaining
pressurized volatiles were released and the liquid was
removed from the Parr bomb. A very aromatic aroma was
observed coming from the liquid. This procedure was
repeated with the starting materials of Burley tobacco
dust, flue-cured tobacco dust, and Turkish tobacco
dust.
Tobacco in the form of cigarette dust was
ground as described in Example 1. 375 g of the ground
tobacco material was mixed with 1125 g of water to
provide a suspension. This suspension was reacted in a
Parr bomb at 175°C for 30 minutes. After cooling and
venting as described above, a very powerful aroma was
noted. This procedure was repeated with the starting
materials of Burley tobacco dust, flue-cured tobacco
dust, and Turkish tobacco dust.
Dynamic headspace/gas chromatography/mass
selective detection/flame ionization detection
(P&T/GC/MSD/FID) analyses were performed on the
aromatic liquids produced as in Examples 1 and 2 using
a TEKMAR (Cincinnati, Ohio, USA) LSC 2000 equipped with
a TEKMAR 2016 heated sampling station. To 1.0 mL of
sample, either control compounds or heat-treated
samples in 5 mL Sparge tube (TEKMAR) was added 1.0 mL
of an aqueous solution containing cyclohexanone at 21.3
µg/mL. Four or five analyses of each sample were
performed to obtain adequate values for precision
measurements. The samples were each preheated at 70°C
for 5 minutes prior to being swept for 10 minutes with
a stream of helium at 40 mL/min. The sample
temperature was held at 70°C. The volatiles were
trapped on a Tenax (TEKMAR) trap and were then
thermally desorbed onto the GC column set at 10°C by
heating at 180°C for 5 minutes. The TEKMAR headspace
system was directly interfaced with to a Hewlett-Packard
5880 gas chromatograph (GC) equipped with a DB
1701 fused silica column (J&W Scientific, Folsom, CA)
30 meters long, 0.32 mm inner diameter, and 1 micron
film thickness. The outlet of the column was split
between a flame ionization detector (FID) and a mass
selective detector (MSD) operating in the electron
impact mode at 70 V. The GC injection port, the MSD
interface, and the FID detector were set at 250°C.
After the transfer was complete, the column oven was
programmed from 10°C to 47°C at 2°C per minute followed
by 10°C per minute to 240°C. The FID area counts for
cyclohexanone were employed in the calculation of the
amount of each identified volatile component. The
volatile components were identified from both mass
spectral library search routines and GC retention time
databases.
In Table 1, below, each identified volatile
components from the cigarette dust, Burley tobacco
dust, flue-cured tobacco dust, and Turkish tobacco dust
is presented as an average concentration of the
component over five samples, in µg/mL. In Table 2,
each identified volatile component from the four kinds
of dust used is presented as an average percentage
distribution of the component over five samples. In
both Tables, C2 pyrazines mean pyrazines with 2 carbons
attached (e.g., dimethylpyrazine); C3 pyrazines mean
pyrazines with 3 carbons attached (e.g.,
ethylmethylpyrazines); C4 pyrazines mean pyrazines with
4 carbons attached (e.g., ethyldimethylpyrazines).
AVERAGE CONCENTRATION OF VOLATILES IN TREATED TOBACCO SUSPENSIONS | ||||
Compound | 10% C-Dust | 10% Burley Dust | 10% Flue-Cured Dust | 10% Turkish Dust |
2-methylpropanal | 15.36 | 9.69 | 24.50 | 24.04 |
methylfuran isomer | 5.21 | 2.29 | 6.44 | 5.57 |
methylfuran isomer | 0.99 | 0.53 | 0.79 | 0.97 |
2-butanone | 10.18 | 9.05 | 10.97 | 10.50 |
2,3-butanedione | 9.89 | 6.79 | 15.83 | 14.65 |
3-methylbutanal | 16.24 | 13.55 | 20.84 | 20.96 |
2-methylbutanal | 10.06 | 8.17 | 13.37 | 11.97 |
dimethylfuran | 0.62 | 0.31 | 0.51 | 2.15 |
2,3-pentanedione | 4.16 | 2.65 | 7.23 | 7.78 |
pyrazine | 0.29 | 0.71 | 0.46 | 0.53 |
2-methyl-2-butenal | 1.50 | 3.88 | .038 | 0.72 |
pyridine | 0.16 | 0.83 | 2.91 | 2.20 |
methylpyrazine | 2.09 | 3.65 | 2.65 | 1.96 |
1H-pyrrole | 0.92 | 1.52 | 0.85 | 3.60 |
furfural | 18.05 | 5.57 | 47.06 | 43.91 |
C2 pyrazines | 2.49 | 4.84 | 1.60 | 1.76 |
2-furanmethanol | 0.73 | 0.55 | 0.82 | 1.35 |
2-acetylfuran | 1.43 | 0.45 | 2.59 | 1.19 |
6-methyl-2-heptanone | 0.91 | 0.52 | 0.58 | 3.16 |
limonene | 0.29 | 0.33 | 0.36 | 1.37 |
C3pyrazines | 2.72 | 4.45 | 2.79 | 1.28 |
benzaldehyde | 1.25 | 1.32 | 0.38 | 1.31 |
5-methylfurfural | 17.43 | 10.00 | 34.48 | 33.07 |
C4 pyrazines | 0.82 | 1.82 | 1.00 | 0.36 |
benzeneacetaldehyde | 1.78 | 1.23 | 2.27 | 2.80 |
methoxyphenol | 0.49 | 0.85 | 0.50 | 0.66 |
menthol | 2.81 | 0.74 | .030 | 0.50 |
1-(3-methylphenyl)-ethanone | 0.99 | 0.48 | .050 | 1.90 |
solanone | 7.09 | 5.92 | 2.22 | 5.30 |
β-damascenone | 1.01 | 0.54 | 0.68 | 1.49 |
neophytadiene | 0.67 | 1.78 | 1.66 | 0.95 |
AVERAGE PERCENTAGE DISTRIBUTION OF VOLATILES IN TREATED TOBACCO SUSPENSIONS | ||||
Compound | 10% C-Dust | 10% Burley Dust | 10% Flue-Cured Dust | 10% Turkish Dust |
2-methylpropanal | 8.83 | 7.44 | 10.24 | 9.52 |
methylfuran isomer | 2.99 | 1.76 | 2.69 | 2.21 |
methylfuran isomer | 0.57 | 0.41 | 0.33 | 0.38 |
2-butanone | 5.86 | 6.95 | 4.59 | 4.16 |
2,3-butanedione | 5.70 | 5.22 | 6.62 | 5.80 |
3-methylbutanal | 9.35 | 10.41 | 8.72 | 8.30 |
2-methylbutanal | 5.79 | 6.27 | 5.59 | 4.74 |
dimethylfuran | 0.36 | 0.24 | 0.21 | 0.85 |
2,3-pentanedione | 2.40 | 2.04 | 3.02 | 3.08 |
pyrazine | 0.17 | 0.54 | 0.19 | 0.21 |
2-methyl-2-butenal | 0.86 | 2.97 | 0.16 | .028 |
pyridine | 0.10 | 0.64 | 1.21 | 0.87 |
methylpyrazine | 1.20 | 2.81 | 1.11 | 0.78 |
1H-pyrrole | 0.53 | 1.16 | 0.35 | 1.43 |
furfural | 10.41 | 4.29 | 19.68 | 17.42 |
C2 pyrazines | 1.44 | 3.72 | 0.67 | 0.70 |
2-furanmethanol | 0.42 | 0.42 | 0.34 | 0.54 |
2-acetylfuran | 0.83 | 0.35 | 1.08 | 0.47 |
6-methyl-2-heptanone | .052 | 0.40 | 0.24 | 1.25 |
limonene | 0.17 | 0.25 | 0.15 | 0.54 |
C3pyrazines | 1.26 | 3.42 | 1.17 | 0.51 |
benzaldehyde | 0.58 | 1.02 | 0.16 | 0.52 |
5-methylfurfural | 10.05 | 7.69 | 14.42 | 13.12 |
C4 pyrazines | 0.47 | 1.40 | 0.42 | 0.14 |
benzeneacetaldehyde | 1.02 | 0.94 | 0.95 | 1.11 |
methoxyphenol | 0.28 | 0.65 | 0.21 | 0.26 |
menthol | 1.62 | 0.56 | 0.12 | 0.20 |
1-(3-methylphenyl)-ethanone | 0.57 | 0.37 | 0.21 | 0.75 |
solanone | 4.08 | 4.53 | 0.93 | 2.10 |
β-damascenone | 0.58 | 0.41 | 0.28 | 0.59 |
neophytadiene | 0.38 | 1.35 | 0.70 | 0.38 |
A tobacco blend was prepared containing about
20 parts Burley tobacco, 55 parts flue-cured tobacco,
and 25 parts Oriental tobacco, in the form of tobacco
strips. The strip blend dry weight was approximately
2400 gm. To this blend of tobacco strips, a suspension
of heat-treated tobacco dust was added. The suspension
contained 10% tobacco dust and 90% water by weight
(about 150 grams of tobacco dust and 1350 gm of water).
After application of the suspension, the tobacco
strips' final weight was about 2550 gm and contained
150 gm of the heat-treated tobacco suspension
(approximately 5.8% by weight of the strip blend.)
The strip blend was cut at 32 cuts per inch
at a moisture of approximately 18%. The cut filler was
dried to approximately 13% in a heated pill coater
drum. To this blend of cut filler material, 2040 gm
(40 parts) of expanded flue-cured tobacco cut filler
and 510 gm (10 parts) of cut-rolled expanded stems.
The final blend was top-dressed with 1.5% by
weight of glycerine containing a small amount of
flavoring. The tobacco cut filler was used to prepare
cigarettes that were 88 mm in length (57 mm tobacco rod
wrapped with RJR Ref. 456 paper (Ecusta Corp., Pisgah
Forest, NC, USA) and a 27 mm shaped acetate filter from
Filtron International Ltd. (Great Britain, code SAF).
The cigarettes were ventilated at approximately 13 mm
from the mouth-end. The average ventilation was about
55%. A total of five cigarettes were prepared in this
manner, as follows:
All five cigarettes were submitted for FTC
smoke analysis and had a tar yield per cigarette of
about 10 mg. All of the cigarettes were tested against
Cigarette A. All test cigarettes (B, C, D, E)
delivered more tobacco taste, and were considered
smoother and richer than the control cigarette.
Additionally, the test cigarettes were preferred by
individual smokers over Cigarette A. All four test
products had a pleasant tobacco aroma.
The results of this experiment indicated that
tobacco dust suspensions can be prepared and employed
to enhance tobacco taste and aroma characteristics of
cigarettes.
In the specification and examples, there have
been disclosed preferred embodiments of the invention.
Although specific terms are employed in these examples,
they are used in a generic and descriptive sense only
and not for the purpose of limitation, the scope of the
invention being defined by the following claims.
Claims (9)
- A process for altering the chemical nature of tobacco material, comprising subjecting a tobacco suspension to heat treatment (i) in a pressure controlled environment to above ambient pressure, and (ii) at a temperature above 100°C so that the chemical nature of the tobacco material is altered.
- The process according to claim 1, wherein said tobacco material is obtained by grinding tobacco material to provide finely ground tobacco material.
- The process according to claim 1 or 2, wherein said tobacco suspension is produced by contacting said tobacco material with an aqueous liquid.
- The process according to one or several of claims 1 to 3, wherein the tobacco suspension contains 10 percent or greater tobacco material by weight.
- The process according to one or several of claims 1 to 4, wherein the pressure controlled environment is a closed system.
- The process according to one or several of claims 1 to 5, wherein the tobacco suspension is subjected to heat treatment at a temperature below about 250°C.
- The process according to one or several of claims 1 to 6, wherein the tobacco suspension is subjected to heat treatment at a pressure of about 10 psig to about 1000 psig.
- The process according to one or several of claims 1 to 7, wherein the tobacco suspension is subjected to heat treatment at a pressure of about 20 psig to about 500 psig.
- The process according to one or several of claims 1 to 8, whereby the tobacco suspension is subjected to heat treatment at a pressure exceeding 100 psig.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US69115896A | 1996-08-01 | 1996-08-01 | |
US691158 | 1996-08-01 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0821886A2 true EP0821886A2 (en) | 1998-02-04 |
EP0821886A3 EP0821886A3 (en) | 1998-08-19 |
Family
ID=24775391
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97113000A Withdrawn EP0821886A3 (en) | 1996-08-01 | 1997-07-29 | Method of providing aromatic compounds from tobacco |
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EP (1) | EP0821886A3 (en) |
JP (1) | JPH1066559A (en) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2000028840A1 (en) * | 1998-11-18 | 2000-05-25 | R. J. Reynolds Tobacco Company | Tobacco flavoring components of enhanced aromatic content and method of providing same |
US6440223B1 (en) | 2000-02-15 | 2002-08-27 | R. J. Reynolds Tobacco Co. | Smoking article containing heat activatable flavorant-generating material |
US6499489B1 (en) | 2000-05-12 | 2002-12-31 | R. J. Reynolds Tobacco Company | Tobacco-based cooked casing formulation |
US6695924B1 (en) | 2000-07-25 | 2004-02-24 | Michael Francis Dube | Method of improving flavor in smoking article |
WO2004041006A1 (en) * | 2002-10-31 | 2004-05-21 | R.J. Reynolds Tobacco Company | Tobacco blends incorporating oriental tobaccos |
US10159273B2 (en) | 2011-01-28 | 2018-12-25 | R.J. Reynolds Tobacco Company | Tobacco-derived casing composition |
WO2020245414A1 (en) * | 2019-06-05 | 2020-12-10 | Philip Morris Products S.A. | Liquid tobacco extract, method for making and aerosol-generating articles comprising such |
WO2020245410A1 (en) * | 2019-06-05 | 2020-12-10 | Philip Morris Products S.A. | Improved method of producing a liquid tobacco extract |
WO2020245411A1 (en) * | 2019-06-05 | 2020-12-10 | Philip Morris Products S.A. | Concentration of wet tobacco extracts |
EP3662765A4 (en) * | 2017-09-05 | 2021-04-07 | Japan Tobacco Inc. | Tobacco material |
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WO2011146264A2 (en) * | 2010-05-21 | 2011-11-24 | Global Vapor Trademarks Incorporated | Method for preparing tobacco extract for electronic smoking devices |
EP2537423A1 (en) * | 2011-06-22 | 2012-12-26 | Nestec S.A. | Method of producing an aromatised aqueous liquid |
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WO2023157878A1 (en) * | 2022-02-18 | 2023-08-24 | 日本たばこ産業株式会社 | Method for augmenting amount of solanone in leaf tobacco, method for manufacturing tobacco raw material, and method for extracting solanone |
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CN114007449B (en) * | 2019-06-05 | 2023-09-12 | 菲利普莫里斯生产公司 | Nicotine composition, method of making and aerosol-generating article comprising the same |
CN113795156B (en) * | 2019-06-05 | 2023-11-17 | 菲利普莫里斯生产公司 | Liquid tobacco extract, method of making and aerosol-generating article comprising the liquid tobacco extract |
EP4285744A3 (en) * | 2019-06-05 | 2024-02-14 | Philip Morris Products S.A. | Improved method of producing a liquid tobacco extract |
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EP0821886A3 (en) | 1998-08-19 |
JPH1066559A (en) | 1998-03-10 |
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