RU2633205C2 - Method of producing raw tobacco material - Google Patents

Abstract

FIELD: tobacco industry.

SUBSTANCE: method for producing raw tobacco material includes a step of smoking a dried tobacco leaf; a step of introducing an alcohol and/or sugar alcohol into the smoked and dried tobacco leaf; a step of storing the tobacco leaf, into which alcohol was introduced; and a step of introducing polyol into the tobacco leaf after the storing step.

EFFECT: improving the flavour of the raw tobacco material while increasing the level of such flavoring ingredients in the raw tobacco material.

4 cl, 3 dwg, 3 ex

Description

FIELD OF THE INVENTION

The present invention relates to a method for producing starting tobacco material.

BACKGROUND OF THE INVENTION

So far, attempts have been made to improve the flavor of the original leaf tobacco. For example, Patent Document 1 describes a method in which ethyl alcohol is introduced into leaf tobacco before the stage of maturation of leaf tobacco on a drum.

According to this document, the chemical actions of ethyl alcohol adsorbed on leaf tobacco accelerate the reactions of oxidation, decomposition, deamination, etc. protein-containing macromolecular compounds, nitrogen-containing compounds and sugars in leaf tobacco, so that tobacco ripening occurs when a large amount of carbon dioxide is released. The smoke emitted when cigarettes are smoked that use leaf tobacco obtained by such fermentation reportedly contains high levels of organic acids such as formic acid and acetic acid. It is also indicated that levels of substances such as acetaldehyde, acetone, acrolein and acetol are reduced, which cause unpleasant odors and irritation during smoking.

Patent Document 1: Japanese Patent Application Laid-Open No. S56-51976

SUMMARY OF THE INVENTION

Despite the fact that Patent Document 1 claims that the method described therein, when using ethanol in leaf tobacco, is able to increase the content of organic acids introduced into the smoke emitted when cigarettes using said leaf tobacco are smoked, compounds that increase, are only organic acids.

In contrast, the present invention focuses on ester compounds as ingredients that add flavor to leaf tobacco, providing a method for improving the flavor of the starting tobacco material while increasing the level of such flavoring ingredients in the starting tobacco material.

The authors of the present invention conducted extensive research, the result of which is considered in this application, in the original tobacco material obtained by the production method, which contains: the stage of smoke treatment of the dried tobacco sheet; the step of introducing alcohol into the smoke-dried dried tobacco sheet; and the step of storing the tobacco sheet into which the alcohol has been added, the content of aromatic perfection esters is increased.

The present invention is provided below.

[1] A method for producing a starting tobacco material, comprising: a smoke treatment step of a dried tobacco sheet; the step of introducing alcohol into the smoke-dried dried tobacco sheet; and a step of storing the tobacco sheet into which the alcohol was introduced.

[2] The production method according to [1], which further comprises, after the storage step, the step of introducing the polyol into the tobacco sheet.

[3] The production method according to p. [1] or [2] in which the storage step is carried out in the range from room temperature to 70 ºC for a period of one week (168 hours) or more.

[4] The production method according to any one of [1] to [3], wherein the storage step is carried out in closed conditions.

[5] The production method according to any one of [1] to [4], wherein the smoke treatment is carried out during cold fumigation.

[6] A tobacco product that contains tobacco raw material obtained by the production method according to any one of [1] to [5].

The present invention provides a method for producing a starting tobacco material that has an increased content of ester compounds as flavoring ingredients.

Brief Description of the Drawings

Figure 1 presents graphs showing the relationship between the number of smoke treatments of tobacco sheets and the organic acid content of the tobacco sheet, and Figure 1A shows the content of acetic acid, and Figure 1B shows the contents of isobutyric acid, butyric acid, isovalerianic acid, 2-methylbutyric acids and valerianic acid.

Figure 2 is a graph showing the difference in the composition of the organic acid when the type of wood used in the smoke treatment of tobacco leaves is different.

Figure 3 is a graph showing the composition of the organic acid in the corresponding tobacco raw materials obtained by performing only the smoke treatment stage, when performing the smoke processing stage after the ethanol injection step, when performing the smoke processing step after the menthol introduction step, and when performing the smoke treatment step after the ethanol introduction step and menthol.

Figure 4 presents graphs showing the amount of change in the organic acid esters in the starting tobacco material into which propylene glycol was introduced at various concentrations, after the stage in which the alcohol was introduced into the smoke-dried dried tobacco sheet (horizontal axis 1 in the graphs), and after the stage , on which the tobacco sheets obtained with the introduction of alcohol were stored for one week (168 hours) (horizontal axes 2-4 on the graphs).

MODE FOR CARRYING OUT THE INVENTION

The present invention is described in detail below by means of embodiments, examples, and the like. However, the invention is not limited to the following embodiments and examples, and may use any modifications if they do not depart from the essence and scope of the invention.

The present process for preparing a starting tobacco material comprises the steps of smoke processing a dried tobacco sheet, introducing alcohol into the smoke-dried dried tobacco sheet, and storing the tobacco sheet into which the alcohol has been introduced.

A tobacco sheet subjected to smoke treatment in a method for producing the invention is a tobacco sheet that has been subjected to a drying treatment. Drying processing is carried out by methods that are well known. In this invention, the expression "dried tobacco leaf" refers to tobacco leaves that have been dried to a moisture content of usually less than 15% wt.

Drying processing can be performed using a known method without special restrictions.

The tobacco sheets used, although not specifically limited, are illustrated by the following varieties of the Nicotian genus: draft dried and gross varieties of N. Tabacum and the Brazilian variety N. rustica.

These tobacco sheets are cut in a known manner to produce ground tobacco.

Smoke treatment stage

The method of smoke processing of the tobacco sheet is carried out by such known methods as hot smoke treatment, warm smoke treatment and cold smoke treatment.

Hot smoke treatment is a treatment in which a tobacco sheet is processed at a temperature of the sheet from about 60 ° C to about 120 ° C. The processing time can be set as required based on the required amount of organic acid given to the tobacco leaf, and is usually from about 10 minutes to about 1 hour.

Warm smoke treatment is a treatment in which a tobacco sheet is processed at a temperature of the sheet from about 30 ° C to about 60 ° C. Processing time can be set as required based on the required amount of organic acid given to the tobacco leaf, and is usually from about 10 minutes to about 1 day (24 hours).

Cold smoke treatment is a treatment in which a tobacco sheet is processed at a temperature of the sheet from about 15 ° C to about 30 ° C. Processing time can be set as required based on the required amount of organic acid given to the tobacco leaf, and is usually from about 10 minutes to about 4 weeks (672 hours).

The type of wood used to generate fumigation smoke is not specifically limited and includes, for example, white oak, cherry, hazel, apple, beech, oak and hickory. Fumigation smoke can be generated by burning or by heating wood. The heating temperature can be set from 350 ° C to 650 ° C and preferably from 450 ° C to 500 ° C.

All of these smoke treatments can be performed using a known fumigation device.

By exposing the tobacco leaf to smoke treatment, the tobacco leaves are given organic acids such as acetic acid, butyric acid, isobutyric acid, valerianic acid, isovaleric acid and 2-methylbutyric acid.

Organic acids can be added to the tobacco sheet using any of the above smoke treatments. By way of illustration, in one embodiment, from the point of view of technological equipment (ease of washing), the smoke treatment is carried out by cold smoke treatment. The smoke treatment time in this case is preferably from 10 minutes to 1 day (24 hours), and more preferably from 1 hour to 3 hours.

Stage of introduction of alcohol

The alcohol introduced into the tobacco sheet obtained by smoke treatment, although not specifically limited, is illustrated by monovalent aliphatic alcohols such as ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-1-propanol, 2 , 2-dimethylethanol and cyclohexanol; monovalent alcohols having an aromatic substituent, such as benzyl alcohol and phenylethyl alcohol; and sugar alcohols such as sorbitol, maltitol, xylitol, erythritol, lactitol, sorbitan, xylose, arabinose, mannose and trehalose.

These alcohols may be used alone, or two or more may be used in combination.

Storage of a smoke-treated tobacco sheet, which was given organic acids and into which alcohol was subsequently added, provides the interaction of organic acids and alcohol, causing esterification. As a result, the ester compounds in the resulting starting tobacco material increase.

Alcohol introduced into the tobacco sheet may be introduced to a degree of from 0.000001 to 0.1 parts by weight / part by weight. tobacco leaf.

The introduction of alcohol is carried out using a conventional method, such as spraying, in order to apply the alcohol as uniformly as possible on the crushed tobacco sheet.

At the stage of introducing alcohol, other flavors can be introduced along with alcohol. Examples of such flavorings include one or more representatives selected from essential oils and flavoring extracts such as menthol, rum, peppermint oil, spearmint oil, menthol oil, rosemary oil, licorice extract, St. John and Cocoa.

Flavors introduced into the tobacco leaf may be added to a degree of from 0.000001 to 0.1 parts by weight / part by weight. tobacco leaf.

Storage stage

The storage step of the tobacco sheet into which the alcohol has been added is preferably carried out under conditions where the ester compounds that are formed during storage do not volatilize. Such conditions are illustrated by closed conditions.

Closed conditions may be conditions formed using a closed vessel. Alternatively, closed conditions may be conditions in which volatile ingredients, such as low molecular weight ester compounds, do not volatilize.

The storage period is not specifically limited if it is a period sufficient for the formation of ester compounds, although a period of one week (168 hours) or more is preferable to ensure that sufficient reactions take place.

No special upper limit is entered for the storage period. Taking into account the period during which the starting tobacco material is transported, the storage period can be up to, for example, about 30 weeks (5040 hours).

The temperature during storage is preferably the temperature at which the formation of the ester compound completely takes place.

This temperature is preferably the temperature at which the enzymes are present in the tobacco sheet and promote the esterification reactions, as well as the temperature at which the chemical esterification reactions easily take place.

In one embodiment, the temperature may be controlled in the range from room temperature to 70 ° C. Alternatively, the temperature may suitably be set in the range of 30 ° C to 80 ° C.

In addition to the organic acids given to the tobacco sheet by smoke treatment, the tobacco sheet may also contain organic acids already present therein, such as myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid. As a result, in the presence of a production method passing through the alcohol introduction step and the storage step described above, organic acid esters are already present in the tobacco sheet, and also are formed upon the introduction of alcohol.

The tobacco sheet also contains the following alcohols: methanol, benzyl alcohol and phenylethyl alcohol. In the presence of a process for preparing the invention through the above steps, it is contemplated that these alcohols also contribute to the formation of an ester.

Illustrative examples of organic acid esters whose levels increase in the starting tobacco material obtained by the process for producing the invention include ethyl acetate, ethyl valerate, ethyl crotonate, ethyl hexanoate, ethyl myristate, ethyl palmitate, ethyl stearate, ethyl oleate, ethyl succinate.

The method for producing the invention may also comprise, after the storage step, the step of introducing the polyol into the ground tobacco sheet. As the polyol, propylene glycol, glycerin or a mixture thereof can be used. The polyol can be introduced into the crushed tobacco sheet in an amount of from 0.1% wt. up to 5% wt.

The introduction of the polyol is preferably carried out by spraying or some other conventional method used in the methods for producing tobacco, so that the polyol impregnates the entire ground tobacco sheet.

As shown in the experiments described below, polyols serve to suppress esterification reactions between the introduced alcohol and organic acids. However, with the introduction of the polyol after the storage step, the formation of ester compounds due to additional reactions caused by the alcohol that has been introduced can be suppressed. As a result of this invention, the composition of the ester compounds that are formed during the storage step is unlikely to change over time.

The reason for this is that, compared to alcohols, the polyol that has been introduced preferably forms esters with organic acids. After the production method passes through the polyol injection step with the complete suppression of the esterification reactions between the alcohol that has been introduced and the organic acids, storage for about a week (168 hours) or more is preferred. Such storage is preferably carried out in closed conditions.

Additives, such as the above essential oils and extracts of flavorings, can be introduced in any quantity and at any stage of the method of obtaining the invention.

Tobacco product

The starting tobacco material of the invention can be converted, for example, into an oral tobacco product, such as snus. In this case, the original tobacco material obtained by the above production method is packaged in a known manner in a package made of non-woven fabric or the like. For example, snus is obtained by filling the package with a controlled amount of the original tobacco material, then brewing the package with a tool such as heat welding.

Packaging is not subject to any specific limitation, although the use of cellulose-containing non-woven fabric is preferred.

In cases where the oral tobacco product is gum, the latter can be obtained by a known method of mixing the starting tobacco material obtained by the above production method with a known rubber base. Chewing tobacco, "snuff", as well as pressed tobacco, in addition to using the starting tobacco material obtained by the production method of the invention, can be obtained by known methods. Similarly, edible films also, in addition to using the starting tobacco material obtained by the production method of the invention, can be obtained using a known material or method.

The starting tobacco material of the invention can be mixed in any ratio with traditional ground tobacco, and the resulting mixture is used to make cigarettes. Alternatively, the starting tobacco material of the invention may be placed in a filter portion of known cigarettes. The placement in the filter portion may entail, for example, the placement of the source tobacco material in the cavity or the dispersion of the source tobacco material among the fibers of the filter.

The starting tobacco material of the invention can also be used in substitutes for heating or non-heating type cigarettes.

The method of obtaining the invention provides the creation of starting tobacco materials containing an improved level of flavoring ingredients. Also, the starting tobacco material obtained by the method of the invention can be used as all the starting tobacco material in the tobacco product or can be used as part of the starting tobacco material in the tobacco product. In those cases where the starting tobacco material obtained according to this invention is used as part of the starting tobacco material in the tobacco product, it can be used in any proportion.

Examples

The present invention is described in more detail below by way of examples. However, the invention, since it does not depart from its essence and scope, is not limited to the following examples.

Experiment 1

The use of short chain fatty acids in the smoke processing of tobacco sheets (details of the smoke treatment)

Wood chips of white oak, 20 g, are weighed on aluminum foil, then distributed on the bottom of the fumigation device.

Then 20 g of crushed tobacco is placed on a grid in a fumigation device. The lid of the fumigation device is closed and the heater (600 W) is turned on. After the start of smoke generation, heating is carried out at 600 W for another 5 minutes, after which the power supply to the heater is stopped. The length of time from the start of smoke is about 6-7 minutes. The fumigation device is then left to stand for 30 minutes with the lid remaining closed (cooling).

In those cases where the processed ground tobacco is subjected to additional smoke treatment, the above operations are repeated.

During the above treatment, the temperature of the tobacco is about 100 ° C and the temperature of the wood chips is about 600 ° C.

Analysis method

The concentration of acetic acid introduced into the tobacco sheet, which was subjected to smoke treatment, is determined as follows.

Ultrapure water, 10 ml, is added to 0.5 g of smoke-processed ground tobacco and extraction is carried out with 30 minutes of shaking.

The extract was ultrafiltered (molecular weight slice 3000), and the filtrate was collected. The filtrate is diluted with ultrapure water so that it falls within the range of the working curve, and a capillary electrophoresis (DAD detector) quantitative analysis is performed.

Further analysis of other organic acids is carried out by the method of solid-phase extraction gas chromatography - mass spectrometry ((TFE-GC-MS) (SPE-GC-MS)).

Ultrapure water, 50 ml, is added to 0.5 g of smoke-processed ground tobacco and extraction is carried out with 30 minutes of shaking.

The extract is filtered and recovered, then the pH is adjusted to pH 2 by the addition of hydrochloric acid.

The extract was passed through a solid phase extraction cartridge (Oasis HLB), conditioned with approximately 20 ml of each of diethyl ether, methanol and an aqueous solution of 0.01 N hydrochloric acid, after which the cartridge was dried using a stream of nitrogen. Organic acids that are adsorbed in the cartridge are washed with diethyl ether and quantitatively analyzed by the GC-MS method.

Figure 1 presents comparative data on the results of the analysis of organic acids before and after smoke treatment.

The results presented in figure 1, it was confirmed that the content of organic acids introduced into the tobacco sheet increased as a result of the passage of the tobacco sheet smoke treatment. In addition, it was also confirmed that an increase in the number of smoke treatments increases the amount of organic acids introduced into tobacco leaves.

In addition, the difference in the concentration of acetic acid obtained using various types of wood in smoke treatment was investigated.

The procedure performed for each type of wood was the same as described above for white oak.

The results are presented in figure 2.

From the results presented in FIG. 2, it can be seen that even when the type of wood used in the smoke treatment is different, the content of organic acids in the tobacco leaves increases.

Experiment 2

Change in the composition of organic acids accompanying esterification treatment

Etherification Operations

10 g of ground tobacco that has passed 8 smoke treatments with white oak is placed together with alcohol (0.5 g of ethanol, 0.5 g of menthol or 0.5 g of ethanol + 0.5 g of menthol) in a threaded throat ampoule which is then sealed. A sealed ampoule is stored in a closed vessel when heated at a given temperature (70 ° C) for a specified period of time (one week (168 h)).

With regard to such an esterification treatment, the concentrations of organic acids for smoke treatment (8 smoke treatments with white oak) are investigated separately for the introduction of ethanol after the smoke treatment, for the introduction of menthol after the smoke treatment and for the introduction of ethanol and menthol after the smoke treatment. The results are presented in figure 3.

The determination of the content of organic acids is carried out by the same method as in experiment 1 above.

Based on the results presented in FIG. 3, it can be assumed that in the smoke-treated tobacco sheet, into which the alcohol was introduced, and which was heated in a closed vessel, the content of organic acids decreases, and esterification reactions took place.

Experiment 3

The formation of various esters accompanying esterification treatment

Hardening of smoke-treated ground tobacco with ethyl esterification and polyol injection

Etherification and hardening conditions

Ethanol (5% based on the weight of the crushed tobacco sheet after smoke treatment) is introduced into the smoke-processed tobacco sheet, after which the tobacco sheet is placed in a throat ampoule, which is then sealed at 40 ° C for one week (168 h). After one week (168 h) of storage in this way, propylene glycol is introduced into the tobacco sheet in a certain concentration (1% wt., 2% wt. Or 5% wt. Relative to the tobacco sheet).

Organic acid esters are each analyzed at the operations indicated below, after 0 weeks (0 h) (without treatment), one week (168 h) after ethanol (before propylene glycol), and with a weekly (168 h) interval thereafter (after the introduction of propylene glycol).

Analysis of ester compounds is performed as follows.

After accurately weighing 0.5 g of ground tobacco in an ampoule (20 ml capacity) of solid-phase microextraction ((TFME) (SPME)), the ampoule is sealed by attaching an ampoule cover and the analysis is carried out using a (gas chromatography) mass spectrometer ((GC-MS) ) (GCMS)) equipped with an automated TFME injection system.

In addition, the sample obtained by injecting 25 μl of an acetonitrile solution of para-bromophene-ethyl alcohol (1 mg / ml) into another TFME ampule is analyzed in a similar manner, the ratio of the peak surface area of the analyte and para-bromophene-ethanol is determined, and based on the calculated values, they are compared the amount of analyte contained in the respective tobacco samples.

Analysis conditions

Equipment: Mobile Gas Chromatograph (6890A)

Mobile Mass Detector (5973N)

Injection volume: 1 μl (injected in a pulsed whole version)

Column: INNOWAX

Oven: 40 ° C → 250 ° C (3 ° C / min)

Mass detector: TIC version (mass number 29-550)

Analytes

Ester compounds: ethyl acetate, ethyl valerate, ethyl hexanoate, ethyl crotonate, ethyl myoistate, ethyl palmitate, ethyl stearate, ethyl oleate.

The results of experiment 3 are presented in figa-4H. The digital values on the vertical axis in FIG. 4 do not represent the concentration of organic acid esters, but the surface area of the peaks obtained in the GC-MS analysis. The digital values on the horizontal axis in FIG. 4 represent the number of weeks (hours) that have been spent.

As can be seen from figure 4, after one week (168 h) of storage, it was found that the esters of organic acids are formed in the tobacco sheets into which the alcohol was introduced. Tobacco sheets, into which propylene glycol was then introduced, are compared with tobacco sheets, into which propylene glycol was not introduced, it was found that the formation of organic acid esters was suppressed with the passage of time.

Industrial applicability

A process for the preparation of the invention is provided which provides a starting tobacco material containing an increased level of flavoring ingredients such as organic acid esters.

Claims (8)

1. A method of obtaining a source of tobacco material, including: a smoke treatment step of the dried tobacco sheet; the step of introducing alcohol and / or sugar alcohol into the smoke-dried dried tobacco sheet; a step of storing the tobacco sheet into which the alcohol was introduced; and the step of introducing the polyol into the tobacco sheet after the storage step. 2. The production method according to claim 1, in which the storage stage is carried out in the range from room temperature to 70 ° C for a period of one week or more. 3. The production method according to claim 1 or 2, in which the storage stage is carried out in closed conditions. 4. The production method according to claim 1 or 2, in which the smoke treatment is carried out during cold fumigation.

Images