CN109475181B - Tobacco filler for non-combustion heating smoking article - Google Patents
Tobacco filler for non-combustion heating smoking article Download PDFInfo
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- CN109475181B CN109475181B CN201680087892.0A CN201680087892A CN109475181B CN 109475181 B CN109475181 B CN 109475181B CN 201680087892 A CN201680087892 A CN 201680087892A CN 109475181 B CN109475181 B CN 109475181B
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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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
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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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
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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
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/32—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by acyclic compounds
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D1/00—Cigars; Cigarettes
- A24D1/14—Tobacco cartridges for pipes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D1/00—Cigars; Cigarettes
- A24D1/20—Cigarettes specially adapted for simulated smoking devices
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/10—Devices using liquid inhalable precursors
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/20—Devices using solid inhalable precursors
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F47/00—Smokers' requisites not otherwise provided for
Abstract
The purpose of the present invention is to provide a tobacco filler that can suppress the "feeling of flavor inhibition" while maintaining a good flavor in a non-combustion type heated smoking article in the form of a filler containing a tobacco material. A tobacco filler for a non-combustion type heated smoking article comprising a tobacco material and an aerosol-generating liquid, wherein the aerosol-generating liquid comprises at least one of diacetin and monoacetin, and the tobacco material has an acetic acid production rate constant of 1.25 x 10‑8s‑1The following.
Description
Technical Field
The present invention relates to a tobacco filler for a non-combustion type heated smoking article, which is used by being filled in the non-combustion type heated smoking article.
Background
In recent years, non-combustion type heated smoking articles that taste a cigarette without burning tobacco have been developed, and as representative examples, there are known non-combustion type heated smoking articles that are used by filling a pod (pod) -shaped container with a component that generates an aerosol and a component that generates a flavor, non-combustion type heated smoking articles that include a heat source at the tip, and the like.
In addition, a technique of adding glycerin, triethylene glycol, and propylene glycol to a filler in such a non-combustion heating smoking article has also been reported (see patent document 1).
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. 63-148975
Disclosure of Invention
Problems to be solved by the invention
When smoking a cigarette using a non-combustion type heated smoking article, it is required to sufficiently evaporate a flavor component and reduce a so-called "flavor-blocking feeling".
For example, patent document 1 describes that when glycerin, triethylene glycol, and propylene glycol are used as the aerosol-generating liquid, the fragrance becomes good. On the other hand, propylene glycol added in the invention of patent document 1 has a low boiling point and a high vapor pressure, and therefore has a property of being easily volatilized in the oral cavity. Therefore, components other than propylene glycol contained in the aerosol become an atmosphere in which the components are easily volatilized, and the phase changes to a gas phase in the same manner as propylene glycol. Since these volatile components include, in addition to the fragrant smell component, a substance that inhibits the perception of the fragrant smell, it is necessary to greatly increase the amount of propylene glycol produced or change the amount of propylene glycol to a non-volatile aerosol-generating liquid in order to eliminate the sensation of inhibition of the fragrant smell.
Accordingly, an object of the present invention is to provide a tobacco filler for a non-combustion type heated smoking article, which can maintain a good flavor and suppress a "flavor-disturbing feeling".
Means for solving the problems
The present inventors have made intensive studies to solve the above-mentioned problems, and as a result, have found that an aerosol-generating liquid containing at least one of diacetin and monoacetin is added to a tobacco filler, whereby an acetic acid production rate constant of 1.25 × 10 is used as a tobacco material-8s-1The following tobacco materials can solve the above problems, and the present invention has been completed.
Namely, the present invention is as follows.
[1] A tobacco filler for a non-combustible heated smoking article comprising a tobacco material and an aerosol-generating liquid,
the aerosol-generating liquid comprises at least one of diacetin and monoacetin,
the acetic acid generation rate constant of the tobacco material was 1.25X 10-8s-1Hereinafter, the amount of the aerosol-generating liquid added is 50% by weight or more and 300% by weight or less based on the weight of the tobacco material.
[2] Tobacco filler according to [1], wherein the aerosol-generating liquid comprises both diacetin and monoacetin.
[3] The tobacco filler according to [1] or [2], wherein the total content of diacetin and monoacetin in the aerosol-generating liquid is 50% by weight or more.
[4] A tobacco pod for a non-combustion heating smoking article, which is filled with the tobacco filler according to any one of [1] to [3 ].
[5] A non-combustion type heated smoking article comprising the tobacco filler according to any one of [1] to [3 ].
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, in a non-combustion type heated smoking article in which a filler containing a tobacco material is heated, a "feeling of flavor inhibition" can be suppressed while maintaining a good flavor.
Drawings
Fig. 1 is a graph showing the relationship between the remaining aerosol percentage after dilution and the feeling of smell inhibition.
Fig. 2 is a graph showing the relationship between the amount of diacetin added and the sensation of smell inhibition.
FIG. 3 is a graph showing the relationship between the amount of water added and the amount of acetic acid.
Fig. 4 is a graph showing the relationship between the amount of acetic acid and the acidity.
FIG. 5 is a graph showing the relationship between the number of days of storage and the amount of acetic acid produced.
FIG. 6 is a graph showing the relationship between the number of days of storage and the production ratio of acetic acid.
FIG. 7 is a graph showing the number of days of storage in combination with-ln (1-C/C)max) A graph of the relationship of (1).
Fig. 8 is a sectional view showing an example of a non-combustion type heated smoking article.
Detailed Description
The present invention is described by way of specific examples, but the present invention is not limited to the following, and can be carried out by making appropriate changes without departing from the spirit of the present invention.
< tobacco filler for non-combustion type heating smoking article >
A tobacco filler for a non-combustion type heated smoking article (hereinafter, may be simply referred to as "tobacco filler of the present invention") as one embodiment of the present invention contains acetic acid with a rate constant of 1.25 × 10-8s-1The aerosol-generating liquid is added in an amount of 50 to 300 wt% based on the weight of the tobacco material.
< acetic acid formation Rate constant of tobacco Material >
The tobacco material contained in the tobacco filler of the present invention has an acetic acid production rate constant of 1.25X 10-8s-1The following.
By making acetic acid generation rate constant of tobacco material 1.25X 10-8s-1As described below, the activity of the hydrolase (acetylesterase) of the tobacco material contained in the tobacco filler is sufficiently suppressed, and the amount of acetic acid produced by hydrolysis of monoacetin and diacetin is suppressed when the tobacco filler is stored. This can prevent deterioration of the flavor of the tobacco filler when the tobacco filler is used.
The acetic acid generation rate constant of the tobacco material is more preferably 1.17X 10-8s-1The following, particularly preferably 1.00X 10-8s-1The following.
Referring to fig. 6 showing the relationship between the acetic acid production ratio and the number of days of storage, which are confirmed in examples described later, the production of acetic acid (decomposition of diacetin) until the number of days of storage reaches 21 days shows a behavior of a primary reaction. Thus, the following primary reaction rate formula can be expressed by arranging the acetic acid production rate constant k with respect to the number of days of storage t.
[ mathematical formula 1]
In the above formula, C represents the amount of acetic acid, CmaxRepresents the maximum amount of acetic acid generated by hydrolysis of the added diacetin.
The conditions for calculating the acetic acid production rate constant were as follows.
100mg of diacetin was added relative to 100mg (wet weight) of the tobacco material, thereby preparing a mixture of the tobacco material and diacetin.
The prepared mixture was stored at 22 ℃ and 60% humidity for 2 months.
The stored mixture was put in a spiral tube, extracted with methanol solvent for 40 minutes under shaking, and then quantified for acetic acid by GC-MS, and the rate constant of acetic acid formation was calculated from the above equation.
The tobacco material having the acetic acid production rate constant as described above may be a tobacco material in the form of a sheet obtained by pulverizing tobacco leaves (leaf tobaccos) into powder and then molding the pulverized tobacco leaves, which is obtained by a treatment for inactivating a hydrolase, as described below, in addition to tobacco shreds.
The type of tobacco used as the tobacco material is not particularly limited, and examples thereof include yellow tobacco, Burley tobacco, native tobacco, and regenerated tobacco, and examples thereof include leaves (cut filler), stems, veins (cut filler), roots, and flowers.
The cut tobacco is not limited in size, and the ball equivalent diameter is usually 1.5mm or less, preferably 0.5mm or less, and usually 0.01mm or more by a measurement method using a projected cross-sectional area (for example, a method using a Camsizer (Retsch).
When the tobacco shred is used, tobacco shreds obtained by cutting tobacco leaves (tobaco leaf) to a size (maximum diameter) of 0.01 to 100mm may be used.
In the present invention, the raw material used for obtaining the tobacco material as described above is used so that the acetic acid rate constant becomes 1.25X 10-8s-1The material treated in the following manner was used as a tobacco material.
Such a treatment may be a treatment of inactivating a hydrolase contained in a tobacco leaf or the like in a raw material serving as a tobacco material, which affects the rate constant of acetic acid production.
Examples of the treatment for inactivating the hydrolase in the tobacco leaf include a treatment that varies depending on the structure of the protein constituting the enzyme, and examples thereof include a heat treatment. Specifically, the heating may be performed at a temperature of 130 ℃ or higher for 60 minutes or longer. When the temperature is set to a higher temperature, the heating time can be reduced as appropriate.
Other treatments for inactivating the hydrolase include physical treatments such as drying while heating and freeze-drying.
In addition, as another treatment, chemical treatment in which a raw material used as a tobacco material is used in the presence of an organic solvent and an acid/alkali is added to tobacco leaves can be cited.
The content of the tobacco material in the tobacco filler of the present invention is usually 20% by weight or more, preferably 30% by weight or more, more preferably 40% by weight or more, usually 80% by weight or less, preferably 70% by weight or less, more preferably 60% by weight or less. When the amount is within the above range, the "smell-blocking feeling" can be more effectively suppressed while the smell during use can be favorably maintained.
The tobacco filler of the present invention contains an aerosol-generating liquid comprising at least one of diacetin and monoacetin.
As will be shown in the examples described below, by incorporating an aerosol-generating liquid containing at least one of diacetin and monoacetin in the tobacco filler of the present invention, when a non-combustible smoking article containing the tobacco filler of the present invention is used, the aerosol generated is less likely to volatilize by dilution in the oral cavity, and components that hinder the perception of the flavor components contained in the aerosol are less likely to change to the gas phase. This reduces the feeling of smell inhibition.
In the present invention, the degree of volatilization of the generated aerosol caused by dilution in the oral cavity is evaluated by measuring the "remaining aerosol percentage after dilution". The higher the remaining rate of aerosol after dilution, the lower the smell inhibition feeling.
At least one of diacetin and monoacetin is included in the aerosol-generating liquid used in the invention.
The content thereof is 50% by weight or more and 300% by weight or less based on the amount of the aerosol-generating liquid added to the tobacco material contained in the tobacco filler.
By setting the content of the aerosol-generating liquid containing at least one of diacetin and monoacetin to 50% by weight or more relative to the tobacco material, it is possible to ensure effective reduction of the sensation of blocking the aroma and taste.
On the other hand, in order to smoothly heat the tobacco filler when the tobacco filler is used in a non-combustion type smoking article, the upper limit of the content of the aerosol-generating liquid containing at least one of diacetin and monoacetin is 300 wt% or less.
It is noted that, in the case of diacetin and monoacetin, it is difficult to prepare liquids containing diacetin and monoacetin separately, and a commercially available "diacetin" solution contains about 42% by weight of diacetin and about 38% by weight of monoacetin. On the other hand, a commercially available "monoacetin" solution contains about 45% by weight of monoacetin and about 36% by weight of diacetin.
Thus, for example, when a commercially available "diacetin" solution is prepared as a solution containing at least one of diacetin and monoacetin and 50% by weight of the solution is added to a tobacco material, the content of diacetin is about 21% by weight and the content of monoacetin is about 19% by weight of the tobacco material.
In addition, the total content of diacetin and monoacetin was 81% by weight in the solution of the commercially available product of "diacetin", and the total content of diacetin and monoacetin was 81% by weight in the solution of the commercially available product of "monoacetin".
Therefore, in the tobacco filler of the present invention, when a commercially available "diacetin" solution or a commercially available "monoacetin" solution is added to the tobacco material in an amount of 50 wt%, the total amount of diacetin and monoacetin is about 40 wt% of the tobacco material.
Examples of the aerosol-generating liquid used in the present invention include a system containing both diacetin and monoacetin.
The total content of diacetin and monoacetin in the aerosol-generating liquid used in the present invention is preferably 50% by weight or more, more preferably 70% by weight or more, and particularly preferably 75% by weight or more.
The aerosol-generating liquid may contain other components as needed in addition to at least one of diacetin and monoacetin as described above.
For example, the following acids having a first acid dissociation constant of 4.0 or more and 6.0 or less and a boiling point of 366 ℃ or more and 600 ℃ or less are exemplified. The "first acid dissociation constant" refers to an acid dissociation constant in water at normal temperature (25 ℃).
Further, "boiling point" means a boiling point at a pressure of 760 mmHg.
Examples of such acids include ascorbic acid, isoascorbic acid, heneicosanoic acid, tetracosanoic acid, octacosanoic acid, and nonadecanoic acid.
Among them, ascorbic acid, erythorbic acid and the like are particularly preferable.
With the acid as described above, it is possible to more easily suppress a decrease in the amount of evaporation of the fragrant component and to more effectively suppress the "feeling of blocking the fragrance".
When the tobacco filler of the present invention contains the acid, the content thereof is usually 0.25% by weight or more, preferably 1% by weight or more, and usually 10% by weight or less. When the amount is within the above range, the "smell-blocking feeling" can be more favorably reduced while the decrease in the amount of the smell component evaporated can be more easily suppressed.
Examples of additives other than the acids include polyhydric alcohols such as glycerin, propylene glycol, triethylene glycol, and tetraethylene glycol; aliphatic carboxylic acid esters such as methyl stearate, dimethyl dodecanedioate, and dimethyl tetradecanedioate.
These components are not limited to 1 kind, and 2 or more kinds may be used in combination.
It is expected that the amount of acetic acid in the tobacco filler of the invention after its preparation and after storage for more than 2 months will only increase to less than 1.1% by weight relative to the added weight of added aerosol-generating liquid. This is because, as described above, the hydrolase contained in the tobacco material is inactivated, and thus the tobacco material has a low acetic acid production rate constant.
Therefore, the tobacco filler of the present invention is also excellent in storage stability.
The tobacco filler of the present invention includes tobacco shreds and an aerosol-generating liquid, but since components such as water contained in the tobacco shreds are usually dissolved out into the aerosol-generating liquid, it can be said that the tobacco filler of the present invention also contains water.
The tobacco filler of the present invention contains water in an amount of usually 5 wt% or more, preferably 7.5 wt% or more, more preferably 10 wt% or more, usually 30 wt% or less, preferably 25 wt% or less, more preferably 20 wt% or less, based on the whole tobacco filler. When the amount is within the above range, the "smell-blocking feeling" can be more effectively suppressed while the smell during use is favorably maintained.
The tobacco filler of the present invention may be distributed in the form of a container filled with a pod (hereinafter also referred to as pod) as shown below in order to be used in a non-combustion type heated smoking article. The shape of the pod in this case may be a known shape, and the material thereof is not particularly limited, and a metal having high thermal conductivity such as aluminum may be used.
The amount of tobacco filler to be filled into the tobacco pod can be adjusted as appropriate depending on the kind of article to be sold.
The tobacco filler of the present invention is a tobacco filler for a non-combustion type heated smoking article containing tobacco shreds and an aerosol-generating liquid, and the specific configuration and the like of the non-combustion type heated smoking article filled with the tobacco filler of the present invention are not particularly limited, and known configurations can be suitably employed. Hereinafter, specific examples will be described.
As the non-combustion type heating smoking article, there is exemplified a non-combustion type heating smoking article having a structure of the non-combustion type heating smoking article 10 shown in fig. 8. Fig. 8 is a cross-sectional view of a cylindrical non-combustion type heated smoking article 10 cut along its longitudinal direction, and is configured to include a battery 101, a pod 103 for containing a filler 102, a heater 104, and a mouthpiece 105. The tobacco filler of the present invention is filled into tobacco pods 103 and an aerosol is generated by heating.
The heating temperature of the tobacco filler in the non-combustion heating smoking article is usually 22 ℃ or higher, preferably 100 ℃ or higher, more preferably 150 ℃ or higher, and usually 350 ℃ or lower, preferably 300 ℃ or lower, more preferably 250 ℃ or lower. In order to solve the problem of "smell-hindering feeling", when the tobacco filler of the present invention is used in a non-combustion type heated smoking article in which the heating temperature of the tobacco filler is in the above range, the characteristics of the tobacco filler of the present invention can be more effectively utilized.
Examples
The present invention will be described more specifically with reference to the following examples, but may be modified as appropriate without departing from the spirit of the present invention.
< examples 1 and 2 and comparative examples 1 to 7: verification of Effect of Aerosol-Forming liquid modification >
In order to verify the effect of reducing the feeling of inhibition of flavor when the aerosol-generating liquid was changed, the same yellow tobacco shreds as in example 5 below (manufactured in Japan, hereinafter also simply referred to as "tobacco shreds") were produced as tobacco materialsConstant: 1.17X 10-8s-1)100mg of each aerosol-generating liquid shown in Table 1 was added to 100mg of the sample.
The cut tobacco was previously pulverized by a household mixer, and then vibrated for 2 minutes by a sieve (AS200, manufactured by Retch) under conditions of amplitude-1.5 mm/"g", and cut tobacco having a mesh diameter of 0.5mm or less was used. The prepared sample was added in a stick form to a pod dedicated to trade name "Ploom" sold by japan tobacco industry co., ltd, and stored at 22 ℃ and 60% humidity for 2 days or more.
The "diacetin" used in the present example is a commercially available solution, and as described above, contains about 42% by weight of diacetin and about 38% by weight of monoacetin. On the other hand, the "monoacetin" used in this example is also a commercially available solution, and as described above, contains about 45% by weight of monoacetin and about 36% by weight of diacetin.
The heating temperature of the tobacco shreds when Ploom was used (during steady operation) was confirmed to be about 160 to 170 ℃ by preliminary measurement using a thermocouple.
As described above, the "difficulty of volatilization of aerosol" which is important in measuring the reduction of the smell inhibition feeling is measured by measuring the amount of aerosol before dilution and the amount of aerosol after dilution with clean air, and evaluating the "remaining aerosol after dilution" as a ratio thereof. The measurement of the aerosol amount before dilution was carried out using a smoking machine (Borgwaldt, RM-26), and the initial 5puff amount was measured under predetermined smoking conditions (55ml/2s, smoking interval 30s) with the prepared pod attached to Ploom.
On the other hand, for the measurement of the amount of the aerosol after the dilution, the aerosol generated by the same method as described above was once collected in an SUS tube (volume: about 127cc, length: 25.0cm, inner diameter: 2.54cm), and clean air was circulated, thereby preparing a simulated dilution condition, and then the amount of the aerosol after the removal of the component in the form of a gas phase was measured by an initial 5puff amount using a Cambridge filter through a charcoal packed layer (100 mg). The functionality of the prepared samples was evaluated by 4 persons, and the "smell-retarding effect" was evaluated on 7 grades of 1 to 7. In the results of the present example, when the feeling of smell inhibition was 2.0 or less, the difference was clearly recognized by the evaluator, and the result was regarded as a region having an excellent effect.
Fig. 1 shows the relationship between the remaining aerosol rate after dilution and the taste-disturbing sensation of fragrance when various aerosol-generating liquids shown in table 1 were used. As can be seen from fig. 1, the higher the aerosol residual ratio after dilution, the more the smell-blocking feeling tends to decrease. That is, it is considered that the generated aerosol is not easily volatilized by dilution in the oral cavity, and the amount of the sol remaining in the oral cavity after dilution in the oral cavity is large, and a substance which is an obstacle when the taste of the fragrance contained in the aerosol is felt is not easily changed into a gas phase, and the taste of the smell is low. It is found that diacetin is an aerosol-generating liquid having the lowest smell inhibition feeling as a result because of its high aerosol remaining rate after dilution.
[ Table 1]
TABLE 1 Aerosol-generating liquids and evaluation results
< examples 2-4 and comparative examples 8-14> examination of the amount of addition effective for reducing the sensation of blocking the smell
As described above, since diacetin and monoacetin are difficult to separate from each other, the compositions of solutions containing diacetin and monoacetin are very similar. Therefore, in the following, studies on the amount of diacetin added, which is effective for reducing the sensation of smell inhibition, were carried out using a solution containing diacetin (commercially available product), as a representative.
In order to examine the amount of the diacetin added to the cut burley tobacco (manufactured by japan) in an amount shown in table 2 and propylene glycol as a comparison, 100mg of the cut burley tobacco was added. The sample was prepared in the same manner as in the previous examples, and stored at 22 ℃ and 60% humidity for 2 days or longer. The functionality of the prepared samples was evaluated by 4 persons, and the "smell-retarding effect" was evaluated on 7 grades of 1 to 7. In the results of the present example, when the feeling of smell inhibition was 2.0 or less, the value was a value that enables the evaluator to clearly recognize the difference, and the result was regarded as a region having an excellent effect.
The relationship between the amount of solution added and the taste-impairing sensation with respect to the weight of tobacco shreds is shown in FIG. 2. As is clear from fig. 2, when the aerosol-generating liquid was not added to the tobacco shreds (when the solution addition rate was 0 wt% based on the weight of the tobacco shreds), the sensation of blocking the aroma was very high, and was 6.8. On the other hand, it is known that when diacetin is added to tobacco shreds as an aerosol-generating liquid, the taste of inhibition of aroma decreases as the rate of addition of the solution to the weight of the tobacco shreds increases.
Further, when the addition rate of the solution is 50 wt% or more based on the weight of the tobacco shred, the taste-disturbing sensation is greatly reduced, and therefore the amount of diacetin added effective for reducing the taste-disturbing sensation is 50 wt% or more based on the weight of the tobacco shred. It is found that when propylene glycol is added in an amount of 100 wt% based on the weight of tobacco shreds as an aerosol-generating liquid for comparison, the taste of the tobacco shreds is substantially the same as when the aerosol-generating liquid is not added to the tobacco shreds. From this, it is found that, in reducing the sensation of blocking the taste of fragrance, not only the increase in the solution addition rate with respect to the weight of the tobacco shred but also the reduction in the sensation of blocking the taste of fragrance is effectively exhibited when diacetin, which is an aerosol-generating liquid effective for reducing the sensation of blocking the taste of fragrance, is used.
[ Table 2]
TABLE 2 preparation of samples and evaluation results
< reference examples 1 to 8: investigation of mechanism of production of diacetin and monoacetin hydrolyzate (acetic acid) >
In order to investigate the mechanism of production of acetic acid, which is a hydrolysate of diacetin and monoacetin, 100mg of diacetin was added to 100mg of tobacco shreds (yellow cut tobacco in japan) and calcium carbonate (simulated cut tobacco free), and the samples shown in table 3 were evaluated for their taste-inhibiting effect on aroma and their amount of acetic acid. In order to examine the influence of hydrolysis based on the amount of water, water was added by increasing the water content as shown in table 3. For the evaluation of functionality, 2 persons were used for evaluation, and the "acidity" was evaluated on a scale of 7, i.e., 1 to 7. In the results of the present example, when the acidity is 1.5 or more, the acidity is a value that can be recognized by the evaluator, and a range of 1.5 or less represents a region having an excellent effect of suppressing the decomposition of diacetin. For quantitative analysis of acetic acid, the samples prepared under the conditions of Table 3 were stored at 22 ℃ and 60% humidity for 1 week, placed in a spiral tube (No.5, manufactured by MARUEM Inc.), extracted with methanol solvent for 40 minutes with shaking, and quantified by GC-MS.
[ Table 3]
TABLE 3 preparation of samples and evaluation/measurement results
FIG. 3 is a graph showing the relationship between the amount of water added and the amount of acetic acid produced. According to fig. 3, the amount of acetic acid in the sample pod showed an extremely low value regardless of the amount of water added to the sample in which diacetin was added to calcium carbonate. On the other hand, it is found that when diacetin is added to tobacco shreds, acetic acid is greatly generated in proportion to the amount of water added. From this, it is found that when only diacetin (including calcium carbonate) is stored, the amount of water added does not substantially affect the decomposition of diacetin, but when diacetin is stored in the coexistence of cut tobacco, the decomposition of diacetin is promoted by the increase in the amount of water added, and acetic acid, which is a decomposition product of diacetin, rapidly increases. Therefore, it is considered that although hydrolysis of diacetin alone does not easily occur, hydrolysis of diacetin is promoted by a hydrolase in tobacco shreds, and acetic acid is produced in a large amount as a decomposition product.
Finally, a graph showing the relationship between the amount of acetic acid and the acidity is shown in FIG. 4. As can be seen from fig. 4, the correlation between the amount of acetic acid and the acidity is high, and the "acidity" felt when smoking the stored sample is caused by an increase in the amount of acetic acid produced based on the decomposition of diacetin.
< examples 5 and 6 and comparative examples 15 to 17: verification of hydrolysis inhibition method >
According to the above examples, it is known that the hydrolase in the cut tobacco acts as a catalyst to generate acetic acid as a hydrolysis product of diacetin. Here, as a method for inactivating the hydrolase, the hydrolysis inhibitory effect of diacetin was verified typically by a heat treatment which is usually performed.
The tobacco shred heating treatment method comprises the following steps: 2g of shredded tobacco (yellow shredded tobacco in Japan) was put in a spiral tube (manufactured by No.5MARUEM Inc.), the cover was closed, and the tube was heated in a hot air circulation oven (KLO-60M, Koyo Thermo Systems Co., Ltd.) at 100 ℃ at 120 ℃ for 60 minutes at 140 ℃ and 160 ℃ for 60 minutes. The samples were prepared in the same manner as in the previous examples, and stored at 22 ℃ and 60% humidity for 2 months to quantify the amount of acetic acid and evaluate the functionality. For the evaluation of functionality, 2 persons were used for evaluation, and the "acidity" was evaluated on a scale of 7, i.e., 1 to 7. In the results of the present example, when the acidity is 1.5 or more, the acidity is a value that can be clearly recognized by the evaluator, and conversely, a range of 1.5 or less is a region having an excellent effect of suppressing the decomposition of diacetin. For quantitative analysis of acetic acid, the samples prepared under the conditions of table 4 were stored at 22 ℃ and 60% humidity for 2 months, placed in a spiral tube (manufactured by No.5maruem inc.), extracted with shaking in a methanol solvent for 40 minutes, and quantified by GC-MS.
"Table 4
TABLE 4 sample information and evaluation results
FIG. 5 is a graph showing the relationship between the number of days of storage and the amount of acetic acid in Pod. As is clear from fig. 5, when the tobacco shreds were not heated, the amount of acetic acid in the Pod increased greatly with respect to the number of days of storage, whereas when only the tobacco shreds were heat-treated in advance, the amount of acetic acid generated in the Pod decreased.
It is understood that, in the case of heating the smokeless filament, the amount of acetic acid produced increases rapidly until the number of days of storage is 21 days (3 weeks), while, in the case of the number of days of storage from 21 days to 60 days (2 months), the rate of increase in the amount of acetic acid is small, the rate of production of acetic acid by the decomposition of diacetin decreases, and the amount of acetic acid gradually approaches the maximum amount of acetic acid produced by the hydrolysis of diacetin. Therefore, the acetic acid production (8.90mg/Pod) after the smokeless filament is heated and stored for 2 months can be compared with the maximum acetic acid production (C) due to hydrolysis of diacetin added to Podmax) Approximately, the amount of acetic acid in the Pod (C) is therefore divided by the maximum amount of acetic acid produced (C)max) The obtained value was defined as the acetic acid production ratio (C/C)max)。
Further, according to fig. 6 showing the relationship between the acetic acid production ratio and the number of days of storage, since the production of acetic acid (decomposition of diacetin) until the number of days of storage is 21 shows the behavior of the primary reaction, the following primary reaction rate formula is used, and the rate constant k of production of acetic acid is arranged with respect to the number of days of storage t, and the following formula is used.
[ mathematical formula 2]
Fig. 7 shows the above equation plotted for each heating temperature condition. From FIG. 7, the acetic acid production rate constant k of the tobacco shreds was calculated from the slope of the curve from 1 day to 21 days of storage. Since the cut tobacco contains acetic acid slightly, the graph of fig. 7 does not pass through the origin.
As is clear from Table 4 in which the acetic acid production rate constant k of tobacco shreds was calculated,the acetic acid formation rate constant of tobacco shreds was 1.17X 10-8s-1In the following cases, the acetic acid content was extremely low after 2 months of storage of the sample, and since the acidity was not recognized at all according to the results of the sensory evaluation, the acetic acid production rate constant was 1.17X 10-8s-1The following tobacco shreds were used together with diacetin, and hydrolysis of diacetin was suppressed. Here, since it can be roughly calculated that the acetic acid production rate constant corresponding to an acidity of 1.5 is 1.25X 10-8s-1Therefore, it is considered that the acetic acid generation rate constant of the tobacco material is 1.25X 10-8s-1The effect of suppressing decomposition can be sufficiently ensured in the following cases.
Industrial applicability
The tobacco filler of the present invention is used for smoking by filling a container such as a pod used for a non-combustion type heated smoking article.
Claims (5)
1. A tobacco filler for a non-combustible heated smoking article comprising a tobacco material and an aerosol-generating liquid,
the aerosol-generating liquid comprises at least one of diacetin and monoacetin,
the acetic acid generation rate constant of the tobacco material was 1.25X 10-8s-1The amount of the aerosol-generating liquid added is 50 to 300 wt% based on the weight of the tobacco material,
the conditions for calculating the acetic acid production rate constant were:
a mixture of a tobacco material and diacetin was prepared by adding 100mg of diacetin to 100mg of the tobacco material in terms of wet weight, the prepared mixture was stored at 22 ℃ and 60% humidity for 2 months, the stored mixture was put in a spiral tube, shaking extraction was carried out for 40 minutes using a methanol solvent, quantification of acetic acid was carried out by GC-MS, and the rate constant of acetic acid formation was calculated from the following formula,
in the above formula, k represents the acetic acid production rate constant, t represents the number of days of storage, C represents the amount of acetic acidmaxRepresents the maximum amount of acetic acid generated by hydrolysis of the added diacetin.
2. A tobacco filling according to claim 1, wherein the aerosol-generating liquid comprises both diacetin and monoacetin.
3. Tobacco filler according to claim 1 or 2, wherein the total content of diacetin and monoacetin in the aerosol-generating liquid is 50% by weight or more.
4. A pod for a non-combustible heated smoking article filled with a tobacco filler as claimed in any one of claims 1 to 3.
5. A non-combustible heated smoking article comprising a tobacco filler according to any one of claims 1 to 3.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2016/071526 WO2018016069A1 (en) | 2016-07-22 | 2016-07-22 | Tobacco filler for non-combustion type heat smoking article |
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| CN109475181A CN109475181A (en) | 2019-03-15 |
| CN109475181B true CN109475181B (en) | 2021-07-20 |
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| CN201680087892.0A Active CN109475181B (en) | 2016-07-22 | 2016-07-22 | Tobacco filler for non-combustion heating smoking article |
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| Country | Link |
|---|---|
| US (1) | US20190142072A1 (en) |
| EP (1) | EP3473117B1 (en) |
| JP (1) | JP6685398B2 (en) |
| KR (1) | KR102197986B1 (en) |
| CN (1) | CN109475181B (en) |
| CA (1) | CA3030815C (en) |
| EA (1) | EA037209B1 (en) |
| WO (1) | WO2018016069A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3081102B1 (en) * | 2015-04-15 | 2019-06-05 | Fontem Holdings 1 B.V. | Electronic smoking device |
| CN113347896A (en) * | 2018-07-23 | 2021-09-03 | 健康洞察技术有限公司 | System for analyzing and controlling consumable media dosing information |
| CN109123811A (en) * | 2018-10-10 | 2019-01-04 | 云南巴菰生物科技有限公司 | A kind of electronic cigarette smoke agent |
| JP7325514B2 (en) * | 2019-07-31 | 2023-08-14 | 日本たばこ産業株式会社 | Heat-not-burn tobacco and heat-not-burn tobacco products |
| KR20220066358A (en) * | 2019-10-31 | 2022-05-24 | 니뽄 다바코 산교 가부시키가이샤 | Tobacco fillings for unburnt heated tobacco, unburnt heated tobacco and electrically heated tobacco products |
| CN113693261B (en) * | 2021-09-01 | 2023-06-27 | 深圳市真味生物科技有限公司 | Atomizing agent, preparation method thereof and application of atomizing agent in heating non-combustible smoking set |
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- 2016-07-22 EP EP16909544.5A patent/EP3473117B1/en active Active
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| Publication number | Publication date |
|---|---|
| CN109475181A (en) | 2019-03-15 |
| EA201990361A1 (en) | 2019-06-28 |
| WO2018016069A1 (en) | 2018-01-25 |
| JP6685398B2 (en) | 2020-04-22 |
| CA3030815C (en) | 2021-10-12 |
| EP3473117B1 (en) | 2021-04-14 |
| EA037209B1 (en) | 2021-02-19 |
| JPWO2018016069A1 (en) | 2019-05-30 |
| KR20190029701A (en) | 2019-03-20 |
| CA3030815A1 (en) | 2018-01-25 |
| KR102197986B1 (en) | 2021-01-04 |
| EP3473117A4 (en) | 2020-02-26 |
| US20190142072A1 (en) | 2019-05-16 |
| EP3473117A1 (en) | 2019-04-24 |
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