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WO2018016069A1 - Tobacco filler for non-combustion type heat smoking article - Google Patents

Tobacco filler for non-combustion type heat smoking article Download PDF

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Publication number
WO2018016069A1
WO2018016069A1 PCT/JP2016/071526 JP2016071526W WO2018016069A1 WO 2018016069 A1 WO2018016069 A1 WO 2018016069A1 JP 2016071526 W JP2016071526 W JP 2016071526W WO 2018016069 A1 WO2018016069 A1 WO 2018016069A1
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WO
WIPO (PCT)
Prior art keywords
tobacco
aerosol
diacetin
acetic acid
weight
Prior art date
Application number
PCT/JP2016/071526
Other languages
French (fr)
Japanese (ja)
Inventor
将之 辻
石川 信幸
Original Assignee
日本たばこ産業株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 日本たばこ産業株式会社 filed Critical 日本たばこ産業株式会社
Priority to CA3030815A priority Critical patent/CA3030815C/en
Priority to EA201990361A priority patent/EA037209B1/en
Priority to KR1020197004690A priority patent/KR102197986B1/en
Priority to PCT/JP2016/071526 priority patent/WO2018016069A1/en
Priority to EP16909544.5A priority patent/EP3473117B1/en
Priority to JP2018528180A priority patent/JP6685398B2/en
Priority to CN201680087892.0A priority patent/CN109475181B/en
Publication of WO2018016069A1 publication Critical patent/WO2018016069A1/en
Priority to US16/249,475 priority patent/US20190142072A1/en

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/167Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/32Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by acyclic compounds
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00Cigars; Cigarettes
    • A24D1/14Tobacco cartridges for pipes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00Cigars; Cigarettes
    • A24D1/20Cigarettes specially adapted for simulated smoking devices
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/10Devices using liquid inhalable precursors
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/20Devices using solid inhalable precursors
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F47/00Smokers' requisites not otherwise provided for

Definitions

  • the present invention relates to a tobacco filling for a non-combustion type heated smoking article to be used by filling the non-combustion type heated smoking article.
  • Patent Document 1 described above describes that when glycerin, triethylene glycol, and propylene glycol are used as the aerosol-generating liquid, the flavor is improved.
  • the propylene glycol added in the invention of Patent Document 1 has a property of being easily volatilized in the oral cavity because of its low boiling point and high vapor pressure. For this reason, an atmosphere other than propylene glycol contained in the aerosol is also easily volatilized, and changes into a gas phase in the same manner as propylene glycol.
  • an object of the present invention is to provide a tobacco filling for a non-combustion-type heated smoking article that can maintain a good flavor and suppress the “feel of flavor inhibition”.
  • the present inventors have added an aerosol-generating liquid containing at least one of diacetin and monoacetin to a tobacco filling, and an acetic acid production rate constant as a tobacco material is 1.25. It has been found that the above problems can be solved by using a material having a value of ⁇ 10 ⁇ 8 s ⁇ 1 or less, and the present invention has been completed. That is, the present invention is as follows.
  • a tobacco filler for a non-combustion type 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 production rate constant of the tobacco material is 1.25 ⁇ 10 ⁇ 8 s ⁇ 1 or less, and the amount of the aerosol-generating liquid added is 50% by weight to 300% by weight with respect to the weight of the tobacco material. object.
  • a pod for a non-combustion type heated smoking article which is filled with the tobacco filler according to any one of [1] to [3].
  • a non-combustion type heated smoking article comprising the tobacco filling according to any one of [1] to [3].
  • the non-combustion type heated smoking article in the form of heating the filling containing the tobacco material, it is possible to suppress the “feeling of flavor inhibition” while maintaining a good flavor.
  • the tobacco filler for non-combustion type heated smoking articles which is one embodiment of the present invention (hereinafter sometimes abbreviated as “the tobacco filler of the present invention”) has an acetic acid production rate constant of 1.25 ⁇ 10 ⁇ 8. s ⁇ 1 or less of the tobacco material and an aerosol-generating liquid containing at least one of diacetin and monoacetin, and the added amount of the aerosol-generating liquid is not less than 50% by weight and not more than 300% by weight of the weight of the tobacco material Tobacco filling.
  • the tobacco material contained in the tobacco packing of the present invention has an acetic acid production rate constant of 1.25 ⁇ 10 ⁇ 8 s ⁇ 1 or less.
  • the acetic acid production rate constant of the tobacco material is 1.25 ⁇ 10 ⁇ 8 s ⁇ 1 or less, the activity of the hydrolase (acetylesterase) of the tobacco material contained in the tobacco packing is sufficiently suppressed, and the tobacco During storage of the filling, the amount of acetic acid produced by hydrolysis of monoacetin and diacetin is suppressed. Thereby, the deterioration of the flavor at the time of use of a tobacco filling can be prevented.
  • the acetic acid production rate constant of the tobacco material is more preferably 1.17 ⁇ 10 ⁇ 8 s ⁇ 1 or less, and particularly preferably 1.00 ⁇ 10 ⁇ 8 s ⁇ 1 or less.
  • the production of acetic acid (diacetin decomposition) up to 21 days of storage shows the behavior of the primary reaction.
  • the acetic acid production rate constant k can be expressed as follows by arranging the acetic acid production rate constant k as the following first-order reaction rate equation and organizing with respect to the storage time t.
  • C represents the amount of acetic acid
  • C max represents the maximum amount of acetic acid produced by hydrolysis of the added diacetin.
  • the conditions for calculating the acetic acid production rate constant are as follows. A mixture of the tobacco material and diacetin is prepared by adding 100 mg of diacetin to 100 mg (wet weight) of the tobacco material. The prepared mixture is stored for 2 months at 22 ° C. and 60% humidity. The mixture after storage is put into a screw tube, extracted with shaking with methanol solvent for 40 minutes, acetic acid is quantified by GC-MS, and acetic acid production rate constant is calculated according to the above formula.
  • Tobacco materials having acetic acid production rate constants as described above are obtained through a process of inactivating a hydrolase described later, in addition to tobacco engraving, a sheet obtained by pulverizing leaf tobacco into powder. be able to.
  • the type of leaf tobacco used as a tobacco material is not particularly limited, and examples include yellow, Burley, native, and regenerated tobacco.
  • the parts used are leaves (relaxed), stems, veins (neutral bone) ), Roots and flowers.
  • the equivalent sphere diameter is usually 1.5 mm or less, preferably by a measurement method using a projected cross-sectional area (for example, a method using Camsizer (Retsch)). Is 0.5 mm or less, and is usually 0.01 mm or more. In the case of using a tobacco cut, a tobacco leaf cut to a size (maximum diameter) of 0.01 to 100 mm can be used.
  • the raw material used for the acquisition of the tobacco material as described above is processed as the tobacco material so that the acetic acid rate constant is 1.25 ⁇ 10 ⁇ 8 s ⁇ 1 or less.
  • Examples of such treatment include a treatment that inactivates a hydrolase contained in a tobacco leaf or the like in a raw material that becomes a tobacco material, which affects the acetic acid production rate constant.
  • Examples of the treatment for inactivating the hydrolase in tobacco leaves include a treatment accompanied by a structural change of the protein constituting the enzyme, for example, a heat treatment. Specifically, an embodiment in which heating is performed at a temperature of 130 ° C. or more for 60 minutes or more can be given. When making temperature higher, you may reduce heating time suitably.
  • a physical treatment such as a treatment for drying at the same time as heating or a freeze-drying can also be mentioned.
  • a chemical treatment using a raw material that becomes a tobacco material in the presence of an organic solvent or adding an acid / base to a tobacco leaf can be mentioned.
  • the content of the tobacco material in the tobacco filling of the present invention is usually 20% by weight or more, preferably 30% by weight or more, more preferably 40% by weight or more, and usually 80% by weight or less, preferably 70% by weight or less. More preferably, it is 60% by weight or less.
  • the savory taste during use can be maintained satisfactorily, and the “savory taste inhibition feeling” can be more effectively suppressed.
  • the tobacco filling of the present invention includes an aerosol-generating liquid that includes at least one of diacetin and monoacetin.
  • an aerosol-generating liquid that includes at least one of diacetin and monoacetin.
  • the generated aerosol is less likely to volatilize due to intraoral dilution, and a component that becomes a hindrance when feeling the flavor component contained in the aerosol is less likely to change into the gas phase. Thereby, a feeling of savory taste inhibition is reduced.
  • the degree of volatilization of the generated aerosol by oral dilution is evaluated by measuring the “aerosol residual ratio after dilution”. The higher the aerosol remaining ratio after dilution, the lower the taste-inhibiting feeling.
  • the aerosol-generating liquid used in the present invention contains at least one of diacetin and monoacetin. About the content, it is 50 to 300 weight% as an additional amount of an aerosol production
  • the content of the aerosol-generating liquid containing at least one of diacetin and monoacetin is 50% by weight or more based on the tobacco material, it is possible to ensure an effective reduction in the taste inhibition feeling.
  • the upper limit of the content of the aerosol-generating liquid containing at least one of diacetin and monoacetin when the tobacco filler is used for a non-combustion type smoking article, the tobacco filler is heated smoothly. Furthermore, it is 300% by weight or less.
  • a commercially available “diacetin” solution contains about 42% by weight of diacetin and about 38% by weight of monoacetin.
  • the commercially available “monoacetin” solution contains about 45 wt% monoacetin and about 36 wt% diacetin. Therefore, for example, when a commercially available “diacetin” solution is added as a solution containing at least one of diacetin and monoacetin at 50% by weight with respect to the tobacco material, the diacetin content is about 21% relative to the tobacco material. %, And the monoacetin content is about 19% by weight.
  • the diacetin and monoacetin solutions contain a total of 81% by weight of diacetin and monoacetin, and the diacetin and monoacetin solution contain 81% by weight in total. become. Therefore, in the tobacco filling of the present invention, when 50% by weight of the commercially available “diacetin” solution or the commercially available “monoacetin” solution is added to the tobacco material, the total amount of diacetin and monoacetin is About 40% by weight.
  • the aerosol-generating liquid used in the present invention include an embodiment 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 required in addition to at least one of diacetin and monoacetin as described above.
  • examples thereof include acids having a first acid dissociation constant of 4.0 to 6.0 and a boiling point of 366 ° C. to 600 ° C. as shown below.
  • first acid dissociation constant means an acid dissociation constant into water at room temperature (25 ° C.).
  • boiling point means a boiling point at a pressure of 760 mmHg.
  • acids include ascorbic acid, isoascorbic acid, heneicosanoic acid, lignoceric acid, octacosanoic acid, and nonadecanoic acid.
  • ascorbic acid isoascorbic acid and the like are particularly preferable.
  • ascorbic acid isoascorbic acid and the like are particularly preferable.
  • it becomes easier to suppress the decrease in the evaporation amount of the flavor component, and the “feeling of flavor inhibition” can be more effectively suppressed.
  • the content thereof is usually 0.25% by weight or more, preferably 1% by weight or more, and usually 10% by weight or less.
  • it becomes easier to suppress a decrease in the evaporation amount of the flavor component, and the “feeling of flavor inhibition” can be further reduced.
  • additives other than the above-mentioned acids include polyhydric alcohols such as glycerin, propylene glycol, triethylene glycol, and tetraethylene glycol; carboxyls such as methyl stearate, dimethyl dodecanedioate, and dimethyl tetradecanedioate. Examples include oxyaliphatic esters. In addition, these components are not restricted to 1 type, You may use combining 2 or more types.
  • the amount of acetic acid in the tobacco filling after storage for more than 2 months only increases to 1.1% by weight or less with respect to the added weight of the added aerosol-generating liquid. It is expected. This is because the tobacco material has a low acetic acid production rate constant due to the deactivation of the hydrolase contained in the tobacco material as described above. Therefore, the tobacco filler of the present invention is also excellent in storage stability.
  • the cigarette filling of the present invention includes a cigarette cut and an aerosol-generating liquid.
  • components such as water contained in the cigarette cut out into the aerosol-generating liquid, so the cigarette filling of the present invention also contains water. It can be said that there is.
  • the water content of the tobacco filling of the present invention is usually 5% by weight or more, preferably 7.5% by weight or more, more preferably 10% by weight or more, and usually 30% by weight or less, preferably of the whole tobacco filling. Is 25% by weight or less, more preferably 20% by weight or less. Within the above range, the savory taste during use can be kept good, and the “savory taste inhibition feeling” can be more effectively suppressed.
  • the tobacco filler of the present invention may be distributed in a form filled in a container such as a pod (hereinafter also referred to as pod) shown below for use in a non-combustion type heated smoking article.
  • a pod hereinafter also referred to as pod
  • a known pod shape can be adopted at that time, and the material is not particularly limited, and a metal having high thermal conductivity such as aluminum can be used.
  • the amount of cigarette filling in the pod can be adjusted as appropriate according to the type of product sold.
  • the cigarette filler of the present invention is a cigarette filler for a non-combustion type heated smoking article containing a tobacco cigarette and an aerosol-generating liquid, and is a specific example of a non-combustion type heated smoking article filled with the cigarette filler of the present invention.
  • a structure is not particularly limited, and a known structure can be appropriately employed.
  • the non-combustion type heated smoking article include those having a structure like the non-combustion type heated smoking article 10 shown in FIG. FIG.
  • FIG. 8 is a cross-sectional view of a cylindrical non-combustion type heated smoking article 10 cut in the longitudinal direction, and has a structure including a battery 101, a pod 103 for containing a filler 102, a heater 104, and a mouthpiece 105. It has become.
  • the cigarette filling of the present invention is filled in the pod 103, and aerosol is generated by heating.
  • the heating temperature of the tobacco filler in the non-combustion type heated smoking article is usually 22 ° C. or higher, preferably 100 ° C. or higher, more preferably 150 ° C. or higher, and usually 350 ° C. or lower, preferably 300 ° C. or lower, more preferably 250. It is below °C.
  • the characteristics of the tobacco filler of the present invention are It can be used more effectively to solve the problem.
  • Examples 1 and 2 and Comparative Example 1-7 Verification of effect of changing aerosol-generating liquid>
  • the same yellow as the following Example 5 as a tobacco material (produced in Japan, hereinafter also simply referred to as “acetic acid rate constant: 1.17”).
  • a sample was prepared by adding 100 mg of various aerosol-generating liquids shown in Table 1 to 100 mg of ⁇ 10 ⁇ 8 s ⁇ 1 ).
  • the chopping is pulverized in advance with a home mixer, and then shaken with a sieve (AS200, manufactured by Retch) for 2 minutes under the condition: amplitude-1.5 mm / "g", and a chopping with a sieve diameter of 0.5 mm or less was used. .
  • the prepared sample was added so as to stick to a pod exclusive for the trade name “Ploom” sold by Japan Tobacco Inc., and stored under conditions of 22 ° C. and 60% humidity for 2 days or more.
  • the “diacetin” used in this example is a commercially available solution and contains about 42% by weight of diacetin and about 38% by weight of monoacetin as described above.
  • “monoacetin” used in this example is also a commercially available solution, and contains about 45 wt% monoacetin and about 36 wt% diacetin as described above.
  • the heating temperature at the time of using Ploom was about 160 ° C. to 170 ° C. by preliminary measurement using a thermocouple.
  • the difficulty of volatilizing aerosols which is important in measuring the reduction in the taste inhibition, is to measure the amount of aerosol before dilution and the amount of aerosol after dilution with clean air. It was evaluated by the “aerosol residual ratio after dilution”. The amount of aerosol before dilution was measured using a smoking machine (Borgwaldt, RM-26), and the prepared pod was attached to the Ploom, under the prescribed smoking conditions (55 ml / 2s, smoking interval 30s). The initial 5 puff was measured.
  • the amount of aerosol after dilution is measured by storing the aerosol generated by the same method as described above once in a SUS tube (volume: about 127 cc, length: 25.0 cm, inner diameter: 2.54 cm), and clean air. After making a pseudo dilution condition by circulating the gas, the amount of aerosol after removing the components present as the gas phase through the charcoal packed bed (100 mg) was measured by the Cambridge filter for the initial 5 puffs. . In addition, sensory evaluation of the prepared samples was performed by four people, and “flavoring taste sensation” was performed in a seven-step evaluation of 1 to 7. In the result of the present example, when the taste inhibition feeling is 2.0 or less, it is a value that can clearly identify the difference for the evaluator, and is a region where the effect is excellent.
  • FIG. 1 shows the relationship between the aerosol remaining ratio after dilution and the taste inhibition feeling when various aerosol-generating liquids shown in Table 1 are used. From FIG. 1, it can be seen that as the residual ratio of the aerosol after dilution increases, the taste inhibition feeling tends to decrease. That is, the generated aerosol is less likely to volatilize by intraoral dilution, and when the amount of aerosol remaining in the oral cavity is greater after intraoral dilution, the substance that becomes alienated when feeling the savory taste contained in the aerosol enters the gas phase. It is considered that the phase change is difficult and the savory taste inhibition is lowered. Since diacetin has a high aerosol residual ratio after dilution, it has been found that as a result, it is an aerosol-generating liquid that has the lowest sense of flavor inhibition.
  • a solution containing diacetin commercially available product
  • the amount of additive effective for reducing the taste inhibition feeling was examined.
  • a sample was prepared by adding diacetin and propylene glycol as a comparison to 100 mg of Burley chopping (produced in Japan). Samples were prepared in the same manner as in the previous examples, and stored for 2 days or longer at 22 ° C.
  • FIG. 2 shows the relationship between the added amount of the solution and the taste inhibition feeling with respect to the tobacco weight.
  • FIG. 2 shows that when the aerosol-generating liquid is not added to the cigarette (when the solution addition rate is 0% by weight with respect to the cigarette weight), the taste inhibition feeling is very high at 6.8.
  • ⁇ Reference Example 1-8 Investigation of formation mechanism of diacetin and monoacetin hydrolysis product (acetic acid)>
  • a hydrolysis product of diacetin and monoacetin 100 mg was added as a representative to 100 mg of tobacco (domestic yellow) and calcium carbonate (simulated without chopping).
  • the sample shown in Table 3 was evaluated for taste inhibition and the amount of acetic acid.
  • water was added as shown in Table 3. The sensory evaluation was performed by two people, and “Supura” was performed in a 7-step evaluation of 1-7.
  • the evaluator can identify the sourness, and the range of 1.5 or less is a region where the diacetin degradation inhibitory effect is excellent.
  • samples prepared under the conditions shown in Table 3 were stored for one week at 22 ° C. and 60% humidity, placed in a screw tube (No. 5, manufactured by Marem Co., Ltd.), and shaken with methanol solvent for 40 minutes. Finally extracted and quantified by GC-MS.
  • FIG. 3 A graph showing the relationship between the amount of water added and the amount of acetic acid produced is shown in FIG. From FIG. 3, in the sample in which diacetin is added to calcium carbonate, the amount of acetic acid in the sample pod shows a very low value regardless of the amount of water added. On the other hand, it was found that when diacetin was added to the cigarette, acetic acid was greatly generated in proportion to the amount of water added. Therefore, when only diacetin is stored (including calcium carbonate), the amount of water added has little effect on the degradation of diacetin, but when diacetin is stored in the presence of tobacco, the increase in the amount of water added causes the degradation of diacetin.
  • Examples 5 and 6 and Comparative Examples 15-17 Verification of hydrolysis inhibition method> From the previous examples, it was found that the hydrolase in the tobacco was used as a catalyst to produce acetic acid, which is a hydrolysis product of diacetin. Here, as a method for inactivating the hydrolase, the effect of inhibiting hydrolysis of diacetin was typically verified by a heat treatment generally performed. Tobacco engraved heat treatment method, 2g of cigarette engraving (domestic yellow engraving) is put into a screw tube (No.
  • FIG. 5 is a graph showing the relationship between the storage days and the amount of acetic acid in the Pod. From FIG. 5, in the case of no heating, the amount of acetic acid in the Pod increases significantly with respect to the number of days of storage, whereas the amount of acetic acid generated in the Pod is increased by preheating only the tobacco. It turns out that it has decreased. Here, in the case of no heating, acetic acid production increased sharply until the storage period was 21 days (3 weeks), while acetic acid was increased from 21 days to 60 days (2 months).
  • the rate of increase in the amount is small, the rate of acetic acid production due to diacetin degradation decreases, and the amount of acetic acid is asymptotic to the maximum amount of acetic acid produced by hydrolysis of diacetin. Therefore, the acetic acid production amount (8.90 mg / pod) after storage for 2 months without heating is approximated to the maximum acetic acid production amount (C max ) due to hydrolysis of diacetin added in the pod.
  • amount of acetic maximum acid production amount of (C) the value obtained by dividing by (C max) is defined as acetic acid production ratio (C / C max).
  • FIG. 7 shows a graph plotting the above equation for each heating temperature condition. From FIG. 7, the acetic acid acetic acid production rate constant k was calculated from the slope of the plot from storage days 1 to 21. Note that the graph of FIG. 7 does not pass through the origin because acetic acid is slightly contained in the tobacco cut. According to Table 4 where the acetic acid production rate constant k was calculated, the acetic acid production rate constant was 1.17 ⁇ 10 ⁇ 8 s ⁇ 1 or less.
  • the hydrolysis of diacetin can be suppressed by using a cigarette with an acetic acid production rate constant of 1.17 ⁇ 10 ⁇ 8 s ⁇ 1 or less together with diacetin.
  • the acetic acid production rate constant corresponding to the sourness 1.5 can be estimated as 1.25 ⁇ 10 ⁇ 8 s ⁇ 1
  • the decomposition inhibiting effect is that the acetic acid production rate constant of the tobacco material is 1.25 ⁇ 10 ⁇ 8. It is considered that a sufficient value can be secured when s ⁇ 1 or less.
  • the tobacco filling of the present invention can be used for smoking by filling a container such as a pod used for a non-combustion type heated smoking article.

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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Abstract

The purpose of the present invention is to provide a tobacco filler that can maintain a good smoking flavor and yet reduce "a feeling of lessened smoking flavor" in a non-combustion type heat smoking article served in the form of a tobacco material-containing filler to be heated. Provided is a tobacco filler for a non-combustion type heat smoking article, said tobacco filler containing a tobacco material and an aerosol-forming liquid, wherein the aerosol-forming liquid contains diacetin and/or monoacetin and the acetic acid production rate constant of the tobacco material is 1.25×10-8s-1 or less.

Description

非燃焼型加熱喫煙物品用のたばこ充填物Tobacco fillings for non-combustion heated smoking articles
 本発明は、非燃焼型加熱喫煙物品に充填して使用する非燃焼型加熱喫煙物品用のたばこ充填物に関する。 The present invention relates to a tobacco filling for a non-combustion type heated smoking article to be used by filling the non-combustion type heated smoking article.
 近年、シガレットに代わり、たばこを燃焼させることなく、香喫味を味わう非燃焼型加熱喫煙物品が開発されており、代表的なものとして、ポッド状の容器内部に香喫味成分とエアロゾルを発生させる成分を充填して使用する形態のものや先端に熱源を備えたものなどが知られている。
 また、このような非燃焼型加熱喫煙物品において、充填物にグリセリン、トリエチレングリコール及びプロピレングリコールを添加する技術も報告されている(特許文献1参照。)。
In recent years, instead of cigarettes, non-combustion-type heated smoking articles have been developed that allow you to taste the savory taste without burning cigarettes, and as a typical example, ingredients that generate a savory taste component and aerosol inside the pod-shaped container The thing of the form which is filled and used, the thing provided with the heat source at the front-end | tip, etc. are known.
In addition, in such a non-combustion type heated smoking article, a technique of adding glycerin, triethylene glycol, and propylene glycol to a filler has also been reported (see Patent Document 1).
特開昭63-148975号公報JP-A 63-148975
 非燃焼型加熱喫煙物品を使用した喫煙においては、香喫味成分の十分な蒸発量が求められるとともに、いわゆる「香喫味阻害感」を低減することが求められている。
 例えば、上述した特許文献1では、グリセリン、トリエチレングリコール、プロピレングリコールをエアロゾル生成液体として用いたときに、香喫味が良好になることが記載されている。一方で、特許文献1の発明で添加するプロピレングリコールについては、沸点が低く蒸気圧が高いため、口腔内で容易に揮発しやすい性質がある。そのため、エアロゾル中に含まれていたプロピレングリコール以外の成分も揮発しやすい雰囲気となり、プロピレングリコールと同様にガス相へと相変化する。これらの揮発した成分には、香喫味成分の他に香喫味を感じる際に阻害となる物質も含まれるため、香喫味の阻害感をなくすためには、プロピレングリコールの生成量自体を大幅に増加させるか、揮発しにくいエアロゾル生成液体へと変更する必要が生じる。
 このことから、本発明では、良好な香喫味を維持するとともに、「香喫味阻害感」を抑制することができる非燃焼型加熱喫煙物品用のたばこ充填物を提供することを目的とする。
In smoking using a non-combustion type heated smoking article, a sufficient amount of evaporation of the flavor component is required, and so-called “flavor inhibition feeling” is required to be reduced.
For example, Patent Document 1 described above describes that when glycerin, triethylene glycol, and propylene glycol are used as the aerosol-generating liquid, the flavor is improved. On the other hand, the propylene glycol added in the invention of Patent Document 1 has a property of being easily volatilized in the oral cavity because of its low boiling point and high vapor pressure. For this reason, an atmosphere other than propylene glycol contained in the aerosol is also easily volatilized, and changes into a gas phase in the same manner as propylene glycol. These volatilized components include substances that interfere with the savory taste in addition to the savory savory ingredients. Therefore, to eliminate the sense of savory taste, the amount of propylene glycol produced is greatly increased. Or change to an aerosol-generating liquid that is less volatile.
Accordingly, an object of the present invention is to provide a tobacco filling for a non-combustion-type heated smoking article that can maintain a good flavor and suppress the “feel of flavor inhibition”.
 本発明者らは、前記の課題を解決すべく鋭意検討を重ねた結果、たばこ充填物にジアセチン及びモノアセチンの少なくとも一方を含むエアロゾル生成液体を添加し、たばこ材料として酢酸生成速度定数が1.25×10-8-1以下であるものを用いることで、上記課題を解決できることを見出し、本発明を完成させた。
 即ち、本発明は以下の通りである。
[1] たばこ材料とエアロゾル生成液体とを含む非燃焼型加熱喫煙物品用のたばこ充填物であって、
 エアロゾル生成液体がジアセチン及びモノアセチンの少なくとも一方を含み、
 たばこ材料の酢酸生成速度定数が1.25×10-8 s-1以下であり、エアロゾル生成液体の添加量が、たばこ材料の重量に対して50重量%以上300重量%以下である、たばこ充填物。
[2] エアロゾル生成液体が、ジアセチンとモノアセチンの両方を含む、[1]に記載のたばこ充填物。
[3] エアロゾル生成液体における、ジアセチン及びモノアセチンの含有量の合計が50重量%以上である、[1]または[2]に記載のたばこ充填物。
[4] [1]~[3]のいずれかに記載のたばこ充填物が充填された、非燃焼型加熱喫煙物品用のポッド。
[5] [1]~[3]のいずれかに記載のたばこ充填物を含む、非燃焼型加熱喫煙物品。
As a result of intensive investigations to solve the above-mentioned problems, the present inventors have added an aerosol-generating liquid containing at least one of diacetin and monoacetin to a tobacco filling, and an acetic acid production rate constant as a tobacco material is 1.25. It has been found that the above problems can be solved by using a material having a value of × 10 −8 s −1 or less, and the present invention has been completed.
That is, the present invention is as follows.
[1] A tobacco filler for a non-combustion type 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 production rate constant of the tobacco material is 1.25 × 10 −8 s −1 or less, and the amount of the aerosol-generating liquid added is 50% by weight to 300% by weight with respect to the weight of the tobacco material. object.
[2] The tobacco filling according to [1], wherein the aerosol-generating liquid contains both diacetin and monoacetin.
[3] The tobacco filling 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 pod for a non-combustion type heated 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 filling according to any one of [1] to [3].
 本発明によれば、たばこ材料を含んだ充填物を加熱する形態の非燃焼型加熱喫煙物品において、良好な香喫味を維持しつつ、「香喫味阻害感」を抑制することができる。 According to the present invention, in the non-combustion type heated smoking article in the form of heating the filling containing the tobacco material, it is possible to suppress the “feeling of flavor inhibition” while maintaining a good flavor.
希釈後エアロゾル残存率と香喫味阻害感の関係を示す図である。It is a figure which shows the relationship between the aerosol remaining rate after dilution, and a savory taste inhibition feeling. ジアセチン添加量と香喫味阻害感の関係を示す図である。It is a figure which shows the relationship between a diacetin addition amount and a flavor inhibition feeling. 水分添加量と酢酸量の関係を示す図である。It is a figure which shows the relationship between the moisture addition amount and the amount of acetic acid. 酢酸量とすっぱさの関係を示す図である。It is a figure which shows the relationship between the amount of acetic acid and sourness. 蔵置日数と酢酸生成量の関係を示す図である。It is a figure which shows the relationship between storage days and an acetic acid production amount. 蔵置日数と酢酸生成割合の関係を示す図である。It is a figure which shows the relationship between storage days and an acetic acid production | generation ratio. 蔵置日数と-ln(1-C/Cmax)の関係を示す図である。It is a figure which shows the relationship between storage days and -ln (1-C / Cmax ). 非燃焼型加熱喫煙物品の例を表した断面図である。It is sectional drawing showing the example of the non-combustion type heating smoking article.
 本発明を説明するに当たり、具体例を挙げて説明するが、本発明の趣旨を逸脱しない限り以下の内容に限定されるものではなく、適宜変更して実施することができる。 In describing the present invention, specific examples will be described. However, the present invention is not limited to the following contents without departing from the gist of the present invention, and can be implemented with appropriate modifications.
<非燃焼型加熱喫煙物品用のたばこ充填物>
 本発明の一態様である非燃焼型加熱喫煙物品用のたばこ充填物(以下、「本発明のたばこ充填物」と略す場合がある。)は、酢酸生成速度定数が1.25×10-8-1以下であるたばこ材料と、ジアセチン及びモノアセチンの少なくとも一方を含むエアロゾル生成液体とを含み、エアロゾル生成液体の添加量が、たばこ材料の重量に対して50重量%以上300重量%以下であるたばこ充填物である。
<Tobacco filling for non-combustion type heated smoking article>
The tobacco filler for non-combustion type heated smoking articles which is one embodiment of the present invention (hereinafter sometimes abbreviated as “the tobacco filler of the present invention”) has an acetic acid production rate constant of 1.25 × 10 −8. s −1 or less of the tobacco material and an aerosol-generating liquid containing at least one of diacetin and monoacetin, and the added amount of the aerosol-generating liquid is not less than 50% by weight and not more than 300% by weight of the weight of the tobacco material Tobacco filling.
 <たばこ材料の酢酸生成速度定数>
 本発明のたばこ充填物に含まれるたばこ材料は、その酢酸生成速度定数が、1.25×10-8-1以下である。
 たばこ材料の酢酸生成速度定数が、1.25×10-8-1以下であることで、たばこ充填物に含まれるたばこ材料の加水分解酵素(アセチルエステラーゼ)の活性が十分に抑制され、たばこ充填物の蔵置時に、モノアセチンやジアセチンが加水分解することにより生成する酢酸の生成量が抑制される。これにより、たばこ充填物の使用時の香喫味の悪化を防止することができる。
 たばこ材料の酢酸生成速度定数は、1.17×10-8-1以下であることがより好ましく、1.00×10-8-1以下であることが特に好ましい。
<Acetic acid production rate constant of tobacco material>
The tobacco material contained in the tobacco packing of the present invention has an acetic acid production rate constant of 1.25 × 10 −8 s −1 or less.
When the acetic acid production rate constant of the tobacco material is 1.25 × 10 −8 s −1 or less, the activity of the hydrolase (acetylesterase) of the tobacco material contained in the tobacco packing is sufficiently suppressed, and the tobacco During storage of the filling, the amount of acetic acid produced by hydrolysis of monoacetin and diacetin is suppressed. Thereby, the deterioration of the flavor at the time of use of a tobacco filling can be prevented.
The acetic acid production rate constant of the tobacco material is more preferably 1.17 × 10 −8 s −1 or less, and particularly preferably 1.00 × 10 −8 s −1 or less.
 後述する実施例で確認した蔵置日数に対する酢酸生成割合の関係を示す図6より、蔵置日数が21日までの酢酸の生成(ジアセチンの分解)は一次反応の挙動を示す。これにより、酢酸生成速度定数kを、以下の一次反応速度式とし、蔵置日数tに対して整理すると以下のように表すことができる。 From FIG. 6 showing the relationship of acetic acid production rate to the storage days confirmed in the examples described later, the production of acetic acid (diacetin decomposition) up to 21 days of storage shows the behavior of the primary reaction. As a result, the acetic acid production rate constant k can be expressed as follows by arranging the acetic acid production rate constant k as the following first-order reaction rate equation and organizing with respect to the storage time t.
Figure JPOXMLDOC01-appb-C000001

上記式において、Cは酢酸量、Cmaxは添加したジアセチンが加水分解して生成する最大酢酸量を示す。
Figure JPOXMLDOC01-appb-C000001

In the above formula, C represents the amount of acetic acid, and C max represents the maximum amount of acetic acid produced by hydrolysis of the added diacetin.
 酢酸生成速度定数を算出するための条件は、以下の通りである。
 たばこ材料100mg(湿重量)に対して、ジアセチンを100mg添加することでたばこ材料とジアセチンの混合物を調製する。
 調製した混合物を2ヶ月22℃、湿度60%の条件で蔵置する。
蔵置後の混合物をスクリュー管に入れ、メタノール溶媒で40分間振とう抽出し、GC-MSで酢酸の定量を行い、上記の式に従って、酢酸生成速度定数を算出する。
The conditions for calculating the acetic acid production rate constant are as follows.
A mixture of the tobacco material and diacetin is prepared by adding 100 mg of diacetin to 100 mg (wet weight) of the tobacco material.
The prepared mixture is stored for 2 months at 22 ° C. and 60% humidity.
The mixture after storage is put into a screw tube, extracted with shaking with methanol solvent for 40 minutes, acetic acid is quantified by GC-MS, and acetic acid production rate constant is calculated according to the above formula.
 上記のような酢酸生成速度定数を有するたばこ材料は、たばこ刻のほか、葉たばこを粉末状に粉砕した後に成形して得られるシート状のものを後述する加水分解酵素を失活させる処理を経て得ることができる。
 たばこ材料として用いる葉たばこの種類は特に制限されず、黄色種、バーレー種、在来種、再生たばこ等が挙げられ、また使用する部位としては、葉(緩和刻)、茎、葉脈(中骨刻)、根、花等が挙げられる。
Tobacco materials having acetic acid production rate constants as described above are obtained through a process of inactivating a hydrolase described later, in addition to tobacco engraving, a sheet obtained by pulverizing leaf tobacco into powder. be able to.
The type of leaf tobacco used as a tobacco material is not particularly limited, and examples include yellow, Burley, native, and regenerated tobacco. The parts used are leaves (relaxed), stems, veins (neutral bone) ), Roots and flowers.
 たばこ刻の寸法は、限定されるものではないが、投影断面積を用いた測定方法(例えば、Camsizer(Retsch社)などを用いた方法)にて、球相当径が通常1.5mm以下、好ましくは0.5mm以下であり、通常0.01mm以上である。
 たばこ刻を使用する場合、たばこ葉を、0.01~100mmの大きさ(最大径)に裁断したものを用いることができる。
Although the size of the cigarette is not limited, the equivalent sphere diameter is usually 1.5 mm or less, preferably by a measurement method using a projected cross-sectional area (for example, a method using Camsizer (Retsch)). Is 0.5 mm or less, and is usually 0.01 mm or more.
In the case of using a tobacco cut, a tobacco leaf cut to a size (maximum diameter) of 0.01 to 100 mm can be used.
 本発明では、上記のようなたばこ材料の取得のために用いる原料を、酢酸速度定数が1.25×10-8-1以下になるように処理したものをたばこ材料として用いる。
 そのような処理としては、酢酸生成速度定数に影響を与える、たばこ材料になる原料中のたばこ葉等に含まれる加水分解酵素を失活させる処理を挙げることができる。
 たばこ葉中の加水分解酵素を失活させる処理としては、酵素を構成するタンパク質の構造変化を伴う処理を挙げることができ、例えば加熱処理を挙げることができる。具体的には、130℃以上の温度で、60分以上加熱させる態様を挙げることができる。温度をより高温にする場合には、加熱時間を適宜減らしてもよい。
 また、加水分解酵素を失活させる別の処理としては、加熱と同時に乾燥させる処理や凍結乾燥などの物理的処理を挙げることもできる。
 さらに別の処理としては、有機溶媒の存在下でたばこ材料となる原料を使用したり、たばこ葉に酸/塩基を加えたりする化学的処理を挙げることができる。
In the present invention, the raw material used for the acquisition of the tobacco material as described above is processed as the tobacco material so that the acetic acid rate constant is 1.25 × 10 −8 s −1 or less.
Examples of such treatment include a treatment that inactivates a hydrolase contained in a tobacco leaf or the like in a raw material that becomes a tobacco material, which affects the acetic acid production rate constant.
Examples of the treatment for inactivating the hydrolase in tobacco leaves include a treatment accompanied by a structural change of the protein constituting the enzyme, for example, a heat treatment. Specifically, an embodiment in which heating is performed at a temperature of 130 ° C. or more for 60 minutes or more can be given. When making temperature higher, you may reduce heating time suitably.
Further, as another treatment for inactivating the hydrolase, a physical treatment such as a treatment for drying at the same time as heating or a freeze-drying can also be mentioned.
As another treatment, a chemical treatment using a raw material that becomes a tobacco material in the presence of an organic solvent or adding an acid / base to a tobacco leaf can be mentioned.
 本発明のたばこ充填物における、たばこ材料の含有量は、通常20重量%以上、好ましくは30重量%以上、より好ましくは40重量%以上であり、通常80重量%以下、好ましくは70重量%以下、より好ましくは60重量%以下である。上記範囲内であると、使用時の香喫味を良好に維持できるとともに、「香喫味阻害感」をより効果的に抑制することができる。 The content of the tobacco material in the tobacco filling of the present invention is usually 20% by weight or more, preferably 30% by weight or more, more preferably 40% by weight or more, and usually 80% by weight or less, preferably 70% by weight or less. More preferably, it is 60% by weight or less. Within the above range, the savory taste during use can be maintained satisfactorily, and the “savory taste inhibition feeling” can be more effectively suppressed.
 本発明のたばこ充填物は、ジアセチン及びモノアセチンの少なくとも一方を含むエアロゾル生成液体を含む。
 後述する実施例で示すように、本発明のたばこ充填物にジアセチン及びモノアセチンの少なくとも一方を含むエアロゾル生成液体が含まれることで、本発明のたばこ充填物を含む非燃焼型喫煙物品を使用した際に、生成するエアロゾルが口腔内希釈によって揮発しにくくなり、エアロゾルに含まれていた香喫味成分を感じる際に阻害となる成分がガス相に相変化しにくくなる。これにより、香喫味阻害感が低減される。
 本発明では、生成するエアロゾルが口腔内希釈による揮発の程度を「希釈後エアロゾル残存率」を測定することで評価している。この希釈後エアロゾル残存率が高いほど、香喫味阻害感が低いことを示す。
The tobacco filling of the present invention includes an aerosol-generating liquid that includes at least one of diacetin and monoacetin.
As shown in the examples to be described later, when the non-combustible smoking article containing the tobacco filler of the present invention is used by including the aerosol-generating liquid containing at least one of diacetin and monoacetin in the tobacco filler of the present invention. In addition, the generated aerosol is less likely to volatilize due to intraoral dilution, and a component that becomes a hindrance when feeling the flavor component contained in the aerosol is less likely to change into the gas phase. Thereby, a feeling of savory taste inhibition is reduced.
In the present invention, the degree of volatilization of the generated aerosol by oral dilution is evaluated by measuring the “aerosol residual ratio after dilution”. The higher the aerosol remaining ratio after dilution, the lower the taste-inhibiting feeling.
 本発明で用いるエアロゾル生成液体には、ジアセチン及びモノアセチンの少なくとも一方を含む。
 その含有量については、たばこ充填物に含まれるたばこ材料に対し、エアロゾル生成液体の添加量として50重量%以上、300重量%以下である。
 ジアセチン及びモノアセチンの少なくとも一方を含むエアロゾル生成液体の含有量として、たばこ材料に対して50重量%以上であることで、香喫味阻害感の効果的な低減を確保できる。
 一方、ジアセチン及びモノアセチンの少なくとも一方を含むエアロゾル生成液体の含有量の上限については、たばこ充填物を非燃焼型喫煙物品に使用した際に、たばこ充填物の加熱がスムーズに行われるようにするために、300重量%以下である。
The aerosol-generating liquid used in the present invention contains at least one of diacetin and monoacetin.
About the content, it is 50 to 300 weight% as an additional amount of an aerosol production | generation liquid with respect to the tobacco material contained in a tobacco filling.
When the content of the aerosol-generating liquid containing at least one of diacetin and monoacetin is 50% by weight or more based on the tobacco material, it is possible to ensure an effective reduction in the taste inhibition feeling.
On the other hand, regarding the upper limit of the content of the aerosol-generating liquid containing at least one of diacetin and monoacetin, when the tobacco filler is used for a non-combustion type smoking article, the tobacco filler is heated smoothly. Furthermore, it is 300% by weight or less.
 なお、ジアセチンやモノアセチンは、それぞれを単独で含む液体を調製することは難しく、市販の「ジアセチン」溶液はジアセチンを約42重量%、モノアセチンを約38重量%含む。一方、市販の「モノアセチン」溶液は、モノアセチンを約45重量%、ジアセチンを約36重量%含んでいる。
 このことから、例えば市販の「ジアセチン」溶液を、ジアセチン及びモノアセチンの少なくとも一方を含む溶液として、たばこ材料に対して50重量%添加する場合には、ジアセチンの含有量がたばこ材料に対して約21重量%となり、モノアセチンの含有量が約19重量%になる。
 また、「ジアセチン」の市販品の溶液には、ジアセチンとモノアセチンが合計で81重量%含まれ、「モノアセチン」の市販品の溶液には、ジアセチンとモノアセチンが合計で81重量%含まれていることになる。
 したがって、本発明のたばこ充填物において、市販品の「ジアセチン」溶液または市販品の「モノアセチン」溶液をたばこ材料に対して50重量%添加する場合、ジアセチン及びモノアセチンの合計量は、たばこ材料に対して約40重量%になる。
 本発明で用いるエアロゾル生成液体では、ジアセチンとモノアセチンの両方を含む態様を挙げることができる。
 本発明で用いるエアロゾル生成液体における、ジアセチン及びモノアセチンの含有量の合計は、50重量%以上であることが好ましく、70重量%以上であることがより好ましく、75重量%以上であることが特に好ましい。
In addition, it is difficult to prepare a liquid containing diacetin and monoacetin alone, and a commercially available “diacetin” solution contains about 42% by weight of diacetin and about 38% by weight of monoacetin. On the other hand, the commercially available “monoacetin” solution contains about 45 wt% monoacetin and about 36 wt% diacetin.
Therefore, for example, when a commercially available “diacetin” solution is added as a solution containing at least one of diacetin and monoacetin at 50% by weight with respect to the tobacco material, the diacetin content is about 21% relative to the tobacco material. %, And the monoacetin content is about 19% by weight.
In addition, the diacetin and monoacetin solutions contain a total of 81% by weight of diacetin and monoacetin, and the diacetin and monoacetin solution contain 81% by weight in total. become.
Therefore, in the tobacco filling of the present invention, when 50% by weight of the commercially available “diacetin” solution or the commercially available “monoacetin” solution is added to the tobacco material, the total amount of diacetin and monoacetin is About 40% by weight.
Examples of the aerosol-generating liquid used in the present invention include an embodiment 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. .
 エアロゾル生成液体には、上記のようなジアセチン及びモノアセチンの少なくとも一方以外にも、必要に応じて他の成分が含まれていてもよい。
 例えば、以下に示すような第一酸解離定数が4.0以上6.0以下、かつ沸点が366℃以上600℃以下である酸を挙げることができる。なお、「第一酸解離定数」とは、常温(25℃)における水への酸解離定数を意味するものとする。
 また、「沸点」とは、圧力が760mmHgにおける沸点を意味するものとする。
 そのような酸としては、アスコルビン酸、イソアスコルビン酸、ヘンエイコサン酸、リグノセリン酸、オクタコサン酸、ノナデカン酸等が挙げられる。
 この中でも、アスコルビン酸、イソアスコルビン酸等が特に好ましい。
 上記のようなものであると、香喫味成分の蒸発量の低下をより抑制し易くなるとともに、「香喫味阻害感」をより効果的に抑制することができる。
The aerosol-generating liquid may contain other components as required in addition to at least one of diacetin and monoacetin as described above.
Examples thereof include acids having a first acid dissociation constant of 4.0 to 6.0 and a boiling point of 366 ° C. to 600 ° C. as shown below. Note that the “first acid dissociation constant” means an acid dissociation constant into water at room temperature (25 ° C.).
Further, the “boiling point” means a boiling point at a pressure of 760 mmHg.
Examples of such acids include ascorbic acid, isoascorbic acid, heneicosanoic acid, lignoceric acid, octacosanoic acid, and nonadecanoic acid.
Among these, ascorbic acid, isoascorbic acid and the like are particularly preferable.
When it is as described above, it becomes easier to suppress the decrease in the evaporation amount of the flavor component, and the “feeling of flavor inhibition” can be more effectively suppressed.
 本発明のたばこ充填物に、上記の酸を含有させる場合、その含有量は、通常0.25重量%以上、好ましくは1重量%以上であり、通常10重量%以下である。上記範囲内であると、香喫味成分の蒸発量の低下をより抑制し易くなるとともに、「香喫味阻害感」をよりよく低減できる。 When the above-mentioned acid is contained in the tobacco packing of the present invention, 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 it is within the above range, it becomes easier to suppress a decrease in the evaporation amount of the flavor component, and the “feeling of flavor inhibition” can be further reduced.
 また、上記のような酸以外の他の添加物としては、グリセリン、プロピレングリコール、トリエチレングリコール、テトラエチレングリコール等の多価アルコール;ステアリン酸メチル、ドデカン二酸ジメチル、テトラデカン二酸ジメチル等のカルボン酸脂肪族エステルが挙げられる。
 なお、これらの成分は1種類に限られず、2種類以上を組み合せて使用してもよい。
Examples of additives other than the above-mentioned acids include polyhydric alcohols such as glycerin, propylene glycol, triethylene glycol, and tetraethylene glycol; carboxyls such as methyl stearate, dimethyl dodecanedioate, and dimethyl tetradecanedioate. Examples include oxyaliphatic esters.
In addition, these components are not restricted to 1 type, You may use combining 2 or more types.
 本発明のたばこ充填物は、その調製後、蔵置2か月以上経過後のたばこ充填物における酢酸量が、添加したエアロゾル生成液体の添加重量に対して1.1重量%以下にまでしか増加しないことが見込まれる。これは、上述したようにたばこ材料に含まれていた加水分解酵素が失活することで、たばこ材料が低い酢酸生成速度定数を有することによるものである。
 したがって、本発明のたばこ充填物は、その保存安定性にも優れる。
After the preparation of the tobacco filling of the present invention, the amount of acetic acid in the tobacco filling after storage for more than 2 months only increases to 1.1% by weight or less with respect to the added weight of the added aerosol-generating liquid. It is expected. This is because the tobacco material has a low acetic acid production rate constant due to the deactivation of the hydrolase contained in the tobacco material as described above.
Therefore, the tobacco filler of the present invention is also excellent in storage stability.
 本発明のたばこ充填物は、たばこ刻とエアロゾル生成液体とを含むものであるが、通常たばこ刻に含まれる水等の成分がエアロゾル生成液体に溶け出すため、本発明のたばこ充填物も水を含んでいるものと言える。
 本発明のたばこ充填物の水の含有量は、たばこ充填物全体の通常5重量%以上、好ましくは7.5重量%以上、より好ましくは10重量%以上であり、通常30重量%以下、好ましくは25重量%以下、より好ましくは20重量%以下である。上記範囲内であると、使用時の香喫味を良好に保つとともに、「香喫味阻害感」をより効果的に抑制することができる。
The cigarette filling of the present invention includes a cigarette cut and an aerosol-generating liquid. Usually, components such as water contained in the cigarette cut out into the aerosol-generating liquid, so the cigarette filling of the present invention also contains water. It can be said that there is.
The water content of the tobacco filling of the present invention is usually 5% by weight or more, preferably 7.5% by weight or more, more preferably 10% by weight or more, and usually 30% by weight or less, preferably of the whole tobacco filling. Is 25% by weight or less, more preferably 20% by weight or less. Within the above range, the savory taste during use can be kept good, and the “savory taste inhibition feeling” can be more effectively suppressed.
 本発明のたばこ充填物は、非燃焼型加熱喫煙物品に用いるために、以下で示すポッド(以下、podとも表記する)のような容器に充填された形態で流通することがある。その際のポッドの形状については公知のものを採用することができ、その材質としても特に制限されず、アルミなどの熱伝導性の高い金属を用いることができる。
 ポッドに充填されるたばこ充填物の量は、販売製品の種類に応じて適宜調整することができる。
The tobacco filler of the present invention may be distributed in a form filled in a container such as a pod (hereinafter also referred to as pod) shown below for use in a non-combustion type heated smoking article. A known pod shape can be adopted at that time, and the material is not particularly limited, and a metal having high thermal conductivity such as aluminum can be used.
The amount of cigarette filling in the pod can be adjusted as appropriate according to the type of product sold.
 本発明のたばこ充填物は、たばこ刻とエアロゾル生成液体とを含む非燃焼型加熱喫煙物品用のたばこ充填物であるが、本発明のたばこ充填物を充填する非燃焼型加熱喫煙物品の具体的な構造等は、特に限定されず、公知のものを適宜採用することができる。以下、具体例を挙げて説明する。
 非燃焼型加熱喫煙物品としては、図8に示される非燃焼型加熱喫煙物品10のような構造を有するものが挙げられる。図8は、円筒形の非燃焼型加熱喫煙物品10をその長手方向に切断した場合の断面図であり、バッテリー101と充填物102を入れるポッド103およびヒーター104とマウスピース105を有した構造となっている。本発明のたばこ充填物をポッド103に充填して、加熱によりエアロゾルが発生することとなる。
 非燃焼型加熱喫煙物品におけるたばこ充填物の加熱温度は、通常22℃以上、好ましくは100℃以上、より好ましくは150℃以上であり、通常350℃以下、好ましくは300℃以下、より好ましくは250℃以下である。たばこ充填物の加熱温度が上記範囲内である非燃焼型加熱喫煙物品に本発明のたばこ充填物を用いた場合、本発明のたばこ充填物の特性を、「香喫味阻害感」についての課題を解決するために、より有効に活用することができる。
The cigarette filler of the present invention is a cigarette filler for a non-combustion type heated smoking article containing a tobacco cigarette and an aerosol-generating liquid, and is a specific example of a non-combustion type heated smoking article filled with the cigarette filler of the present invention. Such a structure is not particularly limited, and a known structure can be appropriately employed. Hereinafter, a specific example will be described.
Examples of the non-combustion type heated smoking article include those having a structure like the non-combustion type heated smoking article 10 shown in FIG. FIG. 8 is a cross-sectional view of a cylindrical non-combustion type heated smoking article 10 cut in the longitudinal direction, and has a structure including a battery 101, a pod 103 for containing a filler 102, a heater 104, and a mouthpiece 105. It has become. The cigarette filling of the present invention is filled in the pod 103, and aerosol is generated by heating.
The heating temperature of the tobacco filler in the non-combustion type heated smoking article is usually 22 ° C. or higher, preferably 100 ° C. or higher, more preferably 150 ° C. or higher, and usually 350 ° C. or lower, preferably 300 ° C. or lower, more preferably 250. It is below ℃. When the tobacco filler of the present invention is used for a non-combustion-type heated smoking article whose heating temperature is within the above range, the characteristics of the tobacco filler of the present invention are It can be used more effectively to solve the problem.
 以下に実施例を挙げて本発明をさらに具体的に説明するが、本発明の趣旨を逸脱しない限り適宜変更することができる。 Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention can be modified as appropriate without departing from the spirit of the present invention.
<実施例1、2および比較例1-7:エアロゾル生成液体変更の効果検証>
 エアロゾル生成液体を変更した場合の香喫味阻害感低減の効果を検証するため、たばこ材料として以下の実施例5と同じ黄色刻(日本産、以下、単に刻ともいう。酢酸速度定数:1.17×10-8-1)100mgに、表1に示す各種エアロゾル生成液体を100mg添加したサンプルを作製した。
 刻は予め家庭用ミキサーにて粉砕した後、ふるい(AS200、 Retch社製)にて条件: amplitude-1.5 mm/”g”において2分間振動させ、ふるい目径0.5mm以下の刻を使用した。調製したサンプルは日本たばこ産業株式会社から発売されている商品名「Ploom」専用のpodに張り付ける様に添加し、2日以上22℃、湿度60%の条件で蔵置した。
 なお、本実施例で使用した「ジアセチン」は市販品の溶液であり、上記の通りジアセチンを約42重量%、モノアセチンを約38重量%含む。一方、「本実施例で使用した「モノアセチン」も市販品の溶液であり、上記の通りモノアセチンを約45重量%、ジアセチンを約36重量%含む。
<Examples 1 and 2 and Comparative Example 1-7: Verification of effect of changing aerosol-generating liquid>
In order to verify the effect of reducing the taste-inhibiting feeling when the aerosol-generating liquid is changed, the same yellow as the following Example 5 as a tobacco material (produced in Japan, hereinafter also simply referred to as “acetic acid rate constant: 1.17”). A sample was prepared by adding 100 mg of various aerosol-generating liquids shown in Table 1 to 100 mg of × 10 −8 s −1 ).
The chopping is pulverized in advance with a home mixer, and then shaken with a sieve (AS200, manufactured by Retch) for 2 minutes under the condition: amplitude-1.5 mm / "g", and a chopping with a sieve diameter of 0.5 mm or less was used. . The prepared sample was added so as to stick to a pod exclusive for the trade name “Ploom” sold by Japan Tobacco Inc., and stored under conditions of 22 ° C. and 60% humidity for 2 days or more.
The “diacetin” used in this example is a commercially available solution and contains about 42% by weight of diacetin and about 38% by weight of monoacetin as described above. On the other hand, “monoacetin” used in this example is also a commercially available solution, and contains about 45 wt% monoacetin and about 36 wt% diacetin as described above.
 なお、Ploomを用いた際における刻の加熱温度(安定稼働時)は、熱電対を用いた事前の計測により160℃~170℃程度であることを確認した。
 前述した通り、香喫味阻害感の低減を測る上で重要となる「エアロゾルの揮発のしにくさ」は、希釈前のエアロゾル量と清浄空気により希釈した後のエアロゾル量をそれぞれ測定し、その比である「希釈後エアロゾル残存率」によって評価した。なお、希釈前のエアロゾル量の測定は、喫煙機(Borgwaldt, RM-26)を用いて実施し、作製したpodをPloomに装着し、規程の喫煙条件(55ml/2s、喫煙間隔30s)の下、初期5puff分を測定した。
In addition, it was confirmed that the heating temperature at the time of using Ploom (at the time of stable operation) was about 160 ° C. to 170 ° C. by preliminary measurement using a thermocouple.
As mentioned above, the difficulty of volatilizing aerosols, which is important in measuring the reduction in the taste inhibition, is to measure the amount of aerosol before dilution and the amount of aerosol after dilution with clean air. It was evaluated by the “aerosol residual ratio after dilution”. The amount of aerosol before dilution was measured using a smoking machine (Borgwaldt, RM-26), and the prepared pod was attached to the Ploom, under the prescribed smoking conditions (55 ml / 2s, smoking interval 30s). The initial 5 puff was measured.
 一方、希釈後のエアロゾル量の測定は、前述と同様の方法で発生させたエアロゾルをSUS管(容積:約127cc、長さ:25.0cm、内径:2.54cm)に一度ため込み、清浄空気を流通することで擬似的な希釈条件を作った後、チャコール充填層(100mg)を通過させ、ガス相として存在している成分を取り除いた後のエアロゾル量をケンブリッジフィルタにて初期5puff分測定した。また、作製したサンプルの官能評価は4名にて実施し、「香喫味阻害感」を1~7の7段階評価にて実施した。本実施例の結果において、香喫味阻害感が2.0以下の場合、評価者にとって明らかに違いを識別できる値であり、効果が優れている領域とした。 On the other hand, the amount of aerosol after dilution is measured by storing the aerosol generated by the same method as described above once in a SUS tube (volume: about 127 cc, length: 25.0 cm, inner diameter: 2.54 cm), and clean air. After making a pseudo dilution condition by circulating the gas, the amount of aerosol after removing the components present as the gas phase through the charcoal packed bed (100 mg) was measured by the Cambridge filter for the initial 5 puffs. . In addition, sensory evaluation of the prepared samples was performed by four people, and “flavoring taste sensation” was performed in a seven-step evaluation of 1 to 7. In the result of the present example, when the taste inhibition feeling is 2.0 or less, it is a value that can clearly identify the difference for the evaluator, and is a region where the effect is excellent.
 表1に示す各種エアロゾル生成液体を用いた際の希釈後エアロゾル残存率と香喫味阻害感の関係を図1に示す。図1より、希釈後エアロゾル残存率が高くなるほど、香喫味阻害感は低下傾向にあることが分かる。すなわち、生成するエアロゾルが口腔内希釈によって揮発しにくく、口腔内希釈後に口腔内に残存するエアロゾル量が多い方が、エアロゾル中に含まれる香喫味を感じる際に疎外となる物質がガス相へと相変化しにくく、香喫味阻害感は低くなると考えられる。ジアセチンは、希釈後エアロゾル残存率が高いことから、結果的に最も香喫味阻害感が低くなるエアロゾル生成液体であることが分かった。 FIG. 1 shows the relationship between the aerosol remaining ratio after dilution and the taste inhibition feeling when various aerosol-generating liquids shown in Table 1 are used. From FIG. 1, it can be seen that as the residual ratio of the aerosol after dilution increases, the taste inhibition feeling tends to decrease. That is, the generated aerosol is less likely to volatilize by intraoral dilution, and when the amount of aerosol remaining in the oral cavity is greater after intraoral dilution, the substance that becomes alienated when feeling the savory taste contained in the aerosol enters the gas phase. It is considered that the phase change is difficult and the savory taste inhibition is lowered. Since diacetin has a high aerosol residual ratio after dilution, it has been found that as a result, it is an aerosol-generating liquid that has the lowest sense of flavor inhibition.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
<実施例2-4および比較例8-14>香喫味阻害感低減に効果的な添加量の検討
 前述したように、ジアセチンおよびモノアセチンはそれぞれ単離が困難なため、ジアセチンおよびモノアセチンを含む溶液の構成は非常に類似している。そこで、以下では代表としてジアセチンを含む溶液(市販品)を用い、香喫味阻害感低減に効果的な添加量の検討を実施した。
 香喫味阻害感の低減に効果的な添加量を検討するため、バーレー刻(日本産)100mgにジアセチンおよび比較としてプロピレングリコールを表2に示す量を添加したサンプルを作製した。サンプルは、先の実施例と同様の方法で作製し、2日以上22℃、湿度60%の条件で蔵置した。また、作製したサンプルの官能評価は4名にて実施し、「香喫味阻害感」を1~7の7段階評価にて実施した。本実施例の結果において、香喫味阻害感が2.0以下の場合、評価者にとって明らかに違いを識別できる値であり、効果が優れている領域とした。
 たばこ刻重量に対する溶液添加量と香喫味阻害感の関係を図2に示す。図2より、たばこ刻にエアロゾル生成液体を添加しない場合(たばこ刻重量に対する溶液添加率が0重量%の場合)、香喫味阻害感は6.8と非常に高い値を示すことが分かる。一方、たばこ刻にエアロゾル生成液体としてジアセチンを添加すると、たばこ刻重量に対する溶液添加率が高くなるにつれて、香喫味阻害感が低減することが分かる。
 さらに、たばこ刻重量に対して溶液の添加率が50重量%以上になると香喫味阻害感は大幅に低減することから、香喫味阻害感低減に効果的なジアセチン添加量は、たばこ刻重量に対して50重量%以上である。比較として、エアロゾル生成液体としてプロピレングリコールをたばこ刻重量に対して100重量%添加した場合、香喫味阻害感はたばこ刻にエアロゾル生成液体を添加しない場合と同等程度であることが分かった。このことから香喫味阻害感の低減は、たばこ刻重量に対する溶液添加率の増加が単に効果的であるのではなく、香喫味阻害感の低減に効果的なエアロゾル生成液体であるジアセチンを使用した場合に効果的に発現することが分かる。
<Example 2-4 and Comparative Example 8-14> Examination of Effective Addition Amount to Reduce Flavor Inhibition Feeling As described above, since diacetin and monoacetin are difficult to isolate, the solution containing diacetin and monoacetin The configuration is very similar. Therefore, in the following, a solution containing diacetin (commercially available product) was used as a representative, and the amount of additive effective for reducing the taste inhibition feeling was examined.
In order to examine the effective addition amount for reducing the taste of flavor inhibition, a sample was prepared by adding diacetin and propylene glycol as a comparison to 100 mg of Burley chopping (produced in Japan). Samples were prepared in the same manner as in the previous examples, and stored for 2 days or longer at 22 ° C. and humidity of 60%. In addition, sensory evaluation of the prepared samples was performed by four people, and “flavoring taste sensation” was performed in a seven-step evaluation of 1 to 7. In the result of the present example, when the taste inhibition feeling is 2.0 or less, it is a value that can clearly identify the difference for the evaluator, and is a region where the effect is excellent.
FIG. 2 shows the relationship between the added amount of the solution and the taste inhibition feeling with respect to the tobacco weight. FIG. 2 shows that when the aerosol-generating liquid is not added to the cigarette (when the solution addition rate is 0% by weight with respect to the cigarette weight), the taste inhibition feeling is very high at 6.8. On the other hand, it can be seen that when diacetin is added as an aerosol-generating liquid to tobacco, the sense of flavor inhibition decreases as the solution addition rate with respect to the tobacco weight increases.
Furthermore, when the addition rate of the solution is 50% by weight or more with respect to the cigarette weight, the sense of taste inhibition is greatly reduced. Therefore, the effective amount of diacetin added to reduce the taste inhibition is less than the weight of the cigarette. And 50% by weight or more. As a comparison, it was found that when propylene glycol was added as an aerosol-generating liquid at 100% by weight with respect to the cigarette weight, the taste-inhibiting feeling was comparable to that when no aerosol-generating liquid was added to the cigarette. For this reason, the reduction in flavor inhibition is not simply due to the increase in the rate of solution addition to the cigarette weight but when diacetin, an aerosol-generating liquid that is effective in reducing flavor inhibition, is used. It turns out that it expresses effectively.
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
<参考例1-8:ジアセチンおよびモノアセチン加水分解生成物(酢酸)の生成機構の調査>
 ジアセチンおよびモノアセチンの加水分解生成物である酢酸の生成機構を調査するため、たばこ刻(国内黄色刻)および炭酸カルシウム(刻なしを模擬)100mgに対して、代表として、ジアセチンを100mg添加することで作製した表3で示すサンプルの香喫味阻害感および酢酸量を評価した。なお、水分量による加水分解の影響を調査するため、表3に示すように水分を上乗せで添加した。官能評価は、2名にて実施し、「すっぱさ」を1~7の7段階評価にて実施した。本実施例の結果において、すっぱさが1.5以上の場合、評価者にとってすっぱさを識別できる値であり、1.5以下の範囲は、ジアセチン分解抑制効果が優れている領域とした。酢酸の定量分析は、表3の条件で作製したサンプルを1週間22℃、湿度60%の条件で蔵置し、スクリュー管(No.5,株式会社マルエム製)に入れ、メタノール溶媒で40分間振とう抽出し、GC-MSにて定量した。
<Reference Example 1-8: Investigation of formation mechanism of diacetin and monoacetin hydrolysis product (acetic acid)>
In order to investigate the production mechanism of acetic acid, a hydrolysis product of diacetin and monoacetin, 100 mg of diacetin was added as a representative to 100 mg of tobacco (domestic yellow) and calcium carbonate (simulated without chopping). The sample shown in Table 3 was evaluated for taste inhibition and the amount of acetic acid. In addition, in order to investigate the influence of hydrolysis by the amount of water, water was added as shown in Table 3. The sensory evaluation was performed by two people, and “Supura” was performed in a 7-step evaluation of 1-7. In the results of this example, when the sourness is 1.5 or more, the evaluator can identify the sourness, and the range of 1.5 or less is a region where the diacetin degradation inhibitory effect is excellent. For quantitative analysis of acetic acid, samples prepared under the conditions shown in Table 3 were stored for one week at 22 ° C. and 60% humidity, placed in a screw tube (No. 5, manufactured by Marem Co., Ltd.), and shaken with methanol solvent for 40 minutes. Finally extracted and quantified by GC-MS.
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
 水分添加量と酢酸生成量の関係を表したグラフを図3に示す。図3より、炭酸カルシウムにジアセチンを添加したサンプルでは、水分添加量によらず、サンプルpod内の酢酸量は極めて低い値を示す。一方、たばこ刻にジアセチンを添加した場合、酢酸は水分添加量に比例して大幅に生成していることが分かった。このことから、ジアセチンのみ(ただし炭酸カルシウム含む)を蔵置した場合、水分添加量自体はジアセチンの分解にほとんど影響しないが、ジアセチンをたばこ刻共存下で蔵置すると、水分添加量の増加によってジアセチンの分解が促進され、ジアセチンの分解生成物である酢酸が急激に増加することが分かった。したがって、ジアセチン単独の加水分解は起こりにくいものの、たばこ刻中の加水分解酵素がジアセチンの加水分解を促進し、分解生成物である酢酸を大量に生成すると考えられる。
 最後に、酢酸量とすっぱさの関係を表したグラフを図4に示す。図4より、酢酸量とすっぱさの相関は高く、蔵置後のサンプルを喫煙した際に感じる「すっぱさ」は、ジアセチン分解による酢酸の生成量の増加によって引き起こされることが分かる。
A graph showing the relationship between the amount of water added and the amount of acetic acid produced is shown in FIG. From FIG. 3, in the sample in which diacetin is added to calcium carbonate, the amount of acetic acid in the sample pod shows a very low value regardless of the amount of water added. On the other hand, it was found that when diacetin was added to the cigarette, acetic acid was greatly generated in proportion to the amount of water added. Therefore, when only diacetin is stored (including calcium carbonate), the amount of water added has little effect on the degradation of diacetin, but when diacetin is stored in the presence of tobacco, the increase in the amount of water added causes the degradation of diacetin. It was found that acetic acid, a decomposition product of diacetin, increased rapidly. Therefore, although hydrolysis of diacetin alone is unlikely to occur, it is considered that the hydrolase in the tobacco promotes the hydrolysis of diacetin and produces a large amount of acetic acid, which is a decomposition product.
Finally, a graph showing the relationship between the amount of acetic acid and the sourness is shown in FIG. As shown in FIG. 4, the correlation between the amount of acetic acid and the sourness is high, and it can be seen that the “sourness” felt when smoking the sample after storage is caused by an increase in the amount of acetic acid produced by diacetin degradation.
 <実施例5、6および比較例15-17:加水分解抑制方法の検証>
 先の実施例より、たばこ刻中の加水分解酵素が触媒となってジアセチンの加水分解生成物である酢酸が生成していることが分かった。ここでは、加水分解酵素を失活させる手法として、一般的に行われている加熱処理によって、代表として、ジアセチンの加水分解抑制効果を検証した。
 たばこ刻の加熱処理方法は、スクリュー管(No.5 株式会社マルエム製)にたばこ刻(国内黄色刻)を2g入れて蓋をし、熱風循環オーブン(KLO-60M、光洋サーモシステム株式会社製)にて100℃、120℃、140℃、160℃で60min加熱することとした。なお、各サンプルの作製方法は、先の実施例と同様の方法で作製し、2ヶ月22℃、湿度60%の条件で蔵置し、酢酸量の定量ならびに官能評価を行った。官能評価は、2名にて実施し、「すっぱさ」を1~7の7段階評価にて実施した。本実施例の結果において、すっぱさが1.5以上の場合、評価者にとってすっぱさを明らかに識別できる値であり、逆に1.5以下の範囲は、ジアセチン分解抑制効果が優れている領域とした。酢酸の定量分析は、表4の条件で作製したサンプルを2か月22℃、湿度60%の条件で蔵置し、スクリュー管(No.5 株式会社マルエム製)に入れ、メタノール溶媒で40分間振とう抽出し、GC-MSにて定量した。
<Examples 5 and 6 and Comparative Examples 15-17: Verification of hydrolysis inhibition method>
From the previous examples, it was found that the hydrolase in the tobacco was used as a catalyst to produce acetic acid, which is a hydrolysis product of diacetin. Here, as a method for inactivating the hydrolase, the effect of inhibiting hydrolysis of diacetin was typically verified by a heat treatment generally performed.
Tobacco engraved heat treatment method, 2g of cigarette engraving (domestic yellow engraving) is put into a screw tube (No. 5 manufactured by Marumu Co., Ltd.), covered, and hot air circulation oven (KLO-60M, manufactured by Koyo Thermo Systems Co., Ltd.) It was decided to heat at 100 ° C., 120 ° C., 140 ° C. and 160 ° C. for 60 minutes. Each sample was prepared by the same method as in the previous example, stored for 2 months at 22 ° C. and 60% humidity, and the amount of acetic acid was quantified and sensory evaluation was performed. The sensory evaluation was performed by two people, and “Supura” was performed in a 7-step evaluation of 1-7. In the results of this example, when the sourness is 1.5 or more, the evaluator can clearly identify the sourness, and conversely, the range of 1.5 or less is a region where the diacetin degradation inhibitory effect is excellent. It was. For quantitative analysis of acetic acid, samples prepared under the conditions shown in Table 4 were stored for 2 months at 22 ° C. and 60% humidity, placed in a screw tube (No. 5 manufactured by Maruemu Co., Ltd.), and shaken with methanol solvent for 40 minutes. Finally extracted and quantified by GC-MS.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
 蔵置日数とPod内酢酸量の関係を表したグラフを図5に示す。図5より、刻加熱なしの場合、蔵置日数に対してPod内酢酸量が大幅に増加していくのに対し、たばこ刻のみを事前に加熱処理することで、Pod内で生成する酢酸量が減少していることが分かる。
 ここで、刻加熱なしの場合、蔵置日数が21日(3週間)までは酢酸の生成量が急激に増加しているが、一方、蔵置日数が21日から60日(2ヶ月)では、酢酸量の増加割合は小さく、ジアセチン分解による酢酸の生成速度が減少し、酢酸量はジアセチンの加水分解による最大酢酸生成量に漸近していることが分かる。したがって、刻加熱なし2か月蔵置後の酢酸生成量(8.90mg/pod)は、Pod内に添加したジアセチンが加水分解したことによる最大酢酸生成量(Cmax)と近似できるため、Pod内酢酸量(C)を最大酢酸生成量(Cmax)で割った値を酢酸生成割合(C/Cmax)と定義する。
 さらに、蔵置日数に対する酢酸生成割合の関係を示した図6より、蔵置日数が21日までの酢酸の生成(ジアセチンの分解)は一次反応の挙動を示すことから、酢酸の生成速度定数kを以下一次反応速度式とし、蔵置日数tに対して整理すると以下式になる。
FIG. 5 is a graph showing the relationship between the storage days and the amount of acetic acid in the Pod. From FIG. 5, in the case of no heating, the amount of acetic acid in the Pod increases significantly with respect to the number of days of storage, whereas the amount of acetic acid generated in the Pod is increased by preheating only the tobacco. It turns out that it has decreased.
Here, in the case of no heating, acetic acid production increased sharply until the storage period was 21 days (3 weeks), while acetic acid was increased from 21 days to 60 days (2 months). It can be seen that the rate of increase in the amount is small, the rate of acetic acid production due to diacetin degradation decreases, and the amount of acetic acid is asymptotic to the maximum amount of acetic acid produced by hydrolysis of diacetin. Therefore, the acetic acid production amount (8.90 mg / pod) after storage for 2 months without heating is approximated to the maximum acetic acid production amount (C max ) due to hydrolysis of diacetin added in the pod. amount of acetic maximum acid production amount of (C) the value obtained by dividing by (C max) is defined as acetic acid production ratio (C / C max).
Furthermore, from FIG. 6 showing the relationship of the acetic acid production ratio to the storage days, acetic acid production (diacetin decomposition) up to 21 days of storage shows the behavior of the primary reaction. When the primary reaction rate equation is used and arranged with respect to the storage time t, the following equation is obtained.
Figure JPOXMLDOC01-appb-M000006
Figure JPOXMLDOC01-appb-M000006
 各加熱温度条件に対して、上式をプロットしたグラフを図7に示す。図7より、蔵置日数1日から21日までのプロットの傾きから、たばこ刻の酢酸生成速度定数kを算出した。なお、たばこ刻中にわずかに酢酸が含まれることから図7のグラフは原点を通らない。
 たばこ刻の酢酸生成速度定数kを算出した表4より、たばこ刻の酢酸生成速度定数が1.17×10-8 s-1以下の場合、サンプル蔵置2ヶ月後も酢酸量は極めて低い値をとり、官能評価結果からもすっぱさを全く識別できないことから、酢酸生成速度定数が1.17×10-8 s-1以下のたばこ刻をジアセチンとともに使用することでジアセチンの加水分解を抑制できることが分かった。ここで、すっぱさ1.5に該当する酢酸生成速度定数は1.25×10-8 s-1と概算できるため、分解抑制効果はたばこ材料の酢酸生成速度定数が1.25×10-8 s-1以下である場合に十分に確保できると考えられる。
FIG. 7 shows a graph plotting the above equation for each heating temperature condition. From FIG. 7, the acetic acid acetic acid production rate constant k was calculated from the slope of the plot from storage days 1 to 21. Note that the graph of FIG. 7 does not pass through the origin because acetic acid is slightly contained in the tobacco cut.
According to Table 4 where the acetic acid production rate constant k was calculated, the acetic acid production rate constant was 1.17 × 10 −8 s −1 or less. In addition, since the sourness cannot be discriminated at all from the sensory evaluation results, the hydrolysis of diacetin can be suppressed by using a cigarette with an acetic acid production rate constant of 1.17 × 10 −8 s −1 or less together with diacetin. I understood. Here, since the acetic acid production rate constant corresponding to the sourness 1.5 can be estimated as 1.25 × 10 −8 s −1 , the decomposition inhibiting effect is that the acetic acid production rate constant of the tobacco material is 1.25 × 10 −8. It is considered that a sufficient value can be secured when s −1 or less.
 本発明のたばこ充填物は、非燃焼型加熱喫煙物品に用いられるポッドなどの容器に充填して喫煙に利用することができる。 The tobacco filling of the present invention can be used for smoking by filling a container such as a pod used for a non-combustion type heated smoking article.

Claims (5)

  1.  たばこ材料とエアロゾル生成液体とを含む非燃焼型加熱喫煙物品用のたばこ充填物であって、
     エアロゾル生成液体がジアセチン及びモノアセチンの少なくとも一方を含み、
     たばこ材料の酢酸生成速度定数が1.25×10-8 s-1以下であり、エアロゾル生成液体の添加量が、たばこ材料の重量に対して50重量%以上300重量%以下である、たばこ充填物。
    A tobacco filler for a non-combustion 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 production rate constant of the tobacco material is 1.25 × 10 −8 s −1 or less, and the amount of the aerosol-generating liquid added is 50% by weight to 300% by weight with respect to the weight of the tobacco material. object.
  2.  エアロゾル生成液体が、ジアセチンとモノアセチンの両方を含む、請求項1に記載のたばこ充填物。 The tobacco filling according to claim 1, wherein the aerosol-generating liquid contains both diacetin and monoacetin.
  3.  エアロゾル生成液体における、ジアセチン及びモノアセチンの含有量の合計が50重量%以上である、請求項1または2に記載のたばこ充填物。 The tobacco filling 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.  請求項1~3のいずれか一項に記載のたばこ充填物が充填された、非燃焼型加熱喫煙物品用のポッド。 A pod for a non-combustion type heated smoking article, which is filled with the tobacco filling according to any one of claims 1 to 3.
  5.  請求項1~3のいずれか一項に記載のたばこ充填物を含む、非燃焼型加熱喫煙物品。 A non-combustion type heated smoking article comprising the tobacco filling according to any one of claims 1 to 3.
PCT/JP2016/071526 2016-07-22 2016-07-22 Tobacco filler for non-combustion type heat smoking article WO2018016069A1 (en)

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