WO2024252653A1 - Tobacco material, production method, and smoking article - Google Patents

Abstract

When, as measured by gas chromatography, the peak area of nicotine is N, and among volatile organic compounds V having a retention index (RI) of at least 1,350, the peak area of a compound X having the minimum peak area is Ax, this tobacco material satisfies Ax/N≥1.5.

Description

Tobacco materials, manufacturing methods, and smoking articles

The present invention relates to tobacco materials, manufacturing methods, and smoking articles.

Known methods for manufacturing tobacco sheets include, for example, the papermaking method, the slurry (casting) method, the rolling method, and the extrusion molding method. In particular, the papermaking method includes a process of subjecting tobacco raw materials to water extraction, a process of separating the extract from its residue, a process of concentrating the extract, a process of making the residue into a sheet, and a process of pouring the concentrated extract back onto the sheet. In other words, the papermaking method includes a so-called reconstitution process.

Technologies have been proposed for processing the extract to improve the quality of tobacco products and remove components of concern. For example, Patent Document 1 proposes removing polymers such as proteins and polysaccharides by ultrafiltration, or using only the polymers for reconstitution. Patent Document 2 proposes removing nitric acid and nicotine, which are precursors of TSNA, by electrodialysis. Non-Patent Document 1 discloses a method in which the pH of the extract is increased to free nicotine, and then extraction is performed with a solvent with low polarity such as hexane, transferring the nicotine to the hexane phase.

Patent Document 3 discloses a method that includes a step of extracting tobacco leaf material with a low-polarity solvent to obtain an extract and a residue, a step of subjecting the residue to extraction with a high-polarity solvent, and a step of applying the extract with the low-polarity solvent back to the residue. This method is said to produce tobacco raw material with a good flavor. Patent Document 4 proposes a method in which the fraction obtained by steam distilling tobacco leaves is mixed with other materials as an essential oil.

Patent document 5 discloses that heating the extract at a high pH level makes it easier for nicotine to evaporate, making it easier to remove. Furthermore, patent document 6 discloses the selective extraction of volatile components in tobacco that do not contain alkaloids using a low-polarity solvent.

Volatile organic compounds (VOCs) are included in the volatile components derived from tobacco. Examples of VOCs include the cembranoids Solanone and Norsolanadione (Non-Patent Document 1), the polyphenol Scopletine (Non-Patent Document 2), and the carotenoid decomposition product Ionone (Non-Patent Document 3). Other VOCs include 3-oxo-α-ionol (Non-Patent Document 5), which is also part of the aroma of wine, and 3-hydroxysolavetivone (Non-Patent Document 6), which has strong antibacterial activity.

Incidentally, there is a growing need for tobacco sheets for use in heated smoking articles. Tobacco sheets are composed of tobacco raw materials, an aerosol former, a binder, and other materials. The amount of tobacco components in a tobacco sheet is at most 100% (Patent Document 7). In addition, technology has been proposed that improves heating efficiency by incorporating an electric resistance heating element into the sheet (Patent Document 8), and that the sheet contains an amorphous solid to retain flavor.

U.S. Pat. No. 9,301,544 U.S. Pat. No. 4,302,308 International Publication No. 2015/029977 Chinese Patent No. 104757703 International Publication No. 2022024307 Patent No. 7054708 International Publication No. 2017097840 European Patent No. 3297460

“Fraction of protonated and unprotonated nicotine in tobacco smoke at various pH values” Gerald P. Morie Tobacco Science 1972, 16-52 p167 ISSN 0082-4523) “Gaschromatography Mass Spectrometry” p277-298 H.Kodama), “Basic Chemical Constituents of Tobacco Leaf and Differences among tobacco types” Chapter 8 Leaf chemistry J.C. Leffingwell Chemistry and Technology) “Volatile constituents of perique tobacco” John C. Leffingwell and E.D.Alford Electronic Journal of Environmental, Agricultural and Food Chemistry 4(2) p899-915 2005.) “Management of Postharvest Grape Withering to optimize the aroma of the final wine: A case study on amarone”Bellincontro A, Matarese F, D'Onofrio C, Accordini D, Tosi E, Mencarelli F. food chemistry 2016) “Tobacco phytoalexins and their synthesis induced by elicitors” Mgr. Petra Literakova MASARYK UNIVERSITY FACULTY OF SCIENCE DEPARTMENT OF BIOCHEMISTRY)

When additives are added to a tobacco sheet, the compositional proportion of tobacco components that produce flavor naturally becomes lower. This makes it difficult to enjoy the inherent volatile components of tobacco. The inventors then came up with the idea that if they could create a tobacco molded body containing a high proportion of tobacco components, they could provide a high-quality tobacco product that exhibits a rich tobacco-derived flavor. In light of these circumstances, the objective of the present invention is to provide a high-quality tobacco product that exhibits a rich tobacco-derived flavor.

The inventors have found that a material containing a specific amount of a specific volatile organic compound can solve the above problems. That is, the above problems are solved by the following invention.
Aspect 1
Measured by gas chromatography,
The peak area of nicotine is N,
When the peak area of compound X having the smallest peak area among volatile organic compounds V having a retention index (RI) of 1350 or more is denoted as Ax,
Ax/N≧1.5;
Tobacco materials.
Aspect 2
2. The tobacco material according to claim 1, wherein Ax/N≧2.5.
Aspect 3
A tobacco material according to aspect 1 or 2, wherein the compound X is selected from the group consisting of cembranoids, polyphenols, and carotenoid degradation products.
Aspect 4
Aspect 4. The tobacco material according to any one of Aspects 1 to 3, wherein said compound X is selected from the group consisting of solanone, norsolanadione, 3-oxa-α-ionol, ionone derivatives, 3-hydroxysolavetivone, and scopoletin.
Aspect 5
When the sum of the peak areas of volatile organic compounds having an RI of 1350 or more is At,
A tobacco material according to any one of the preceding aspects, wherein At/N≧30.
Aspect 6
A tobacco material according to any one of Aspects 1 to 5, in the form of a sheet, a strand, or a cut.
Aspect 7
(a) an extraction step of subjecting a tobacco raw material to extraction to obtain an extract A;
(b) a hydrophilization step of preparing a substrate having a hydrophilic surface; and (c) a step of adding the extraction liquid A to the substrate.
A method for producing a tobacco material according to any one of aspects 1 to 6, comprising:
Aspect 8
The (b) hydrophilization step is
(b1) a step of preparing a substrate from the extraction residue obtained in the (a) extraction step; (b2) a step of filtering the extract A obtained in the (a) extraction step;
(b3) electrodialyzing the filtrate obtained in step (b2); and (b4) adding liquid B obtained in step (b3) to the base material prepared in (b1) to prepare a base material having a hydrophilization treatment applied to its surface.
Aspect 9
The method according to aspect 8, wherein step (b2) is a step of removing substances having a molecular weight of more than 100 kDa.
Aspect 10
A tobacco rod comprising the tobacco material according to any one of aspects 1 to 6.
Aspect 11
A smoking article comprising the tobacco rod according to aspect 10.

The present invention makes it possible to provide high-quality tobacco products that have a rich tobacco-derived flavor.

FIG. 1 shows an embodiment of a non-combustion heating type smoking article. FIG. 1 shows an embodiment of a non-combustion heating type smoking system. FIG. 1 is a diagram illustrating one embodiment of a manufacturing method. FIG. 1 is a diagram illustrating one embodiment of step B in the manufacturing method. Gas Chromatography Chart Gas Chromatography Chart

In this disclosure, "X to Y" includes the end values X and Y.
1. Tobacco Material Tobacco material is material derived from the tobacco plant that can be used in smoking articles. The tobacco material of the present embodiment contains specific amounts of specific volatile organic compounds.

(1) Ax/N
The tobacco material satisfies the relationship Ax/N≧1.5, where N is the peak area of nicotine and Ax is the peak area of compound X that has the smallest peak area among volatile organic compounds V having a retention index (RI) of 1350 or more. N and Ax are measured by gas chromatography.

The RI can be determined by a known method using a standard saturated alkane standard, but in this embodiment, it is preferably determined by the following method.
1) Standard saturated alkane standards (for example, C7-C40 manufactured by Merck) are diluted with hexane to use hexane (C6) to tetracontane (C40) as indicators.
2) The linear retention index is calculated based on the following formula and is defined as RI.
RI=100×{[(tr(unknown)−tr(n)]/[tr(N)−tr(n)]+n}
n = number of carbon atoms in the n-alkane eluting immediately before the unknown component N = number of carbon atoms in the n-alkane eluting immediately after the unknown component tr = retention time

Volatile organic compounds with an RI of 1350 or more express the original aroma of tobacco. The volatile organic compounds are a group of components that include partial decomposition products of chlorophyll, leaf resin, higher fatty acids, and higher hydrocarbons. There is no upper limit to the RI, but in one embodiment it is 2000 or less.

Among the volatile organic compounds V, the compound having the smallest peak area measured by gas chromatography is defined as compound X, and the peak area of compound X is defined as Ax. Compound X is preferably selected from the group consisting of cembranoids, polyphenols, and carotenoid decomposition products. Compound X is more preferably selected from the group consisting of solanone, norsolanadione, 3-oxa-α-ionol, ionone derivatives, 3-hydroxysolavetivone, and scopoletin.

Ax/N is the ratio of compound X to nicotine. Therefore, tobacco materials that satisfy the relationship Ax/N≧1.5 exhibit a rich tobacco-derived flavor. From this perspective, Ax/N is preferably 2.5 or more. There is no upper limit for Ax/N, but it is preferably 70 or less.

(2) At/N
From the viewpoint of obtaining a rich tobacco-derived flavor, it is preferable that the tobacco material satisfies the relationship At/N≧30, where At is the sum of the peak areas of volatile organic compounds having an RI of 1350 or more. At/N is more preferably 50 or more. There is no upper limit, but in one embodiment it is 150 or less.

(3) Form The tobacco material may be in various forms. In consideration of handling, the tobacco material is preferably in the form of sheets, strands, or shreds.

(4) Components The tobacco material may contain known materials in addition to materials derived from tobacco plants. For example, the tobacco material may contain an aerosol source, a non-tobacco flavoring agent, a binder, etc.

1) Aerosol Source The aerosol source is a material that vaporizes when heated and cools to generate an aerosol, or that generates an aerosol by atomization. When the tobacco material contains an aerosol source, a sufficient amount of smoke can be achieved. Known aerosol sources can be used, and examples thereof include glycerin, vegetable glycerin, polyhydric alcohols such as propylene glycol (PG), triethyl citrate (TEC), triacetin, etc. The amount of the aerosol source in the tobacco material is preferably 3 to 30% by weight, more preferably 10 to 15% by weight. If the amount of the aerosol source exceeds the upper limit, stains, etc. may occur on the tobacco segment, and if it is less than the lower limit, the smoke sensation may be reduced.

2) Non-Tobacco Flavoring Materials The tobacco material may further include a non-tobacco flavoring agent. A non-tobacco flavoring agent is a flavoring agent that is not derived from tobacco. Examples of non-tobacco flavoring agents include flavoring agents, cooling agents, and combinations thereof. As the flavoring agent and cooling agent, any known flavoring agent may be used.

In particular, the following fragrances can be used alone or in combination:
Acetanisole, acetophenone, acetylpyrazine, 2-acetylthiazole, alfalfa extract, amyl alcohol, amyl butyrate, trans-anethole, star anise oil, apple juice, balsam of Peru oil, beeswax absolute, benzaldehyde, benzoin resinoid, benzyl alcohol, benzyl benzoate, benzyl phenylacetate, benzyl propionate, 2,3-butanedione, 2-butanol, butyl butyrate, butyric acid, caramel, cardamom oil, carob absolute, β-carotene, carrot juice, L-carvone, β- Caryophyllene, cassia bark oil, cedarwood oil, celery seed oil, chamomile oil, cinnamaldehyde, cinnamic acid, cinnamyl alcohol, cinnamyl cinnamate, citronella oil, DL-citronellol, clary sage extract, cocoa, coffee, konjac oil, coriander oil, cuminaldehyde, davana oil, delta-decalactone, gamma-decalactone, decanoic acid, dill herb oil, 3,4-dimethyl-1,2-cyclopentanedione, 4,5-dimethyl-3-hydroxy-2,5-dihydrofuran-2-one, 3,7-dimethyl-6-octenoic acid, 2,3 -dimethylpyrazine, 2,5-dimethylpyrazine, 2,6-dimethylpyrazine, ethyl 2-methylbutyrate, ethyl acetate, ethyl butyrate, ethyl hexanoate, ethyl isovalerate, ethyl lactate, ethyl laurate, ethyl levulinate, ethyl maltol, ethyl octanoate, ethyl oleate, ethyl palmitate, ethyl phenylacetate, ethyl propionate, ethyl stearate, ethyl valerate, ethyl vanillin, ethyl vanillin glucoside, 2-ethyl-3,(5 or 6)-dimethylpyrazine, 5-ethyl-3-hydroxy-4-methyl-2(5H)-furanone, 2 -Ethyl-3-methylpyrazine, eucalyptol, fenugreek absolute, gene absolute, gentian root infusion, geraniol, geranyl acetate, grape juice, guaiacol, guava extract, gamma-heptalactone, gamma-hexalactone, hexanoic acid, cis-3-hexen-1-ol, hexyl acetate, hexyl alcohol, phenylhexyl acetate, honey, 4-hydroxy-3-pentenoic acid lactone, 4-hydroxy-4-(3-hydroxy-1-butenyl)-3,5,5-trimethyl-2-cyclohexen-1-one, 4- (para-hydroxyphenyl)-2-butanone, sodium 4-hydroxyundecanoate, immortelle absolute, beta-ionone, isoamyl acetate, isoamyl butyrate, isoamyl phenylacetate, isobutyl acetate, isobutyl phenylacetate, jasmine absolute, cola nut tincture, labdanum oil, lemon terpeneless oil, licorice extract, linalool, linalyl acetate, lovage root oil, maltol, maple syrup, menthol, menthone, L-menthyl acetate, paramethoxybenzaldehyde, methyl-2-pyrrolyl ketone, an Methyl tranilate, methyl phenylacetate, methyl salicylate, 4'-methylacetophenone, methylcyclopentenolone, 3-methylvaleric acid, mimosa absolute, honeysuckle, myristic acid, nerol, nerolidol, γ-nonalactone, nutmeg oil, δ-octalactone, octanal, octanoic acid, orange flower oil, orange oil, orris root oil, palmitic acid, ω-pentadecalactone, peppermint oil, petitgrain Paraguay oil, phenethyl alcohol, phenethyl phenylacetate, phenylacetic acid, piperonal, plum extract, propenyl glycol Aethol, Propyl Acetate, 3-Propylidenephthalide, Prune Juice, Pyruvic Acid, Raisin Extract, Rose Oil, Rum, Sage Oil, Sandalwood Oil, Spearmint Oil, Styrax Absolute, Marigold Oil, Tea Distillate, α-Terpineol, Terpinyl Acetate, 5,6,7,8-Tetrahydroquinoxaline, 1,5,5,9-Tetramethyl-13-oxacyclo(8.3.0.0(4.9))tridecane, 2,3,5,6-Tetramethylpyrazine, Thyme Oil, Tomato Extract, 2-Tridecanone, Triethyl Citrate , 4-(2,6,6-trimethyl-1-cyclohexenyl) 2-buten-4-one, 2,6,6-trimethyl-2-cyclohexene-1,4-dione, 4-(2,6,6-trimethyl-1,3-cyclohexadienyl) 2-buten-4-one, 2,3,5-trimethylpyrazine, gamma-undecalactone, gamma-valerolactone, vanilla extract, vanillin, veratraldehyde, violet leaf absolute, N-ethyl-p-menthane-3-carboxamide (WS-3), ethyl-2-(p-menthane-3-carboxamide) acetate (WS-5).

3) Binder The tobacco material may contain a binder to improve moldability. Examples of binders include polysaccharides, proteins, synthetic polymers, etc. These may be used alone or in combination of two or more. Examples of polysaccharides include cellulose derivatives and naturally occurring polysaccharides.

2. Manufacturing method of tobacco material Tobacco material can be manufactured by adjusting the amount of nicotine and volatile organic compound V having an RI of 1500 or more in a material derived from a tobacco plant. For example, the tobacco material is preferably manufactured by a manufacturing method including the following steps.
(a) an extraction step of subjecting a tobacco raw material to extraction to obtain an extract A;
(b) a hydrophilization step of preparing a substrate having a hydrophilic surface; and (c) a step of adding the extraction liquid A to the substrate.

(1) Extraction step a
Fig. 3 shows an overview of the method. In this step, the tobacco raw material to be extracted is subjected to extraction to obtain an extract A. Examples of the tobacco raw material include tobacco leaves and tobacco shreds. The extraction can be carried out as known in the art, and examples include the following methods: 1) a method in which the tobacco raw material is subjected to extraction using a medium to obtain a tobacco extract, 2) a method in which a medium is added to the tobacco raw material and heated, the generated steam is collected, and a tobacco extract is obtained, and 3) a method in which a medium that has been vaporized by heating is passed through the tobacco raw material and the vapor after the passage is collected to obtain a tobacco extract. Examples of the medium include water, a hydrophilic organic solvent such as alcohol, or a combination thereof, and it is preferable that the medium is water or contains water.

In method 1), it is preferable to use water as the medium from the viewpoint of workability, etc. In method 2) or 3), water may be used as the medium from the viewpoint of work efficiency, or a mixed solvent of water and an alcohol such as glycerin, propylene glycol, triacetin, 1,3-butanediol, or ethanol may be used. An acid or alkali may be used for extraction as necessary. The liquid obtained by extraction, which contains the tobacco extract and the medium, is called tobacco extract.

The tobacco raw material may be in the form of shreds or powder (hereinafter also referred to as "raw material pieces"). In such a case, the particle size of the raw material pieces is preferably 0.5 to 1.18 mm. Such raw material pieces are obtained, for example, by sieving in accordance with JIS Z 8815 using a stainless steel sieve conforming to JIS Z 8801. For example, 1) using a stainless steel sieve with 1.18 mm openings, the raw material pieces are sieved for 20 minutes by a dry mechanical shaking method to obtain raw material pieces that pass through the stainless steel sieve with 1.18 mm openings. 2) Next, using a stainless steel sieve with 0.50 mm openings, the raw material pieces are sieved for 20 minutes by a dry mechanical shaking method to remove the raw material pieces that pass through the stainless steel sieve with 0.50 mm openings. In this way, raw material pieces can be prepared that pass through the stainless steel sieve (mesh size = 1.18 mm) that defines the upper limit, but do not pass through the stainless steel sieve (mesh size = 0.50 mm) that defines the lower limit.

In one embodiment, the tobacco raw material is treated with alkali. This treatment generates flavor components, which are then collected to prepare a tobacco extract and a tobacco extract residue. In this case, the flavor components are extracted as a gas from the alkali-treated tobacco raw material, and the gas can be introduced into water to obtain a tobacco extract in which the flavor components have been transferred to a liquid.

The alkaline substance is preferably an alkaline liquid such as an aqueous solution of potassium carbonate. In this case, the alkaline substance is supplied until the pH of the tobacco raw material falls within a specific range. The pH is preferably 8.0 or higher, and more preferably 8.9 to 9.7. The pH of the tobacco raw material refers to the pH of the water when the tobacco raw material is mixed with 10 times the amount of water.

The moisture content in the tobacco raw material used for extraction is not limited, but from the viewpoint of efficiently extracting flavor components, it is preferable that the moisture content is approximately 5 to 30% by weight. The moisture content in the tobacco raw material is measured by a known method, for example, a 1 g sample is taken, heated at 105°C, and the weight loss amount when heated until the weight change rate is 1 mg/min or less is taken as the moisture content. For example, a halogen heating moisture meter (Ohaus MB45, etc.) can be used for this measurement.

The tobacco extract preferably contains a large amount of nicotine. From this perspective, the amount of nicotine in the extraction residue is preferably 1% by weight or less of the amount of nicotine in the tobacco raw material, and more preferably 0.5% by weight or less.

Extract A is rich in volatile organic compound V. Because volatile organic compound V is lipophilic, if the medium used for extraction is lipophilic, volatile organic compound V will dissolve in the medium. On the other hand, even when water is used as the medium, extract A is rich in volatile organic compound V. This is because water dissolves not only electrolytes, but also some polymeric compounds such as proteins and pectin, and these polymeric compounds function as emulsifiers. In addition, most volatile organic compound V is present on the surface of tobacco leaves, and is physically transported into the extract by the water.

(2) Hydrophilization step b
In this step, a substrate with a hydrophilic surface is prepared. The hydrophilic method is not limited and is appropriately selected depending on the substrate. For example, the hydrophilic treatment can be performed by treating the surface of a substrate such as a sheet with a surfactant or the like. The surfactant used in this case is preferably one approved for addition to food. The substrate may be a tobacco substrate such as a tobacco sheet, tobacco shreds, or tobacco granules, or a non-tobacco substrate such as a non-tobacco sheet, non-tobacco shreds, or non-tobacco granules. The tobacco substrate is preferably formed from the extraction residue obtained in the extraction step a. The non-tobacco substrate is preferably formed from a polysaccharide or the like.

In one embodiment, it is preferable to use a substrate formed from the extraction residue. In this embodiment, the hydrophilization step b preferably includes the following steps:
(b1) a step of preparing a substrate from the extraction residue obtained in the extraction step (a); (b2) a step of filtering the extract A obtained in the extraction step (a); (b3) a step of electrodialyzing the filtrate obtained in the step (b2); and (b4) a step of adding the liquid B obtained in the step (b3) to the substrate prepared in the step (b1) to prepare a substrate having a hydrophilized surface.

(2-1) Step b1
4 shows an overview of step b in this embodiment. In step b1, a substrate is prepared from the extraction residue obtained in the extraction step a. The method for this is not limited, and examples include a method in which the residue is made into paper to form a tobacco sheet, the tobacco sheet is cut into tobacco shreds, and the residue is granulated into tobacco granules.

(2-2) Step b2
In this step, the extract A obtained in the extraction step a is filtered. The filtration is carried out by a known method, but is preferably a filtration that removes substances with a molecular weight of more than 100 kDa. This filtration can remove proteins and the like from the extract. Specifically, this filtration is preferably ultrafiltration using an ultrafiltration membrane. The nominal molecular weight cutoff of the ultrafiltration membrane is not limited as long as it is more than 2 kDa, but is preferably 10 to 50 kDa. In one embodiment, the filtration conditions can be a flow rate of 1 to 20 kg/h and an inlet pressure of about 1 to 10 bar. If necessary, the extract A may be concentrated before filtration. The filtrate obtained by filtration may also be concentrated. The concentration is carried out by a known method, but it is preferable to use a centrifugal thin film evaporator from the viewpoint of work efficiency and the like.

(2-3) Step b3
In this step, the filtrate obtained in step b2 is electrodialyzed. If necessary, the filtrate may be concentrated before electrodialysis. The method of concentration is as described above. Electrodialysis is performed using a known device. The conditions are not limited, but in one embodiment, it is performed at 30 to 100 V. The dialysis time is appropriately adjusted, but in one embodiment, it is about 5 to 20 hours. This step makes it possible to remove electrolytes such as nicotine and nitric acid from the filtrate. The liquid obtained in this step is called liquid B. Liquid B is hydrophilic because hydrophobic components such as proteins have been removed. Furthermore, liquid B has the property of having a low viscosity and being easily permeable to a substrate because polymer components have been removed.

(2-4) Step b4
In this step, the liquid B obtained in step b3 is added to the substrate. The method of addition is not limited, and for example, methods such as coating, impregnation, and spraying can be adopted. If necessary, the liquid B may be concentrated before the addition. Concentration. The concentration method is as described above. By treating with the hydrophilic liquid B, a substrate having a hydrophilized surface is prepared.

(3) Step c
In this step, the extract A is added to the substrate whose surface has been hydrophilized in step b. The method of addition is as described above. The extract A is rich in volatile organic compounds V, but also contains polar components, so it is hydrophilic. Generally, the substrate surface is hydrophobic. Therefore, it is difficult to retain a sufficient amount of volatile organic compounds V in the substrate by simply adding the extract A to a substrate that has not been subjected to hydrophilization treatment. However, in the manufacturing method according to the present embodiment, the substrate is hydrophilized, so that a sufficient amount of volatile organic compounds V can be retained in the substrate. The substrate obtained in this manner is rich in volatile organic compounds V, so that Ax/N≧1.5 is satisfied.

3. Smoking Articles Tobacco materials are useful as a flavor source for smoking articles. That is, tobacco materials are useful as a filler for tobacco rods (tobacco segments). In addition, tobacco materials are suitable for non-combustion heat-type smoking articles because they easily release the volatile organic compounds when heated to 200 to 400°C. Smoking articles will be described below using non-combustion heat-type smoking articles as an example.

Figure 1 shows one embodiment of a non-combustion heating smoking article. As shown in the figure, the non-combustion heating smoking article 20 comprises a tobacco segment 20A, a cylindrical cooling section 20B having perforations on the circumference, and a filter section 20C. The non-combustion heating smoking article 20 may have other components. The axial length of the non-combustion heating smoking article 20 is not limited, but is preferably 40 to 90 mm, more preferably 50 to 75 mm, and even more preferably 50 to 60 mm or less. The circumferential length of the non-combustion heating smoking article 20 is preferably 16 to 25 mm, more preferably 20 to 24 mm, and even more preferably 21 to 23 mm. For example, an embodiment can be mentioned in which the tobacco segment 20A has a length of 20 mm, the cooling section 20B has a length of 20 mm, and the filter section 20C has a length of 7 mm. The lengths of these individual components can be changed as appropriate depending on manufacturing suitability, required quality, etc. FIG. 1 shows an embodiment in which the first segment 25 is arranged, but it is also possible to arrange only the second segment 26 downstream of the cooling section 20B without the first segment 25.

1) Tobacco segment 20A
The tobacco rod and the tobacco segment are synonymous and are used interchangeably. The tobacco filler 21 in the tobacco segment 20A includes the tobacco material or a tobacco filler containing the tobacco material. The method of filling the tobacco filler 21 into the wrapper 22 is not particularly limited, and for example, the tobacco filler 21 may be wrapped in the wrapper 22, or the tobacco filler 21 may be filled into a cylindrical wrapper 22. When the tobacco filler has a longitudinal direction such as a rectangular shape, it may be filled so that the longitudinal direction is in an unspecified direction in the wrapper 22, or may be filled so that it is aligned with the axial direction of the tobacco segment 20A or aligned in a direction perpendicular to the axial direction. When the tobacco segment 20A is heated, the tobacco components, the aerosol source, and water contained in the tobacco filler 21 are vaporized and are available for inhalation.

2) Cooling section 20B
The cooling section 20B is preferably constructed of a tubular member. The tubular member may be, for example, a cardboard tube 23 formed by processing cardboard into a cylindrical shape. The cooling section 20B may also be formed by a sheet of thin material that is wrinkled and then pleated, gathered, or folded to form a channel. For example, a sheet material selected from the group consisting of polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate, polylactic acid, cellulose acetate, and aluminum foil may be used as such a material. The total surface area of the cooling section 20B is appropriately adjusted in consideration of the cooling efficiency, and may be, for example, 300 to 1000 mm ² /mm 2 . The cooling section 20B is preferably provided with perforations 24. The presence of the perforations 24 allows outside air to be introduced into the cooling section 20B during inhalation. As a result, the aerosol vaporized components generated by heating the tobacco segment 20A come into contact with the outside air, and the temperature of the components is reduced, so that the components are liquefied, and an aerosol is formed. The diameter (distance across) of the perforations 24 is not particularly limited, and may be, for example, 0.5 to 1.5 mm. The number of perforations 24 is not particularly limited, and may be one or two or more. For example, a plurality of perforations 24 may be provided on the circumference of the cooling portion 20B.

The cooling section 20B may be rod-shaped with an axial length of, for example, 7 to 28 mm. For example, the axial length of the cooling section 20B may be 18 mm. The cooling section 20B may have a substantially circular axial cross-sectional shape with a diameter of 5 to 10 mm. For example, the diameter of the cooling section may be approximately 7 mm.

3) Filter section 20C
The configuration of the filter part 20C is not particularly limited, and may be composed of one or more filling layers. The outside of the filling layer may be wrapped with one or more wrapping papers. The airflow resistance of the filter part 20C can be appropriately changed depending on the amount and material of the filter filling filled in the filter part 20C. For example, when the filter filling is cellulose acetate fiber, the airflow resistance can be increased by increasing the amount of cellulose acetate fiber filled in the filter part 20C. When the filter filling is cellulose acetate fiber, the packing density of the cellulose acetate fiber can be 0.13 to 0.18 g/cm ^3. The airflow resistance is a value measured by an airflow resistance measuring device (product name: SODIMAX, manufactured by SODIM).

The circumferential length of the filter part 20C is not particularly limited, but is preferably 16 to 25 mm, more preferably 20 to 24 mm, and even more preferably 21 to 23 mm. The axial length of the filter part 20C (horizontal direction in FIG. 1) can be selected from 4 to 10 mm, and is selected so that the airflow resistance is 15 to 60 mmH ₂ O/seg. The axial length of the filter part 20C is preferably 5 to 9 mm, and more preferably 6 to 8 mm. The cross-sectional shape of the filter part 20C is not particularly limited, but can be, for example, a circle, an ellipse, a polygon, etc. In addition, a destructible capsule containing a fragrance, fragrance beads, or a fragrance may be directly added to the filter part 20C.

The filter section 20C may have a center hole section as the first segment 25. The center hole section is composed of a first filling layer 25a having one or more hollow sections and an inner plug wrapper (inner wrapping paper) 25b that covers the filling layer. The center hole section has the function of increasing the strength of the mouthpiece section. The center hole section may not have an inner plug wrapper 25b and may maintain its shape by thermoforming. The first filling layer 25a may be, for example, a rod with an inner diameter of φ5.0 to φ1.0 mm, in which cellulose acetate fibers are densely packed and a plasticizer containing triacetin is added at 6 to 20% by weight relative to the weight of the cellulose acetate and hardened. Since the first filling layer 25a has a high fiber packing density, air and aerosol flow only through the hollow section during inhalation and hardly flow inside the first filling layer 25a. Since the first filling layer 25a inside the center hole section is a fiber packing layer, the feel from the outside during use is less likely to cause discomfort to the user. The filter section 20C may include a second segment 26. The second segment 26 is composed of a second packed layer 26a and an inner plug wrapper (inner wrapping paper) 26b that covers the packed layer.

The first filling layer 25a and the second filling layer 26a are connected by an outer plug wrapper (outer wrapping paper) 27. The outer plug wrapper 27 can be, for example, a cylindrical piece of paper. The tobacco segment 20A, the cooling section 20B, and the first filling layer 25a and the second filling layer 26a that have already been connected are connected by a mouthpiece lining paper 28. These connections can be made, for example, by applying a vinyl acetate glue or other adhesive to the inner surface of the mouthpiece lining paper 28 and wrapping the three components. These components may be connected in multiple layers using multiple lining papers.

The combination of a non-combustion heated smoking article and a heating device for generating an aerosol is also referred to as a non-combustion heated smoking system. An example of such a system is shown in Figure 2. In the figure, the non-combustion heated smoking system comprises a non-combustion heated smoking article 20 and a heating device 10 that heats a tobacco segment 20A from the outside.

The heating device 10 comprises a body 11, a heater 12, a metal tube 13, a battery unit 14, and a control unit 15. The body 11 has a cylindrical recess 16, and the heater 12 and the metal tube 13 are arranged at a position corresponding to the tobacco segment 20A to be inserted therein. The heater 12 can be an electric resistance heater, and is heated by being supplied with power from the battery unit 14 in response to an instruction from the control unit 15 that controls the temperature. The heat generated by the heater 12 is transferred to the tobacco segment 20A through the metal tube 13, which has high thermal conductivity. In the figure, the heating device 10 is shown as heating the tobacco segment 20A from the outside, but it may also be heating from the inside. The heating temperature by the heating device 10 is not particularly limited, but is preferably 400°C or less, more preferably 150 to 400°C, and even more preferably 200 to 350°C. The heating temperature refers to the temperature of the heater of the heating device 10. It is also possible to place a susceptor inside the tobacco segment 20A and heat the tobacco segment 20A using the induction method.

The following describes an embodiment.
Aspect 1
Measured by gas chromatography,
The peak area of nicotine is N,
When the peak area of compound X having the smallest peak area among volatile organic compounds V having a retention index (RI) of 1350 or more is denoted as Ax,
Ax/N≧1.5;
Tobacco materials.
Aspect 2
2. The tobacco material according to claim 1, wherein Ax/N≧2.5.
Aspect 3
A tobacco material according to aspect 1 or 2, wherein the compound X is selected from the group consisting of cembranoids, polyphenols, and carotenoid degradation products.
Aspect 4
Aspect 4. The tobacco material according to any one of Aspects 1 to 3, wherein said compound X is selected from the group consisting of solanone, norsolanadione, 3-oxa-α-ionol, ionone derivatives, 3-hydroxysolavetivone, and scopoletin.
Aspect 5
When the sum of the peak areas of volatile organic compounds having an RI of 1350 or more is At,
A tobacco material according to any one of the preceding aspects, wherein At/N≧30.
Aspect 6
A tobacco material according to any one of Aspects 1 to 5, in the form of a sheet, a strand, or a cut.
Aspect 7
(a) an extraction step of subjecting a tobacco raw material to extraction to obtain an extract A;
(b) a hydrophilization step of preparing a substrate having a hydrophilic surface; and (c) a step of adding the extraction liquid A to the substrate.
A method for producing a tobacco material according to any one of aspects 1 to 6, comprising:
Aspect 8
The (b) hydrophilization step is
(b1) a step of preparing a substrate from the extraction residue obtained in the (a) extraction step; (b2) a step of filtering the extract A obtained in the (a) extraction step;
(b3) electrodialyzing the filtrate obtained in step (b2); and (b4) adding liquid B obtained in step (b3) to the base material prepared in (b1) to prepare a base material having a hydrophilization treatment applied to its surface.
Aspect 9
The method according to aspect 8, wherein step (b2) is a step of removing substances having a molecular weight of more than 100 kDa.
Aspect 10
A tobacco rod comprising the tobacco material according to any one of aspects 1 to 6.
Aspect 11
A smoking article comprising the tobacco rod according to aspect 10.

(1) Extraction step a
Yellow seed tea was prepared as a tobacco raw material.
30 kg of yellow seedlings and 250 kg of ion-exchanged water were added to the extraction device. Extraction was then carried out at 85° C. for 30 minutes. The residue was separated using a screw press (HX-200, 1500 L, manufactured by Fukuku Kyogo Co., Ltd.) to obtain 200 kg of extract.

100 kg of the extract was concentrated directly using a centrifugal thin-film evaporator (Okawara Manufacturing Co., Ltd. CEP10S) to obtain 8 kg of concentrated liquid with a Brix of 50°, which was designated as extract A.

(2) Hydrophilization step b
The remaining 100 kg of the extract was filtered using a filtration device (Alfa-Laval Labstak M20) to obtain 90 kg of filtrate containing components with a molecular weight of 100 kDa or less. The filtrate was then treated for 12 hours at 50 V using an electrodialysis device (SR10-100 manufactured by Sunactis Co., Ltd.) to remove electrolytes. 85 kg of the treated liquid thus obtained was concentrated using a centrifugal thin-film evaporator (CEP10S manufactured by Okawara Seisakusho Co., Ltd.) to obtain 3 kg of concentrated liquid with a Brix of 50°, which was designated as Liquid B.

(3) Step c
A sheet (substrate) was produced from the extraction residue obtained by the above extraction using a papermaking machine (Daisho Tekkosho Co. LTD). The sheet was immersed in liquid B for 5 minutes and then dried at 80°C for 60 minutes to prepare a primary reconstituted tobacco sheet (a sheet with a hydrophilized surface). Next, 1g and 2g of extract A were applied to 2g of the primary reconstituted tobacco, respectively, and dried at 80°C for 60 minutes to obtain two types of reconstituted tobacco sheets (tobacco materials) (Level 1, Level 2). Liquid B increased the hydrophilicity of the sheet surface because the polymer had been removed. Therefore, the volatile organic compound V component in extract A was sufficiently retained in the tobacco sheet. In addition, a sheet to which extract A was not added was used as a comparative reconstituted tobacco sheet (Level 3).

(4) Component Analysis The sheets of levels 1 to 3 were each cut to obtain chopped pieces. 2 g of each chopped piece was placed in a 50 ml sample tube, and 30 ml of ethyl acetate was added as an extraction solvent and shaken for 1 hour. Next, 5 ml of the extraction solution (ethyl acetate phase) was transferred to a 20 ml sample tube containing 5 ml of 0.1% H ₂ SO ₄ aqueous solution, and mixed in a vortex mixer (Vortex-Genie2 manufactured by Scientific Industries). After that, the mixture was left to stand for 30 minutes, and the upper organic solvent layer was analyzed by GC/MS to determine the peak and peak area of volatile organic compound V. The analysis conditions are shown below.
Gas chromatography (GC/FID)
Apparatus: Agilent Technologies 7890AGC
Column: DB-5MS (Agilent Technologies), inner diameter 0.25 mm x length 30 m, film thickness 0.25 μm
Injection volume: 1 μL
Injection mode: Split (10:1)
Inlet temperature: 270℃
Septum purge flow rate: 5 mL/min Carrier gas: Helium (He)
Column flow rate: 1 mL/min Oven: 40°C (3 min) - 4°C/min - 280°C (20 min) (total 83 min)
Detector: FID
The sample was treated with an aqueous _{H2SO4 solution} , so that the sample submitted to GC analysis was a sample from which nicotine had been removed.

On the other hand, the samples were analyzed by GC/MS under the same conditions as above, except that the samples were not treated with _{H2SO4 aqueous} solution, and the amount of nicotine in each sample was analyzed. The analysis results are shown in Table 1 and Figures 5 and 6.

As shown in the table, levels 1 and 2 yielded tobacco materials that satisfied Ax/N≧1.5. This is believed to be because a hydrophilized sheet was used, which increased the affinity with liquid B, resulting in a large amount of volatile organic compound V in liquid B remaining in the sheet. On the other hand, level 3, which used a non-hydrophilized sheet, had a low affinity with liquid B, resulting in insufficient volatile organic compound V in liquid B remaining in the sheet. This is believed to be why level 3 had a low Ax/N.

REFERENCE SIGNS LIST 10 heating device 11 body 12 heater 13 metal tube 14 battery unit 15 control unit 16 recess 17 ventilation hole
20 Non-combustion heating smoking article 20A Tobacco segment 20B Cooling section 20C Filter section
21 tobacco filler 22 cigarette paper 23 paper tube 24 perforation 25 first segment 25a first filling layer 25b inner plug wrapper 26 second segment 26a second filling layer 26b inner plug wrapper 27 outer plug wrapper 28 lining paper

Claims (11)

Measured by gas chromatography,
The peak area of nicotine is N,
When the peak area of compound X having the smallest peak area among volatile organic compounds V having a retention index (RI) of 1350 or more is denoted as Ax,
Ax/N≧1.5;
Tobacco materials. The tobacco material according to claim 1, wherein Ax/N≧2.5. The tobacco material according to claim 1 or 2, wherein the compound X is selected from the group consisting of cembranoids, polyphenols, and carotenoid decomposition products. The tobacco material according to any one of claims 1 to 3, wherein the compound X is selected from the group consisting of solanone, norsolanadione, 3-oxa-α-ionol, ionone derivatives, 3-hydroxysolavetivone, and scopoletin. When the sum of the peak areas of volatile organic compounds having an RI of 1350 or more is At,
The tobacco material according to any one of claims 1 to 4, wherein At/N≧30. The tobacco material according to any one of claims 1 to 5, which is in the form of a sheet, strand, or shreds. (a) an extraction step of subjecting a tobacco raw material to extraction to obtain an extract A;
(b) a hydrophilization step of preparing a substrate having a hydrophilic surface; and (c) a step of adding the extraction liquid A to the substrate.
The method for producing a tobacco material according to any one of claims 1 to 6, comprising: The (b) hydrophilization step is
(b1) a step of preparing a substrate from the extraction residue obtained in the (a) extraction step; (b2) a step of filtering the extract A obtained in the (a) extraction step;
(b3) a step of electrodialyzing the filtrate obtained in the step (b2); and (b4) adding the liquid B obtained in the step (b3) to the substrate prepared in the step (b1) to make the surface hydrophilic. A method for producing a tobacco material according to claim 7, comprising the step of preparing a treated substrate. The method of claim 8, wherein step (b2) is a step of removing substances having a molecular weight of more than 100 kDa. A tobacco rod comprising the tobacco material according to any one of claims 1 to 6. A smoking article comprising the tobacco rod according to claim 10.