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WO2023119517A1 - Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac - Google Patents

Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac Download PDF

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Publication number
WO2023119517A1
WO2023119517A1 PCT/JP2021/047673 JP2021047673W WO2023119517A1 WO 2023119517 A1 WO2023119517 A1 WO 2023119517A1 JP 2021047673 W JP2021047673 W JP 2021047673W WO 2023119517 A1 WO2023119517 A1 WO 2023119517A1
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WIPO (PCT)
Prior art keywords
tobacco
residue
flavor
extract
bleached
Prior art date
Legal status (The legal status 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 status listed.)
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PCT/JP2021/047673
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English (en)
Japanese (ja)
Inventor
研児 伊藤
伸也 吉田
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Japan Tobacco Inc
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Japan Tobacco Inc
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Filing date
Publication date
Application filed by Japan Tobacco Inc filed Critical Japan Tobacco Inc
Priority to EP21968954.4A priority Critical patent/EP4454486A4/fr
Priority to JP2023568904A priority patent/JP7681726B2/ja
Priority to PCT/JP2021/047673 priority patent/WO2023119517A1/fr
Publication of WO2023119517A1 publication Critical patent/WO2023119517A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B13/00—Tobacco for pipes, for cigars, e.g. cigar inserts, or for cigarettes; Chewing tobacco; Snuff
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10—Chemical features of tobacco products or tobacco substitutes
    • A24B15/12—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/241—Extraction of specific substances
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/42—Treatment of tobacco products or tobacco substitutes by chemical substances by organic and inorganic substances

Definitions

  • the present invention relates to bleached tobacco residue and its manufacturing method, reconstituted tobacco material and its manufacturing method, and tobacco products.
  • the regenerated tobacco material When regenerated tobacco material is used as a flavor source for a tobacco product, the regenerated tobacco material may be visually recognized by the user, for example, when a cartridge containing the regenerated tobacco material is replaced, or the pigment component in the regenerated tobacco material may envelop the regenerated tobacco material. It may bleed into the packaging material (eg, paper or non-woven fabric). For this reason, the color of the regenerated tobacco material is preferably closer to white in terms of appearance.
  • TSNAs tobacco-specific nitrosamines
  • NNK 4-(methylnitrosoamino)-1-(3-pyridyl)-1-butanone
  • NNN N'-nitrosonornicotine
  • NAT N'-nitrosoanatabine
  • N'- Refers to the four components of nitrosoanabasine (NAB).
  • TSNAs contained in mainstream tobacco smoke are produced by three pathways (Non-Patent Documents 1-3). Specifically, the three routes are a route in which TSNA contained in the tobacco filler is directly transferred to smoke by evaporation, and a route in which alkaloids in the tobacco filler are nitrosated using heat during combustion to form TSNA.
  • One is the synthesis route, and the other is the route in which NNK bound to lignin-like polymer components is dissociated by heat during combustion and transferred into smoke.
  • NNK bound to the lignin-like polymer component in the tobacco filler is called "bound NNK”
  • NNK free without binding to the lignin-like polymer component in the tobacco filler is called "called "free NNK”.
  • the present invention is a technology related to whitened tobacco residue with reduced 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (hereinafter also referred to as NNK), which is a type of tobacco-specific nitrosamine. intended to provide
  • a method of making bleached tobacco residue comprising treating tobacco residue with an aqueous solution comprising peracetic acid, acetic acid, and hydrogen peroxide to bleach the tobacco residue.
  • a bleached tobacco residue obtainable by the aforementioned method.
  • a method for producing reconstituted tobacco material comprising mixing the bleached tobacco residue and the tobacco flavor liquid.
  • a reconstituted tobacco material obtainable by the above method.
  • a tobacco product comprising reconstituted tobacco material as described above.
  • NNK 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone
  • FIG. 1 is a flow chart illustrating an exemplary method for producing bleached tobacco residue and reconstituted tobacco material.
  • FIG. 2 is a perspective view showing an example of a non-combustion heating type flavor inhaler.
  • FIG. 3 is a cross-sectional view of a non-combustion heated flavor inhalation article.
  • FIG. 4 is a diagram showing the internal structure of the aerosol generator.
  • FIG. 5 is a graph showing the relationship between the concentration of bleaching solution and the color of tobacco residue.
  • FIG. 6 is a graph showing the relationship between the concentration of bleach and the color of tobacco residue.
  • FIG. 7 is a graph showing the relationship between the reaction time and the color of tobacco residue.
  • FIG. 8 is a graph showing the relationship between the concentration of bleaching solution and the amount of bound NNK.
  • FIG. 9 is a graph showing the relationship between the concentration of bleaching agent in the bleaching solution and the amount of bound NNK.
  • FIG. 10 is a graph showing the relationship between the reaction time and the amount of bound NNK.
  • FIG. 11 is a graph showing the relationship between the amount of bleaching solution and the amount of bound NNK with respect to tobacco residue.
  • FIG. 12 is a graph showing the relationship between the concentration of bleaching solution and the mass ratio of tobacco residue.
  • FIG. 13 is a graph showing the relationship between the concentration of bleaching solution and the mass ratio of tobacco residue.
  • FIG. 14 is a graph showing the results of color analysis of tobacco flavor liquid.
  • FIG. 15 is a graph showing the relationship between the pH of the acidic tobacco extract and the nicotine content in the tobacco flavor liquid.
  • FIG. 16 is a graph showing the relationship between the ethanol concentration in the acidic tobacco extract and the benzaldehyde content in the tobacco flavor liquid.
  • a method of making bleached tobacco residue includes treating tobacco residue with an aqueous solution comprising peracetic acid, acetic acid, and hydrogen peroxide to bleach the tobacco residue.
  • the bleached tobacco residue manufacturing method comprises extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent prior to the bleaching treatment to prepare tobacco residue. further includes
  • the method for producing bleached tobacco residue comprises: (S1) extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain tobacco residue; (S2) treating the tobacco residue with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to bleach the tobacco residue.
  • FIG. 1 A method according to a preferred embodiment is shown in FIG. In addition to the "method for producing bleached tobacco residue", FIG. 1 also shows the "method for producing reconstituted tobacco material”.
  • extraction step (S1) water-soluble components contained in the tobacco material are extracted from the tobacco material with an aqueous solvent to obtain tobacco residue.
  • extraction step (S1) a tobacco extract is obtained at the same time as tobacco residue is obtained (see FIG. 1).
  • cut tobacco ready to be blended into tobacco products such as combustion type or heating type flavor inhalers can be used.
  • "Shredded tobacco ready to be incorporated into tobacco products” means a drying process at a farm, followed by a long-term aging process of one to several years at a raw material plant, and then blending and chopping at a manufacturing plant. It refers to shredded tobacco that is ready to be blended into tobacco products after undergoing various processing such as
  • Tobacco cuts are cut tobacco leaves.
  • Tobacco shredded includes deboned leaves, shredded ribs, and reconstituted tobacco (i.e., tobacco processed into a reusable form from leaf scraps, shredded scraps, shredded ribs, fine powder, etc. generated in the factory work process. material), or a mixture thereof.
  • Tobacco shreds may be pulverized in order to increase extraction efficiency, and the resulting pulverized material may be used for extraction.
  • shredded tobacco can be used, for example, yellow variety, burley variety, orient variety can be used.
  • a single variety of shredded tobacco may be used, or a mixture of different varieties may be used.
  • aqueous solvent water or an ethanol aqueous solution with a concentration of 10% by mass or less can be used.
  • the aqueous solvent is generally water, preferably water at room temperature (eg, about 20°C) to 70°C.
  • Aqueous solvents can be used, for example, in an amount of 500-5000% by weight relative to the tobacco material.
  • Extraction is carried out, for example, by immersing the tobacco material in warm water of 40-60°C for 30-180 minutes, or by shaking the tobacco material in warm water of 40-60°C for 30-180 minutes (eg, 200 rpm). be able to.
  • the extraction may be performed by repeating the extraction operation multiple times. Specifically, the water-soluble components contained in the tobacco material are extracted from the tobacco material with an aqueous solvent, and then the obtained tobacco residue is put into a new aqueous solvent and subjected to a second extraction operation. The extraction may be carried out by repeating the extraction procedure with a new aqueous solvent.
  • a mixture of tobacco residue and tobacco extract is obtained by extraction.
  • the tobacco extract contains water-soluble components contained in the tobacco material.
  • water-soluble components contained in tobacco materials include components that contribute to tobacco flavor (eg, organic acids, foliar resins, terpenoids, and polyphenols).
  • the tobacco residue and the tobacco extract are separated, and the tobacco extract can be used as a raw material for obtaining the tobacco flavor liquid.
  • the tobacco residue can be mixed with the finally obtained tobacco flavor liquid, and the resulting mixture can be appropriately processed to produce a tobacco filler (hereinafter also referred to as regenerated tobacco material).
  • a tobacco filler hereinafter also referred to as regenerated tobacco material.
  • the tobacco residue may be mixed with the finally obtained tobacco flavoring liquid, and the resulting mixture may be used to produce tobacco moldings such as sheet tobacco.
  • the tobacco residue may be mixed with the tobacco flavoring liquid finally obtained and the resulting mixture dried and ground for use in making tobacco powder.
  • bleaching step (S2) In the bleaching step (S2), the tobacco residue obtained in the extraction step (S1) is treated with an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide to bleach the tobacco residue (see FIG. 1). This gives a bleached tobacco residue.
  • bleached tobacco residue refers to tobacco residue that has been bleached. In other words, the “bleached tobacco residue” may be bleached, and does not need to be completely changed to white by the bleaching treatment.
  • the bleaching process can be performed by immersing the tobacco residue in an aqueous solution containing peracetic acid, acetic acid and hydrogen peroxide.
  • the reduced amount of peracetic acid consumed by the reaction of tobacco residue and peracetic acid is produced by the reaction of acetic acid and hydrogen peroxide.
  • the peracetic acid can be supplemented, thereby allowing the peracetic acid to exist in the reaction solution at a concentration equal to or higher than the predetermined concentration. In this case, the bleaching efficiency of tobacco residue can be improved.
  • the concentration of peracetic acid in the aqueous solution is, for example, 0.015-10% by mass, preferably 0.15-1.5% by mass.
  • the concentration of acetic acid in the aqueous solution is, for example, 0.04-4% by mass, preferably 0.4-4% by mass.
  • the concentration of hydrogen peroxide in the aqueous solution is, for example, 0.0055-0.55% by mass, preferably 0.055-0.55% by mass.
  • Aqueous solutions containing peracetic acid, acetic acid, and hydrogen peroxide that are commercially available as peracetic acid preparations can be used.
  • a peracetic acid formulation approved as a food additive can be used.
  • Persun MP2-J Korean MP2-J (Kanto Kagaku Co., Ltd.) can be used.
  • Persan MP2-J is composed of 15% by weight peracetic acid, 40% by weight acetic acid, 5.5% by weight hydrogen peroxide, less than 1% by weight stabilizer, and the balance water.
  • the bleaching process can be carried out by immersing the tobacco residue in a bleaching solution under conditions that allow the tobacco residue to be bleached.
  • the bleaching step can be carried out at a temperature of 22-100° C. for 15-240 minutes.
  • the bleaching step is preferably carried out with heating, for example at a temperature of 40 to 100°C.
  • the ratio (solid-liquid ratio) of the mass of the tobacco residue to the mass of the aqueous solution (bleaching solution) can be, for example, 1:30 to 1:100.
  • the tobacco residue can be efficiently bleached and the amount of bound NNK in the tobacco residue can be reduced (see Examples 1 and 2 below).
  • the above-described method produces tobacco residue that is whitened and has a superior appearance (i.e., the color desired by users when incorporated into tobacco products) and that contains reduced amounts of bound NNKs. can do.
  • the term "whitened” refers to the change in the visual color of tobacco residue to a lighter color due to the bleaching process. That is, the term “whitened” encompasses not only cases in which the tobacco residue has visually completely turned white, but also cases in which the tobacco residue has not visually completely turned white.
  • a whitened regenerated tobacco material can be produced by combining the bleached tobacco residue obtained in the bleaching step (S2) with the colorless tobacco extract.
  • the method for producing reconstituted tobacco material comprises: adjusting the pH of the tobacco extract obtained in the extraction step (S1) to 4.1 or less to obtain an acidic tobacco extract; treating the acidic tobacco extract with a reverse-phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid (i.e., a colorless tobacco extract); It includes mixing the bleached tobacco residue obtained in the bleaching step (S2) with the tobacco flavor liquid (see FIG. 1).
  • a method for producing a reconstituted tobacco material comprises: (S1) extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco extract and tobacco residue; (S2) treating the tobacco residue with an aqueous solution comprising peracetic acid, acetic acid and hydrogen peroxide to obtain a bleached tobacco residue; (S3) adjusting the pH of the tobacco extract to 4.1 or less to obtain an acidic tobacco extract; (S4) treating the acidic tobacco extract with a reverse-phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid (that is, a colorless tobacco extract); , (S5) including mixing the bleached tobacco residue and the tobacco flavor liquid (see FIG. 1).
  • the liquid obtained by extracting the water-soluble component from the tobacco material is called “tobacco extract”
  • the solid obtained during this extraction is called “tobacco residue”
  • the pH of the tobacco extract is
  • the liquid obtained by adjusting to 4.1 or less is called “acidic tobacco extract”
  • the liquid obtained by treating the acidic tobacco extract with a reversed-phase adsorbent is called “tobacco flavor liquid”.
  • pH adjustment step (S3) In the pH adjustment step (S3), the pH of the tobacco extract obtained in the extraction step (S1) is adjusted to 4.1 or less to obtain an acidic tobacco extract (see FIG. 1).
  • the pH of the tobacco extract is preferably adjusted within the range of 1-4.1, more preferably within the range of 2-3.
  • the pH can be adjusted by adding to the tobacco extract a pH adjuster for lowering the pH of the tobacco extract in an amount necessary to reach a desired pH.
  • a pH adjuster for example, weak acids such as phosphoric acid, citric acid and acetic acid may be used, and strong acids such as nitric acid, hydrochloric acid and sulfuric acid may be used.
  • the pH is a value measured with a pH meter using a glass electrode according to the pH measurement method described in JIS Z 8802:2011, that is, using two electrodes, a glass electrode and a reference electrode, It refers to the value obtained by measuring the potential difference generated between these two electrodes.
  • a commercially available pH meter based on the glass electrode method such as LAQUA F-72 (HORIBA), can be used as the pH meter.
  • the pH measurement can be performed, for example, on the tobacco extract at 20°C.
  • the measured value of pH is obtained to the second decimal place or less, the value obtained by rounding off the second decimal place or less can be regarded as the pH value.
  • the acidic tobacco extract may be prepared to contain ethanol at a concentration of 10% by mass or less.
  • the acidic tobacco extract may be prepared to contain ethanol at a concentration of 1-10% by mass. That is, the acidic tobacco extract is prepared by adjusting the tobacco extract obtained in the extraction step (S1) or the pH to 4.1 or less so that the final concentration is 10% by mass or less (preferably 1 to 10% by mass). It may further comprise adding ethanol to the tobacco extract.
  • the tobacco flavor liquid obtained as the final product exhibits a colorless or nearly colorless color while containing a greater amount of tobacco flavor components. (see Example 7 below).
  • Treatment step with reversed-phase adsorbent (S4)
  • the acidic tobacco extract is treated with a reverse-phase adsorbent to remove colored components from the acidic tobacco extract.
  • a tobacco flavor liquid is thus obtained (see FIG. 1).
  • reverse-phase solid-phase extraction is a process in which a polar solution or suspension (mobile phase) is passed over a non-polar solid (stationary phase), and hydrophobic components contained in the mobile phase are adsorbed onto the stationary phase. Refers to the method of separation.
  • reversed-phase adsorbents examples include adsorbents in which hydrophobic groups such as octadecylsilyl groups (ODS) are bonded to silica gel carrier particles, and adsorbents composed of hydrophobic polymer particles such as styrenedivinylbenzene copolymers. be done.
  • hydrophobic groups such as octadecylsilyl groups (ODS) are bonded to silica gel carrier particles
  • ODS octadecylsilyl groups
  • Reversed phase adsorbents are commercially available, for example, InterSep C18 (GL Sciences Co., Ltd.) solid phase extraction cartridges, Oasis HLB (Nippon Waters Co., Ltd.) solid phase extraction cartridges, and Diaion HP series (Mitsubishi Chemical Co., Ltd.) ), Amberlite XAD series (Organo Corporation) and other synthetic adsorbents.
  • the reversed-phase adsorbent is not limited to those exemplified, and known adsorbents having the same separation mode as those exemplified can be used.
  • the treatment step (S4) may be performed by passing the acidic tobacco extract through a solid phase comprising a reversed-phase adsorbent, or by adding particles of the reversed-phase adsorbent to the acidic tobacco extract, followed by reverse This may be done by removing particles of the phase adsorbent from the acidic tobacco extract, such as by filtration.
  • the treatment step (S4) can be performed by passing the acidic tobacco extract through a solid phase comprising a reversed-phase adsorbent.
  • the treatment step (S4) can be performed by passing the acidic tobacco extract through a column filled with a reversed-phase adsorbent.
  • a "reversed-phase sorbent" may generally consist of a collection of particles of a reversed-phase sorbent.
  • the colored components and tobacco-specific nitrosamines (TSNAs) can be removed from the tobacco extract without damaging the tobacco flavor components contained in the tobacco extract (Examples 4 to 4 described later). 6).
  • the colored components and tobacco-specific nitrosamines (TSNAs) contained in the tobacco extract can be adsorbed on the column, and the tobacco extract is The tobacco flavor component contained in can be eluted in the eluate.
  • TSNAs tobacco-specific nitrosamines
  • NNK butanone
  • NNN N'-nitrosonornicotine
  • NAT N'-nitrosoanatabine
  • NAB N'-nitrosoanabasine
  • the bleached tobacco residue may be molded into a specific form such as a sheet or granules to prepare tobacco moldings such as sheet tobacco or tobacco granules, and the obtained tobacco moldings may be mixed with a tobacco flavoring liquid. .
  • the tobacco flavor liquid may be concentrated to prepare a concentrate of the tobacco flavor liquid, and the obtained concentrate may be mixed with tobacco residue or tobacco moldings.
  • bleached tobacco residue is mixed with colorless tobacco extract (that is, tobacco flavoring liquid) to produce reconstituted tobacco material.
  • colorless tobacco extract that is, tobacco flavoring liquid
  • the present invention is not limited to this embodiment, and the bleached tobacco residue may be mixed with the tobacco extract obtained in the extraction step (S1) to produce reconstituted tobacco material.
  • the tobacco residue can be efficiently bleached and the amount of bound NNK in the tobacco residue can be reduced (see Examples 1 and 2 below).
  • Reconstituted tobacco materials can be produced that contain, but have reduced amounts of, tobacco-specific nitrosamines (TSNAs).
  • the bleached tobacco residue is whitened, has an excellent appearance, and contains a reduced amount of bound NNK. Therefore, when bleached tobacco residue is incorporated into a tobacco product, it can provide the user with a desirable appearance while providing the user with a reduced amount of NNK during use of the tobacco product.
  • bound NNK in tobacco residue is dissociated by heat and converted to free NNK, which migrates into smoke. A reduced amount of NNK can be provided to the user, especially when heated.
  • the bleached tobacco residue has a lower mass than the tobacco residue before bleaching (see Example 3 below). Therefore, when bleached tobacco residue is incorporated into a tobacco product, a greater amount of tobacco residue can be incorporated into the tobacco product.
  • the bleached tobacco residue can be incorporated into tobacco products such as flavor inhalers according to known techniques. Examples of the use of bleached tobacco residue are described below.
  • the bleached tobacco residue is mixed with the tobacco flavoring liquid obtained in the above treatment step (S4), the resulting mixture is dried, and the resulting dried product is used as a tobacco flavoring source for tobacco products. can do.
  • the bleached tobacco residue is mixed with the tobacco flavoring liquid obtained in the treatment step (S4), and the obtained mixture is used to prepare tobacco moldings such as sheet tobacco and tobacco granules, and tobacco moldings are carried out.
  • the body can be used as a tobacco flavor source for tobacco products.
  • the bleached tobacco residue is mixed with the tobacco flavoring liquid obtained in the above treatment step (S4), the resulting mixture is dried and pulverized to prepare tobacco powder, and the tobacco powder is used as a tobacco material ( deboned leaves and leaf tobacco) and the resulting mixture can be used as a tobacco flavor source for tobacco products.
  • the bleached tobacco residue is mixed with the tobacco flavoring liquid obtained in the above treatment step (S4), the resulting mixture is dried and pulverized to prepare tobacco powder, and the tobacco powder is suspended in water.
  • a tobacco slurry may be prepared by clouding, the tobacco slurry may be added to a tobacco material (eg, deboned leaves or leaf tobacco), and the resulting mixture may be used as a tobacco flavor source for tobacco products.
  • the reconstituted tobacco material is whitened, has an excellent appearance, and contains sufficient amounts of tobacco flavor components, but contains reduced amounts of tobacco-specific nitrosamines (TSNAs). Accordingly, when such reconstituted tobacco material is incorporated into a tobacco product, it provides the user with a desirable appearance while providing a sufficient amount of tobacco flavoring components and a reduced amount of tobacco specific nitrosamines (TSNAs) to the user during use of the tobacco product.
  • TSNAs tobacco-specific nitrosamines
  • the bleached tobacco residue contained in the reconstituted tobacco material has a lower mass than the tobacco residue before bleaching (see Example 3 below). Therefore, when reconstituted tobacco material is incorporated into a tobacco product, a greater amount of reconstituted tobacco material can be incorporated into the tobacco product.
  • the regenerated tobacco material is obtained by drying a mixture of the bleached tobacco residue obtained in the bleaching step (S2) and the tobacco flavor liquid obtained in the treatment step (S4). It may be a product. This product can be used as a tobacco flavor source in tobacco products.
  • the regenerated tobacco material is a mixture of the bleached tobacco residue obtained in the above bleaching step (S2) and the tobacco flavor liquid obtained in the above treatment step (S4) in a sheet shape, a granule shape, or the like. It may also be a tobacco molded article obtained by molding into a specific shape.
  • the tobacco molded body can be used as a tobacco flavor source for tobacco products.
  • the reconstituted tobacco material is obtained by drying a mixture of the bleached tobacco residue obtained in the bleaching step (S2) and the tobacco flavoring liquid obtained in the treatment step (S4) and turning it into a powder.
  • Tobacco powder obtained by grinding may also be used.
  • Tobacco powder can be added to tobacco materials (eg, deboned leaves and leaf tobacco) to enhance the flavor of the tobacco materials.
  • the flavor-enhanced tobacco material can be used as a tobacco flavor source in tobacco products.
  • the reconstituted tobacco material is obtained by drying a mixture of the bleached tobacco residue obtained in the bleaching step (S2) and the tobacco flavoring liquid obtained in the treatment step (S4) and turning it into a powder. It may be a tobacco slurry obtained by pulverizing and suspending the resulting powder in water. Tobacco slurry can be added to tobacco materials (for example, deboned leaves and leaf tobacco) to enhance the flavor of the tobacco materials.
  • the flavor-enhanced tobacco material can be used as a tobacco flavor source in tobacco products.
  • the reconstituted tobacco material may contain additives such as binders, pH adjusters, preservatives, and antioxidants as necessary.
  • Tobacco products The "reconstituted tobacco material” described above can be incorporated into any tobacco product.
  • a tobacco product comprising a "reconstituted tobacco material” as described above.
  • Tobacco products include combustion flavor inhalers, heated flavor inhalers, unheated flavor inhalers, and smokeless tobacco.
  • a "combustion type flavor inhaler” is a flavor inhaler that provides tobacco flavor to the user by burning a tobacco filler (such as cut tobacco or molded tobacco). Examples of burning flavor inhalers include cigarettes, pipes, pipes, cigars, or cigarillos.
  • a "heated flavor inhaler” is a flavor inhaler that provides tobacco flavor to a user by heating tobacco filler without burning it.
  • a heating type flavor inhaler a carbon heat source flavor inhaler that heats the tobacco filler with the heat of combustion of the carbon heat source (see e.g. WO2006/073065);
  • An electrically heated flavor inhaler comprising a tobacco stick containing tobacco filler and a heating device for electrically heating the tobacco stick (see e.g. WO2010/110226); and sucks the flavor derived from the tobacco filler together with the aerosol (see, for example, WO2015/046385) etc.
  • non-heating flavor inhaler is a flavor inhaler that provides the user with tobacco flavor without burning or heating the tobacco filler.
  • a non-heating flavor inhaler a non-heating tobacco flavor inhaler (for example, see WO2012/023515).
  • “Smokeless tobacco” is a product that allows the user to enjoy the tobacco flavor by putting the product directly into the nasal cavity or oral cavity.
  • the former are called nasal tobacco products and the latter are called oral tobacco products.
  • An example of the former is snuff and an example of the latter is chewing tobacco.
  • the aforementioned "reconstituted tobacco material” can be incorporated into a heated flavor inhaler.
  • a heated flavor inhaler comprising the aforementioned "reconstituted tobacco material”.
  • the heated flavor inhaler may further include a heater for heating tobacco filler including reconstituted tobacco material.
  • the aforementioned "reconstituted tobacco material” can be incorporated into oral tobacco products.
  • an oral tobacco product comprising the aforementioned "reconstituted tobacco material”.
  • the oral tobacco product may further comprise a liquid-permeable wrapper (eg, a nonwoven sachet) encasing the tobacco filler comprising reconstituted tobacco material.
  • the oral tobacco product may have the shape of a tea bag in which the tobacco flavor source is wrapped in a nonwoven sachet.
  • FIG. 2 is a perspective view showing an example of a non-combustion heating type flavor inhaler.
  • FIG. 3 is a cross-sectional view of a non-combustion heated flavor inhalation article.
  • FIG. 4 is a diagram showing the internal structure of the aerosol generator.
  • the flavor inhaler 100 a flavor inhalation article 110 comprising a "reconstituted tobacco material" as described above and an aerosol source; an aerosol generator 120 for heating the flavor inhalation article 110 to atomize the aerosol source and release flavor components from the reconstituted tobacco material.
  • the flavor inhaling article 110 is a replaceable cartridge and has a columnar shape extending along one direction. Flavor inhalation article 110 is configured to generate an aerosol containing a flavor component when heated while being inserted into aerosol generator 120 .
  • the flavor inhaling article 110 forms one end thereof and includes a base portion 110A including a filler 111 and a first wrapping paper 112 around which the filler 111 is wrapped, and a base portion 110A. and a mouthpiece portion 110B forming the opposite end.
  • the base material portion 110A and the mouthpiece portion 110B are connected by a second wrapping paper 113 .
  • the mouthpiece portion 110B has a paper tube portion 114 and a filter 118 adjacent thereto.
  • the filter 118 has a filter plug 115, a hollow plug 116 and a forming paper 117 connecting them by covering them.
  • the paper tube portion 114 is a paper tube formed by rolling paper into a cylindrical shape, and the inside is hollow.
  • the hollow plug 116 is arranged adjacent to the paper tube portion 114, and the filter plug 115 is arranged at the end of the mouthpiece portion 110B.
  • the filter plug 115 includes a filter medium 102 such as acetate tow, and a first plug winding paper 101 around which the filter medium 102 is wound.
  • the hollow plug 116 includes a filling layer 104 and a second plug winding paper 103 around which the filling layer 104 is wound.
  • the packing layer 104 is composed of densely packed fibers and has one or more channels (hollow portions). Each of the one or more channels extends along the length of the flavor inhaling article 110 (hereinafter referred to as the longitudinal direction). Therefore, during suction, air or aerosol flows only through the channels and hardly flows through the gaps between the fibers. In the flavor inhalation article 110, when it is desired to reduce the reduction due to filtration of the aerosol component at the filter plug 115, shortening the length of the filter plug 115 and replacing it with the hollow plug 116 is effective for increasing the delivery amount of the aerosol. is.
  • the filter 118 may consist of two plugs, as shown in FIG. 3, three or more plugs, or only one plug.
  • filter 118 may omit hollow plug 116 and consist only of filter plug 115 . That is, the filter plug 115 and the paper tube portion 114 can be arranged adjacent to each other to form the mouthpiece portion 110B.
  • the mouthpiece portion 110B is composed of two segments, the paper tube portion 114 and the filter 118, but the mouthpiece portion 110B may be composed of one segment, or composed of three or more segments. may
  • the mouthpiece 110B may be provided with an opening to take in air from the outside. In this case, it is desirable to provide an opening in the paper tube portion 114 .
  • the longitudinal dimension of the flavor inhaling article 110 is preferably 40 to 90 mm, more preferably 50 to 75 mm, even more preferably 50 to 60 mm.
  • the circumference of the flavor inhaling article 110 is preferably 15 to 25 mm, more preferably 17 to 24 mm, even more preferably 20 to 23 mm.
  • the length of the base material portion 110A may be 20 mm
  • the length of the paper tube portion 114 may be 20 mm
  • the length of the hollow plug 116 may be 8 mm
  • the length of the filter plug 115 may be 7 mm.
  • the length of each of these segments can be changed as appropriate according to manufacturability, required quality, and the like.
  • the filling 111 includes the aforementioned "reconstituted tobacco material” and an aerosol source. From the viewpoint of the effects of the invention, it is preferable that the filler 111 is composed only of the above-mentioned "reconstituted tobacco material” and an aerosol source. However, as long as the effect of the invention is exhibited, the filler 111 may contain a tobacco filler other than the above-mentioned "recycled tobacco material”.
  • Aerosol source is heated to a predetermined temperature to generate vapor.
  • Aerosol sources can include, for example, glycerin, propylene glycol, triacetin, 1,3-butanediol, and mixtures thereof.
  • the aerosol source can be included in an amount of, for example, 15-19% by weight relative to the total tobacco filler contained in filler 111 .
  • the content of the filler 111 in the flavor inhaling article 110 is, for example, 200 to 400 mg, preferably 250 to 320 mg, when the base portion 110A has a circumference of 22 mm and a length of 20 mm.
  • the same wrapping paper and tipping paper used in cigarettes can be used, respectively.
  • the first plug winding paper 101, the second plug winding paper 103 and the forming paper 117 the same plug winding paper and forming paper used for cigarettes can be used.
  • the aerosol generator 120 has an insertion hole 130 into which the flavor inhalation article 110 can be inserted. That is, the aerosol generator 120 has an inner cylindrical member 132 that forms the insertion hole 130 .
  • the inner tubular member 132 may be made of a thermally conductive material such as aluminum or stainless steel (SUS).
  • the aerosol generator 120 may have a lid portion 140 that closes the insertion hole 130 .
  • the lid portion 140 is slidable and can change between a state in which the insertion hole 130 is closed and a state in which the insertion hole 130 is exposed (see FIG. 2).
  • the aerosol generator 120 may have an air flow path 160 communicating with the insertion hole 130 .
  • One end of the air channel 160 is connected to the insertion hole 130 , and the other end of the air channel 160 communicates with the outside (outside air) of the aerosol generator 120 at a location different from the insertion hole 130 .
  • the aerosol generator 120 may have a lid portion 170 that covers the end of the air flow path 160 on the side communicating with the outside air.
  • the lid portion 170 can cover the end of the air flow path 160 on the side communicating with the outside air, or can leave this end exposed.
  • the lid portion 170 is in a state of covering the end portion of the air flow path 160, but does not airtightly block the air flow path 160. That is, the lid portion 170 covers the air flow path 160, but is separated from the end portion of the air flow path 160, so that outside air can flow into the air flow path 160 through the gap between them. ing.
  • the user With the flavor suction article 110 inserted into the aerosol generator 120, the user holds one end of the flavor suction device 110, specifically, the mouthpiece 110B shown in FIG. 3, and performs a suction operation. Outside air flows into the air flow path 160 due to the suction action of the user. The air flowing into the air channel 160 passes through the flavor inhaling article 110 inside the insertion hole 130 and is guided into the user's oral cavity.
  • the aerosol generating device 120 may have a temperature sensor inside the air flow path 160 or on the outer surface of the wall that constitutes the air flow path 160 .
  • the temperature sensor may be, for example, a thermistor, a thermocouple, or the like.
  • the aerosol generator 120 has a battery 10, a control unit 20, and a heater 30.
  • Battery 10 stores power for use in aerosol generator 120 .
  • the battery 10 may be a rechargeable secondary battery.
  • Battery 10 may be, for example, a lithium-ion battery.
  • the heater 30 may be provided around the inner cylindrical member 132 .
  • the space accommodating the heater 30 and the space accommodating the battery 10 may be separated from each other by the partition wall 180 .
  • the air heated by heater 30 can be prevented from flowing into the space housing battery 10 . Therefore, the temperature rise of battery 10 can be suppressed.
  • the heater 30 preferably has a tubular shape capable of heating the outer circumference of the columnar flavor inhaling article 110 .
  • the heater 30 may be, for example, a film heater.
  • the film heater may have a pair of film-like substrates and a resistance heating element sandwiched between the pair of substrates.
  • the film-like substrate is preferably made of a material with excellent heat resistance and electrical insulation, typically made of polyimide.
  • the resistance heating element is preferably made of one or more metal materials such as copper, nickel alloy, chromium alloy, stainless steel, platinum rhodium, etc. For example, it can be formed of a stainless steel base material.
  • the resistance heating element may be plated with copper on the connection part and its lead part in order to connect with the power supply through the flexible printed circuit (FPC).
  • a heat-shrinkable tube is preferably provided outside the heater 30 .
  • a heat-shrinkable tube is a tube that shrinks radially by heat, and is made of, for example, a thermoplastic elastomer.
  • the heater 30 is pressed against the inner cylindrical member 132 by the contraction action of the heat-shrinkable tube. As a result, the adhesion between the heater 30 and the inner tubular member 132 is enhanced, so that the thermal conductivity from the heater 30 to the flavor inhaling article 110 via the inner tubular member 132 is enhanced.
  • the aerosol generator 120 may have a cylindrical heat insulator radially outside the heater 30, preferably outside the heat-shrinkable tube.
  • the heat insulating material can serve to prevent the outer surface of the housing of the aerosol generating device 120 from reaching excessively high temperatures by blocking the heat of the heater 30 .
  • Insulators can be made from aerogels, such as silica aerogels, carbon aerogels, alumina aerogels, for example.
  • the airgel as a thermal insulator may typically be a silicic aerogel with high thermal insulation performance and relatively low manufacturing cost.
  • the heat insulating material may be a fiber heat insulating material such as glass wool or rock wool, or may be a foamed heat insulating material such as urethane foam or phenol foam.
  • the insulation may be vacuum insulation.
  • An outer cylindrical member 134 is provided outside the heat insulating material. Thermal insulation may be provided between the inner tubular member 132 facing the flavor inhaling article 110 and the outer tubular member 134 .
  • the outer tubular member 134 may be made of a thermally conductive material such as aluminum or stainless steel (SUS). It is preferable that the heat insulating material is provided within a closed space.
  • the control unit 20 may include a circuit board, central processing unit (CPU), memory, and the like. Also, the aerosol generator 120 may have a notification unit for notifying the user of various information under the control of the control unit 20 .
  • the notification portion may be a light emitting element, such as a light emitting diode (LED), or a vibrating element, or a combination thereof.
  • the control unit 20 When the control unit 20 detects the user's activation request, the control unit 20 starts supplying power from the battery 10 to the heater 30 .
  • the user's activation request is made, for example, by the user's operation of a push button or slide switch, or by the user's suction action.
  • a user activation request may be made by pressing a push button 150 . More specifically, the user's activation request may be made by pressing the push button 150 while the lid 140 is open.
  • the user activation request may be made by sensing the user's sucking action. The user's sucking action can be detected, for example, by a temperature sensor as described above.
  • [A1] A method for producing bleached tobacco residue, comprising treating tobacco residue with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide to bleach the tobacco residue.
  • [A2] The method according to [A1], further comprising, prior to the treatment, extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to prepare the tobacco residue.
  • the aqueous solvent is water.
  • the aqueous solvent is an ethanol aqueous solution having a concentration of 10% by mass or less.
  • [A5] The method according to any one of [A1] to [A4], wherein the treatment is performed by immersing the tobacco residue in the aqueous solution.
  • [A6] The method according to any one of [A1] to [A5], wherein the concentration of peracetic acid in the aqueous solution is 0.015 to 10% by mass, preferably 0.15 to 1.5% by mass.
  • [A7] The method according to any one of [A1] to [A6], wherein the concentration of acetic acid in the aqueous solution is 0.04 to 4% by mass, preferably 0.4 to 4% by mass.
  • [A8] Any one of [A1] to [A7], wherein the concentration of hydrogen peroxide in the aqueous solution is 0.0055 to 0.55% by mass, preferably 0.055 to 0.55% by mass. the method of.
  • [A9] The method according to any one of [A1] to [A8], wherein the treatment is performed at a temperature of 22 to 100°C.
  • [A10] The method according to any one of [A1] to [A9], wherein the treatment is performed at a temperature of 40 to 100°C.
  • [A11] The method according to any one of [A1] to [A10], wherein the treatment is performed for 15 to 240 minutes.
  • [A12] The method according to any one of [A1] to [A11], wherein the ratio of the mass of the tobacco residue to the mass of the aqueous solution is 1:30 to 1:100.
  • [B1] A bleached tobacco residue obtained by the method according to any one of [A1] to [A12].
  • [C1] extracting water-soluble components contained in the tobacco material from the tobacco material with an aqueous solvent to obtain a tobacco extract and tobacco residue; treating the tobacco residue with an aqueous solution comprising peracetic acid, acetic acid and hydrogen peroxide to obtain a bleached tobacco residue; obtaining an acidic tobacco extract by adjusting the pH of the tobacco extract to 4.1 or less; treating the acidic tobacco extract with a reverse-phase adsorbent to remove colored components from the acidic tobacco extract, thereby obtaining a tobacco flavor liquid; A method for producing reconstituted tobacco material, comprising mixing the bleached tobacco residue and the tobacco flavoring liquid.
  • [C2] The method according to [C1], wherein the aqueous solvent is water.
  • the aqueous solvent is an ethanol aqueous solution having a concentration of 10% by mass or less.
  • [C4] The method according to any one of [C1] to [C3], wherein the treatment with the aqueous solution is performed by immersing the tobacco residue in the aqueous solution.
  • [C5] The method according to any one of [C1] to [C4], wherein the concentration of peracetic acid in the aqueous solution is 0.015 to 10% by mass, preferably 0.15 to 1.5% by mass.
  • [C6] The method according to any one of [C1] to [C5], wherein the concentration of acetic acid in the aqueous solution is 0.04 to 4% by mass, preferably 0.4 to 4% by mass.
  • [C7] Any one of [C1] to [C6], wherein the concentration of hydrogen peroxide in the aqueous solution is 0.0055 to 0.55% by mass, preferably 0.055 to 0.55% by mass. the method of.
  • [C8] The method according to any one of [C1] to [C7], wherein the treatment with the aqueous solution is performed at a temperature of 22 to 100°C.
  • [C9] The method according to any one of [C1] to [C8], wherein the treatment with the aqueous solution is performed at a temperature of 40 to 100°C.
  • [C10] The method according to any one of [C1] to [C9], wherein the treatment with the aqueous solution is performed for 15 to 240 minutes.
  • [C11] The method according to any one of [C1] to [C10], wherein the ratio of the mass of the tobacco residue to the mass of the aqueous solution is 1:30 to 1:100.
  • [C12] The method according to any one of [C1] to [C11], wherein the treatment with the reversed-phase adsorbent is performed by passing the acidic tobacco extract through a solid phase comprising the reversed-phase adsorbent.
  • [C13] The method according to any one of [C1] to [C12], wherein the treatment with the reversed-phase adsorbent is performed by passing the acidic tobacco extract through a column packed with the reversed-phase adsorbent.
  • [C14] The method according to any one of [C1] to [C13], wherein the pH of the tobacco extract is adjusted to 1-4.1, preferably 2-3.
  • Obtaining the acidic tobacco extract further comprises adding ethanol to the tobacco extract or to the tobacco extract adjusted to pH 4.1 or less so that the final concentration is 10% by mass or less.
  • [D1] Regenerated tobacco material obtained by the method according to any one of [C1] to [C15].
  • [E1] A tobacco product comprising the regenerated tobacco material according to any one of [D1] to [D3].
  • Example 1 In Example 1, a color analysis of bleached tobacco residue was performed.
  • Persun MP2-J is an aqueous solution containing 15% by mass of peracetic acid, 40% by mass of acetic acid, and 5.5% by mass of hydrogen peroxide.
  • bleached tobacco residue was obtained in the same procedure as above, except that hydrogen peroxide solution was used as the bleaching solution.
  • ANALYTICAL METHODS The bleached tobacco residue was subjected to color analysis. Color measurement was performed using a colorimeter (Konica Minolta, CM-5) and analysis software (Konica Minolta, Spectra Magic DX), and quantified using the L*a*b* color system. The bleached tobacco residue was freeze-dried, and the resulting tobacco residue was filled in a glass container with a transparent bottom and measured by a reflection method. Color difference ( ⁇ E*ab) was calculated by the following formula.
  • FIG. 5 shows the results of the example of the present invention
  • FIG. 6 shows the results of the comparative example.
  • the horizontal axis indicates the concentration of the bleaching solution (the concentration of Parsan MP2-J or the concentration of the hydrogen peroxide solution)
  • the vertical axis indicates the color difference.
  • white circles show the results when the reaction temperature is 22°C
  • black circles show the results when the reaction temperature is 60°C.
  • a reaction time of 120 minutes was employed in the experiments of Figures 5 and 6 .
  • Parsan MP2-J an aqueous solution containing 1.5% by weight of peracetic acid, 4% by weight of acetic acid, and 0.55% by weight of hydrogen peroxide
  • 1% by weight of Parsan MP2-J an aqueous solution containing 0.15% by weight of peracetic acid, 0.4% by weight of acetic acid, and 0.055% by weight of hydrogen peroxide
  • 0.1% by weight of Persan MP2-J an aqueous solution containing 0.015% by weight peracetic acid, 0.04% by weight acetic acid, and 0.0055% by weight hydrogen peroxide
  • 10% by mass hydrogen peroxide solution, 1% by mass hydrogen peroxide solution, and 0.1% by mass hydrogen peroxide solution were used as three types of bleaching solutions.
  • the example of the present invention (Fig. 5) has a lower concentration of bleaching agent contained in the bleaching solution than the comparative example (Fig. 6).
  • Fig. 5 has a lower concentration of bleaching agent contained in the bleaching solution than the comparative example (Fig. 6).
  • the results of FIG. 5 show that the bleaching efficiency can be increased by using an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide as the bleaching solution and performing the bleaching treatment while heating.
  • the preferred bleaching reaction temperature is about 55°C to 100°C.
  • FIG. 7 shows the results of an example of the present invention.
  • the horizontal axis indicates reaction time, and the vertical axis indicates color difference.
  • 10% by weight Parsan MP2-J was used as the bleaching solution and a reaction temperature of 60° C. was used.
  • reaction time can be set within the range of, for example, 15 minutes to 240 minutes.
  • Example 2 In Example 2, the amount of bound NNK in bleached tobacco residue was analyzed.
  • Method Bleached tobacco residue was prepared according to the method described in Example 1, and the amount of bound NNK in the bleached tobacco residue was analyzed. Analysis was performed by releasing bound NNK in tobacco residue. Specifically, 3 mL of water was added to 30 mg of bleached tobacco residue, and the mixture was heated in a closed container at 160° C. for 2 hours. After cooling, the liquid portion (containing NNK released from bound NNK) was subjected to LC-MS-MS analysis.
  • FIG. 8 shows the results of the example of the present invention
  • FIG. 9 shows the results of the example of the present invention and a comparative example.
  • the horizontal axis indicates the concentration of bleaching solution (concentration of Parsan MP2-J), and the vertical axis indicates the amount of bound NNK in relative values.
  • white circles show the results when the reaction temperature is 22°C
  • black circles show the results when the reaction temperature is 60°C.
  • the horizontal axis indicates the concentration of bleaching agent in the bleaching solution (concentration of peracetic acid in Parsun MP2-J or concentration of hydrogen peroxide in hydrogen peroxide water), and the vertical axis indicates the amount of bound NNK relative to value.
  • white circles indicate the results of the comparative example
  • black circles indicate the results of the example of the present invention.
  • a reaction time of 120 minutes was employed in the experiments of Figures 8 and 9 .
  • FIG. 8 show that bleaching tobacco residue with an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide can reduce the amount of bound NNK contained in tobacco residue.
  • FIGS. 8 and 9 show that when an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide is used as a bleaching solution, the effect of reducing bound NNK is greater than when hydrogen peroxide solution is used. high, indicating that this results in tobacco residue containing reduced amounts of bound NNK.
  • results of FIG. 8 show that the effect of reducing bound NNK can be enhanced by using an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide as the bleaching solution and performing the bleaching treatment while heating.
  • the preferred bleaching reaction temperature is about 55°C to 100°C.
  • FIG. 10 shows the results of an example of the present invention.
  • the horizontal axis indicates the reaction time
  • the vertical axis indicates the amount of bound NNK as a relative value.
  • 10% by weight Parsan MP2-J was used as the bleaching solution, and a reaction temperature of 60° C. was used.
  • FIG. 11 shows the results of an example of the present invention.
  • the horizontal axis indicates the amount of bleaching solution (solid-liquid ratio) with respect to tobacco residue, and the vertical axis indicates the amount of bound NNK in relative values.
  • 10% by weight Parsan MP2-J was employed as the bleaching solution, and a reaction temperature of 60° C. and a reaction time of 30 minutes were employed.
  • Example 3 In Example 3, the mass of bleached tobacco residue was measured.
  • Method A bleached tobacco residue was prepared according to the method described in Example 1 and the mass of the bleached tobacco residue was measured.
  • FIG. 12 shows the results of the example of the present invention
  • FIG. 13 shows the results of the comparative example
  • the horizontal axis indicates the concentration of bleaching solution (the concentration of Parsan MP2-J or the concentration of hydrogen peroxide solution)
  • the vertical axis indicates the weight of bleached tobacco residue relative to the mass of tobacco residue before bleaching. Indicates mass ratio. 12 and 13, white circles show the results when the reaction temperature is 22°C, and black circles show the results when the reaction temperature is 60°C. A reaction time of 120 minutes was employed in the experiments of Figures 12 and 13 .
  • the example of the present invention has a lower concentration of bleaching agent contained in the bleaching solution than the comparative example (Fig. 13).
  • Fig. 12 has a lower concentration of bleaching agent contained in the bleaching solution than the comparative example (Fig. 13).
  • results of FIG. 12 show that using an aqueous solution containing peracetic acid, acetic acid, and hydrogen peroxide as the bleaching solution and performing the bleaching treatment while heating can enhance the effect of reducing the mass of tobacco residue.
  • the preferred bleaching reaction temperature is about 55°C to 100°C.
  • Example 4 In Example 4, color analysis was performed on the tobacco flavor liquid.
  • Tobacco Flavor Liquid 751 g of Burley tobacco material was extracted with hot water at 60°C. After that, an aqueous solution of phosphoric acid adjusted to a predetermined pH was added, and the mixture was immersed for 30 minutes while stirring, followed by extraction with shaking for 1 hour. Thereafter, centrifugation (3000 rpm, 5 minutes) was performed, and the supernatant was filtered through a 0.45 ⁇ m membrane filter to separate the filtrate (tobacco extract) and extraction residue (tobacco residue).
  • aqueous phosphoric acid solution an aqueous potassium hydroxide solution, and an aqueous sodium sulfate solution were added to 0.5 mL of the obtained tobacco extract to adjust the pH to various values.
  • LAQUA F-72 HORIBA
  • Each of the pH-adjusted solutions (acidic tobacco extract) was passed through a reversed-phase solid-phase extraction column (Oasis-HLB). A tobacco flavor liquid was thus obtained.
  • Fig. 14 shows the analytical results of the tobacco flavor liquid obtained from the pH 2.2 acidic tobacco extract.
  • Table 1 shows the analysis results of tobacco flavor liquids obtained from acidic tobacco extracts with various pHs. In Table 1, an absorbance of about 0.1 or less indicates that the tobacco flavor liquid has the desired colorlessness.
  • results in FIG. 14 show that the acidic tobacco extract is colored, but the tobacco flavor liquid is colorless as the colored components are removed.
  • results in Table 1 show that the tobacco flavor liquid obtained from the acidic tobacco extract having a pH of 5.6 or less is colorless because the colored components are removed.
  • Example 5 In Example 5, the flavor components in the tobacco flavor liquid were analyzed.
  • Method A tobacco flavor liquid was prepared according to the method described in Example 4, and the tobacco flavor liquid was subjected to GC-MS analysis.
  • a tobacco flavor liquid was prepared from an acidic tobacco extract having a pH of 0.9 to 5.3.
  • flavor components the amounts of nicotine, myosmine, anabasine, nicotyline, anatabine, and dipyridyl were analyzed.
  • FIG. 15 shows the analysis results of nicotine.
  • FIG. 15 is a graph showing the relationship between the pH of the acidic tobacco extract and the nicotine content in the tobacco flavor liquid.
  • results of FIG. 15 show that when the tobacco flavor liquid is prepared from the acidic tobacco extract adjusted to pH 4.1 or less, nicotine is hardly removed from the acidic tobacco extract by treatment with the reversed-phase solid-phase extraction column, but when the pH is 5.5. 3, nicotine is easily removed from the acidic tobacco extract by treatment with a reversed-phase solid-phase extraction column.
  • Example 6 tobacco-specific nitrosamines (TSNAs) in tobacco flavor liquids were analyzed.
  • TSNAs tobacco-specific nitrosamines
  • Method A tobacco flavor liquid was prepared according to the method described in Example 4, and the tobacco flavor liquid was subjected to LC-MS-MS analysis.
  • a tobacco flavor liquid was prepared from an acidic tobacco extract having a pH of 0.9 to 5.3.
  • the TSNA contents shown in Table 2 are 4-(methylnitrosoamino)-1-(3-pyridyl)-1-butanone (NNK) content, N'-nitrosonornicotine (NNN) content, N'-nitrosoanatabine (NAT) content and the sum of N'-nitrosoanabasine (NAB) content.
  • the TSNA reduction rate shown in Table 2 indicates a value calculated by the following formula.
  • TSNA reduction rate [%] ⁇ (TSNA content in acidic tobacco extract) - (TSNA content in tobacco flavoring liquid) / (TSNA content in acidic tobacco extract) ⁇ x 100
  • Table 2 show that TSNAs were removed by treatment with a reversed-phase solid-phase extraction column in all cases where tobacco flavor liquids were prepared from acidic tobacco extracts adjusted to pH 0.9 to 4.1. show.
  • Example 7 In Example 7, the effect of ethanol addition on the preparation of tobacco flavor liquid was investigated.
  • Tobacco Flavor Liquid An acidic tobacco extract (pH 2.2 or 3.2) was prepared according to the method described in Example 4, and ethanol was added to the acidic tobacco extract to give a predetermined ethanol concentration. The acidic tobacco extract was then passed through a reverse-phase solid-phase extraction column (Oasis-HLB). A tobacco flavor liquid was thus obtained.
  • Tobacco flavor liquid was subjected to GC-MS analysis. Tobacco flavor liquids were prepared from acidic tobacco extracts containing various concentrations of ethanol. As flavor components, the amounts of myosmin, anabasine, anatabine, dipyridyl, benzaldehyde, phenethyl alcohol, and megastigmatrienone were analyzed.
  • FIG. 16 shows the analysis results of benzaldehyde.
  • FIG. 16 is a graph showing the relationship between the ethanol concentration in the acidic tobacco extract and the benzaldehyde content in the tobacco flavor liquid.
  • the results in FIG. 16 show that adding ethanol to the acidic tobacco extract and preparing a tobacco flavoring liquid using the obtained tobacco extract can increase the benzaldehyde content in the tobacco flavoring liquid.
  • ethanol content in the acidic tobacco extract increased, it became difficult to remove colored components by treatment with a reversed-phase solid-phase extraction column, and the colorlessness of the tobacco flavor liquid decreased.
  • the ethanol content in the acidic tobacco extract is 50% by mass, the tobacco flavoring liquid is colored brown, and when the ethanol content in the acidic tobacco extract is 10% by mass, the tobacco flavoring liquid is almost It was colorless. Therefore, ethanol is preferably added to the acidic tobacco extract so that the final concentration is 10% by mass or less.
  • the tobacco flavor liquid obtained as the final product exhibits a colorless or nearly colorless color, while exhibiting a colorless or nearly colorless color. It can be seen that the tobacco flavoring component can be included in an amount of
  • Example 8 flavor and taste evaluation was performed using a non-combustion heated flavor inhaler containing regenerated tobacco material.
  • Paper-processed sheet tobacco was prepared as a regenerated tobacco material.
  • Paper-made sheet tobacco refers to sheet tobacco manufactured using paper-making technology.
  • a tobacco material consisting of 60% by mass of yellow seeds and 40% by mass of burley seeds was extracted with hot water at 50°C for 1 hour.
  • the ratio of the mass of tobacco material to the mass of hot water was 1:20.
  • the obtained extract was separated into a liquid (tobacco extract) and a solid (tobacco residue), and each was recovered.
  • a bleaching solution ie, an aqueous solution containing 1.5% by weight peracetic acid, 4% by weight acetic acid, and 0.55% by weight hydrogen peroxide
  • the ratio of the mass of the tobacco residue to the mass of the bleaching solution was 1:40.
  • a cut sheet tobacco (example of the present invention) was prepared by cutting the paper-made sheet tobacco into pieces having a width of 0.8 mm.
  • control paper-made sheet tobacco was prepared in the same manner as the paper-made sheet tobacco above, except that the tobacco residue was not bleached.
  • the control sheet tobacco was similarly cut into 0.8 mm widths to prepare chopped sheet tobacco (control).
  • DESCRIPTION OF SYMBOLS 100... Flavor inhaler, 110... Flavor inhaling article, 120... Aerosol generator, 130... Insertion hole, 140... Lid part, 150... Push button, DESCRIPTION OF SYMBOLS 110A... Base material part 110B... Mouthpiece part 101... 1st plug winding paper 102... Filter material 103... 2nd plug winding paper 104... Filling layer 111... Filling material 112... 1st wrapping paper 113... 2nd wrapping paper , 114...Paper tube portion, 115...Filter plug, 116...Hollow plug, 117...Molding paper, 118...Filter, DESCRIPTION OF SYMBOLS 10... Battery, 20... Control unit, 30... Heater, 132... Inner cylinder member, 134... Outer cylinder member, 160... Air flow path, 170... Lid part, 180... Partition wall

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Abstract

L'invention concerne un procédé de production de résidu de tabac blanchi, le résidu de tabac étant traité avec une solution aqueuse contenant de l'acide peracétique, de l'acide acétique et du peroxyde d'hydrogène pour blanchir le résidu de tabac.
PCT/JP2021/047673 2021-12-22 2021-12-22 Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac Ceased WO2023119517A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP21968954.4A EP4454486A4 (fr) 2021-12-22 2021-12-22 Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac
JP2023568904A JP7681726B2 (ja) 2021-12-22 2021-12-22 漂白されたたばこ残渣およびその製造方法、再生たばこ材料およびその製造方法、並びにたばこ製品
PCT/JP2021/047673 WO2023119517A1 (fr) 2021-12-22 2021-12-22 Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac

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PCT/JP2021/047673 WO2023119517A1 (fr) 2021-12-22 2021-12-22 Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac

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PCT/JP2021/047673 Ceased WO2023119517A1 (fr) 2021-12-22 2021-12-22 Résidu de tabac blanchi, procédé de production s'y rapportant, matière de tabac reconstituée, procédé de production s'y rapportant et produit de tabac

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EP (1) EP4454486A4 (fr)
JP (1) JP7681726B2 (fr)
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See also references of EP4454486A4

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