WO2023210814A1 - Oral composition containing inorganic porous material - Google Patents

Oral composition containing inorganic porous material Download PDF

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Publication number
WO2023210814A1
WO2023210814A1 PCT/JP2023/016876 JP2023016876W WO2023210814A1 WO 2023210814 A1 WO2023210814 A1 WO 2023210814A1 JP 2023016876 W JP2023016876 W JP 2023016876W WO 2023210814 A1 WO2023210814 A1 WO 2023210814A1
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Prior art keywords
less
weight
oral
composition
inorganic porous
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PCT/JP2023/016876
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French (fr)
Japanese (ja)
Inventor
正人 宮内
雅之 古越
広通 武藤
慶 小林
啓佑 佐々木
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日本たばこ産業株式会社
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Publication of WO2023210814A1 publication Critical patent/WO2023210814A1/en

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B13/00Tobacco for pipes, for cigars, e.g. cigar inserts, or for cigarettes; Chewing tobacco; Snuff
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/33Heterocyclic compounds
    • A61K31/395Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
    • A61K31/435Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with one nitrogen as the only ring hetero atom
    • A61K31/465Nicotine; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02Inorganic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/10Dispersions; Emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P25/00Drugs for disorders of the nervous system
    • A61P25/26Psychostimulants, e.g. nicotine, cocaine

Definitions

  • the present invention relates to an oral composition containing an inorganic porous material.
  • the oral composition that is the filler of the oral pouch product contains water. However, in products with high moisture content, moisture may seep out due to changes in humidity during storage.
  • porous silica materials are used as carriers for pharmaceuticals and the like by taking advantage of the characteristics of their pores (see Patent Documents 1 and 2).
  • this patent document does not disclose the use of porous silica materials in oral compositions containing nicotine.
  • An object of the present invention is to provide an oral composition and an oral pouch product that suppress water seepage.
  • Aspect 1 an inorganic porous material having an average particle size of 60 ⁇ m or more as a base material; Contains nicotine and In the inorganic porous material, the pore volume of pores with a pore diameter of less than 2 nm measured by a nitrogen adsorption method and calculated using the HK method is 0.10 cm 3 /g or more, Oral composition.
  • Aspect 2 the inorganic porous material is selected from the group consisting of silica, silicate, alumina, zeolite, hydroxyapatite, hydrotalcite, and combinations thereof; The oral composition according to aspect 1.
  • Aspect 3 The inorganic porous material has a BET specific surface area of 200 to 1200 m 2 /g.
  • Aspect 4 The pore volume of pores with a pore diameter of less than 2 nm measured by the nitrogen adsorption method and calculated using the HK method is V1, The pore volume of pores with a pore diameter of 2 nm or more and less than 50 nm, measured by the nitrogen adsorption method and calculated using the BJH method, is V2, When the pore volume of pores with a pore diameter of 50 nm or more measured by mercury intrusion method is V3, V1/(V1+V2+V3) ⁇ 5% by volume, The oral composition according to any one of aspects 1 to 3.
  • Aspect 5 The oral composition according to any one of aspects 1 to 4, wherein the water content is 10% by weight or more.
  • Aspect 6 The oral cavity composition according to any one of aspects 1 to 5, comprising 6% by weight or more of the inorganic porous material.
  • Aspect 7 The oral composition according to any one of aspects 1 to 6, A packaging material for packaging the oral composition;
  • An oral pouch product comprising:
  • the present invention can provide oral compositions and oral pouch products that suppress water seepage.
  • X ⁇ Y includes the end values of X and Y.
  • Oral products are products that are contained in the oral cavity and the active ingredients are ingested through the oral mucosa through saliva.
  • Oral compositions are compositions used in oral products.
  • composition contains a specific inorganic porous material as a base material and nicotine.
  • the base material is a material that constitutes the matrix of the composition, and is also referred to as an excipient.
  • the inorganic porous material has pores with a pore diameter of less than 2 nm (hereinafter also referred to as "micropores”), and the pore volume of the pores is 0.10 cm 3 /g or more.
  • the pore volume of the pores is calculated by applying the HK method to the nitrogen adsorption isotherm obtained by measurement using the nitrogen adsorption method. Specifically, the pore volume (hereinafter referred to as (also referred to as "micropore volume”) can be determined.
  • the HK method is a method used to measure micropores, and is a method for determining pore size distribution from calculations of interactions between adsorbed molecules and interactions between adsorbed molecules and pore wall atoms.
  • pre-treat the inorganic porous material before the measurement.
  • pretreatment include heating at 200 to 250°C for 2 hours for silica, and heating at 105°C for 1 hour for cellulose.
  • an inorganic porous material having a micropore volume within the above range has high water adsorption performance in a high humidity environment, as shown by the adsorption/desorption isotherm in FIG. Therefore, the oral composition containing the inorganic porous material is less likely to be denatured during storage, and particularly water seepage during storage is reduced.
  • the lower limit of the micropore volume is preferably 0.10 cm 3 /g or more.
  • the upper limit is not limited, but is preferably 1.0 cm 3 /g or less.
  • the BET specific surface area of the inorganic porous material is preferably 200 to 1200 m 2 /g.
  • the BET specific surface area is more preferably 200 to 500 m 2 /g.
  • the micropore volume measured by the nitrogen adsorption method and the pore diameter calculated using the HK method is less than 2 nm is V1
  • the pore diameter measured by the nitrogen adsorption method and calculated using the BJH method is 2 nm.
  • V2 the pore volume of mesopores with a diameter of 50 nm or more
  • V3 the pore volume of macropores with a pore diameter of 50 nm or more measured by mercury intrusion porosimetry
  • V1/(V1+V2+V3) ⁇ 5% by volume When the volume fraction is within this range, the moisture adsorbed in the pores becomes difficult to evaporate during storage, resulting in the effect of maintaining the moisture content of the product stably for a long period of time. If the moisture stored in the product is preserved, it is expected that the product will have a moist mouthfeel when placed in the oral cavity, giving a favorable impression to the user. From this point of view, the volume fraction is more preferably 5 to 25% by volume.
  • the BJH method is an analysis method based on Kelvin's capillary condensation theory, which assumes that mesopores have a cylindrical shape.
  • the mercury intrusion method is a method in which mercury is injected into the pores of a solid surface, and the pore distribution and pore volume are determined from the relationship between the pressure applied at that time and the injected mercury volume.
  • the inorganic porous material is preferably selected from the group consisting of silica, silicates, alumina, zeolites, hydroxyapatites, hydrotalcites, and combinations thereof.
  • silica is preferred from the viewpoints of easy availability and less influence on flavor.
  • the content of the inorganic porous material in the composition is preferably 6% by weight or more. Unless otherwise specified, the content refers to the amount in an absolutely dry state.
  • the lower limit of the content is preferably 10% by weight or more, more preferably 15% by weight or more.
  • the upper limit of the content is not limited, but from the viewpoint of the limit to which other raw materials can be blended, it is usually 70% by weight or less, preferably 68% by weight or less, more preferably 65% by weight or less.
  • the average particle size of the inorganic porous material is 60 ⁇ m or more.
  • the average particle size of each material is the particle size (D50) at 50% cumulative volume based on the particle size distribution determined by laser diffraction particle size distribution measurement.
  • Laser diffraction particle size distribution measurement can be performed using, for example, Mastersizer 3000 (manufactured by Malvern Panalytical).
  • the average particle size means the particle size (D50) at which the volume integrated value is 50% in the particle size distribution. If the average particle size is less than the lower limit, the fluidity of the oral composition will decrease.
  • the lower limit of the average particle diameter is preferably 60 ⁇ m or more, more preferably 100 ⁇ m or less, and the upper limit is preferably 500 ⁇ m or less, more preferably 300 ⁇ m or less.
  • Nicotine The composition contains nicotine. Nicotine may be contained in the form of nicotine alone or in the form of a nicotine-containing raw material. Nicotine-containing raw materials refer to raw materials containing nicotine, such as nicotine salts and stabilized nicotine. Examples of stabilized nicotine include nicotine-carrying substances such as nicotine supported on an ion exchange resin. Examples of ion exchange resins include weakly acidic cation exchange resins. As the ion exchange resin on which nicotine is supported, a resin composite specifically called nicotine placrilex containing, for example, 10% by weight or more and 20% by weight or less of nicotine can be used. The ion exchange resin used in Nicotine Puracrilex is a weakly acidic cation exchange resin.
  • the amount added to the oral composition is usually 0.5% by weight or more, preferably 1.0% by weight or more, and more preferably 2.0% by weight or more. preferable.
  • the amount of nicotine puracrilex added to the composition is usually 15.0% by weight or less, preferably 12.0% by weight or less, and 10.0% by weight or less. is more preferable.
  • the nicotine-containing raw material may be a tobacco material containing, for example, tobacco powder obtained by crushing tobacco leaves.
  • Tobacco powder may include shredded dried tobacco leaf lamina, fine powder, fibers, etc., and is prepared, for example, by the method described below.
  • Tobacco leaves may include mesophylls (lamina), veins (stem), or roots.
  • the tobacco material may contain elements derived from the midribs and roots of tobacco leaves, in addition to tobacco powder that is basically obtained from the lamina of tobacco leaves.
  • the particle size of the tobacco powder is not limited, but from the viewpoint of improving its familiarity in the oral cavity and enhancing the feeling of use, and the release of the flavor components contained in the tobacco powder into the oral cavity, a diameter of 1.2 mm is preferred. It is preferable to pass through a mesh, and more preferably to pass through a 1.0 mm mesh.
  • the tobacco species used as a raw material for tobacco powder is not particularly limited, and examples thereof include the Nicotiana genus, such as the yellow variety of Nicotiana tabacum, the Burley variety, and the Brasilia variety of Nicotiana rustica. The same species can be used for tobacco materials and tobacco leaves that will be described later.
  • the tobacco powder is preferably prepared as follows. First, a base is added to tobacco powder obtained by crushing tobacco leaves and mixed.
  • the base to be added may include potassium carbonate or sodium carbonate, and is preferably added as an aqueous solution. Additionally, a pH adjuster such as sodium dihydrogen phosphate may be added, for example, to stabilize nicotine during the production of oral pouch products.
  • the pH of the mixture after addition of the base is preferably adjusted to 8.0 to 9.0.
  • the content of tobacco powder in this mixture is preferably 60 to 90% by weight.
  • heating is performed for example for 0.5 to 3 hours, preferably for 0.8 to 2 hours, under conditions such that the product temperature is 65 to 90°C, preferably 70 to 80°C.
  • Heating can be performed by either or both of heating by steam injection and heating by a jacket.
  • the pH of the mixture after heating is preferably 8.0 to 9.0, and the water content of the mixture after heating is preferably 10 to 50% by weight.
  • the obtained treated tobacco powder is dried by stopping the steam injection and heating only the jacket, if necessary. Thereafter, it may be cooled at about 15 to 25° C. for about 1 hour.
  • the amount added to the oral composition is usually 0.001% by weight or more, preferably 0.01% by weight or more, and 0.05% by weight or more. It is more preferable.
  • the amount added to the composition is usually 90% by weight or less, preferably 80% by weight or less, 70% by weight or less, 45% by weight or less, 40% by weight or less, or 30% by weight. It is as follows.
  • the nicotine-containing raw material may be a nicotine-containing extract obtained by extracting nicotine-containing substances such as tobacco leaves.
  • the above raw materials may be used alone or in combination of two or more.
  • the total nicotine content in the composition is not limited, but from the viewpoint of user preference, it is usually 0.1 to 5.0% by weight.
  • the total nicotine content in the composition is usually 0.1% by weight or more, preferably 1.0% by weight or more, and more preferably 2.0% by weight or more.
  • the total nicotine content in the composition is usually 5.0% by weight or less, preferably 4.0% by weight or less, and preferably 3.0% by weight or less. More preferred. Therefore, when using a nicotine-containing raw material as a plant-derived alkaloid, the amount of the raw material is adjusted so that the total nicotine content falls within this range.
  • the above content rate is the content rate as a nicotine ion.
  • the nicotine content in the composition can be measured using a gas chromatography mass spectrometer (GC-MS), liquid chromatography (LC, UV detection), or the like.
  • the composition includes a pH adjuster.
  • the pH adjuster is not limited, and those that are allowed to be added to foods are preferred. Examples include sodium carbonate, sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate, potassium phosphate, anhydrous sodium phosphate, sodium dihydrogen phosphate, and sodium citrate. Among these, sodium phosphate, potassium carbonate, or sodium dihydrogen phosphate is preferred from the viewpoint of influence on product taste and product stability during storage.
  • One type of pH adjuster may be used alone, or two or more types may be used in combination in any ratio.
  • the composition may contain a known gelling agent and the like.
  • the gelling agent alleviates the foreign body sensation caused by the nonwoven fabric, especially at the initial stage of taking the product, and gives a favorable impression to the user.
  • the gelling agent is preferably a polysaccharide having a carboxyl group as a functional group, such as carrageenan, pectin, gum arabic, xanthan, gellan gum, or gum tragacanth.
  • carrageenan, pectin, and gellan gum are preferred from the viewpoint of being easily gelled in the presence of calcium ions and being able to form a crosslinked structure by creating a junction zone with carboxyl groups and cations.
  • One type of these may be used alone, or two or more types may be used in combination in any ratio.
  • gelation auxiliary components include calcium ions, and the source thereof (gelation auxiliary agent) is not limited, but includes, for example, calcium halogenates (chlorides, etc.), citric acid, carbonates, sulfuric acid, etc. Examples include salts, phosphates, lactates, and the like. Among these, calcium lactate, calcium chloride, or calcium phosphate is preferable from the viewpoint of having little influence on taste, high solubility, and pH after dissolution, and calcium lactate is particularly preferable. One type of these may be used alone, or two or more types may be used in combination in any ratio.
  • gelling auxiliary ingredients other than calcium ions include metal ions such as magnesium, silver, zinc, copper, gold, and aluminum, which can bind the gelling agent through ionic bonds in the same way as calcium ions, and highly cationic ions. Examples include molecular ions. Sources of these (other gelling aids) include, for example, halogenates (chlorides, etc.) of these metal ions, citric acid, carbonates, sulfates, phosphates, and cationic polymers. can be mentioned. One type of these may be used alone, or two or more types may be used in combination in any ratio.
  • the composition may contain a known mold release agent.
  • the inorganic porous material especially silica, also functions as a mold release agent, it is not necessary to contain any mold release agent other than the inorganic porous material.
  • the water content (water content) in the composition is 10% by weight or more from the viewpoint of ease of manufacturing the composition. Furthermore, from the viewpoint of improving production efficiency, improving caking resistance, and suppressing stickiness of the composition, the lower limit of the water content is preferably 30% by weight or more, more preferably 45% by weight or more; The upper limit is usually 60% by weight or less, preferably 50% by weight or less. Further, the water content may be 40% by weight or less, 30% by weight or less, or 20% by weight or less. The water content can be adjusted by adjusting the amount of water added or by providing heat treatment or drying treatment at the manufacturing stage. The water content of the composition is appropriately adjusted depending on the type of product (moist or dry).
  • the water content is usually 20 to 60% by weight, preferably 30 to 50% by weight.
  • the water content is usually 5 to 20% by weight, preferably 10 to 15% by weight.
  • the water content (moisture content) of the composition can be measured using a heat-drying moisture meter (for example, METTER manufactured by TOLEDO: HB 43-S).
  • a heat-drying moisture meter for example, METTER manufactured by TOLEDO: HB 43-S.
  • a sample is placed in a predetermined container and heated to an ultimate temperature of 100°C. The measurement ends when the amount of change becomes 1 mg or less in 60 seconds, and the moisture content is calculated from the weighed values before and after heating.
  • composition may contain other substances in addition to the above.
  • Other substances include, for example, fragrances, sweeteners, humectants, bitterness suppressants, emulsifiers, and the like.
  • the content of the substance is not limited, and the formulation can be adjusted as appropriate depending on the product design.
  • Flavors are not limited, and examples include menthol, leaf tobacco extract, natural plant flavors (for example, cinnamon, sage, herbs, chamomile, kudzu grass, sweet tea, cloves, lavender, cardamom, cloves, nutmeg, bergamot, and geranium). , honey essence, rose oil, lemon, orange, cinnamon bark, caraway, jasmine, ginger, coriander, vanilla extract, spearmint, peppermint, cassia, coffee, celery, cascarilla, sandalwood, cocoa, ylang ylang, fennel, anise, licorice, St.
  • natural plant flavors for example, cinnamon, sage, herbs, chamomile, kudzu grass, sweet tea, cloves, lavender, cardamom, cloves, nutmeg, bergamot, and geranium.
  • honey essence rose oil, lemon, orange, cinnamon bark, caraway, jasmine, ginger, coriander, vanilla extract, spearmint, peppermint
  • John's bread, plum extract, peach extract, etc. sugars (e.g., glucose, fructose, isomerized sugar, caramel, honey, molasses, etc.), cocoa (powder, extract, etc.), esters (e.g., isoamyl acetate) , linalyl acetate, isoamyl propionate, linalyl butyrate, etc.), ketones (e.g., menthone, ionone, damascenone, ethylmaltol, etc.), alcohols (e.g., geraniol, linalool, anethole, eugenol, etc.), aldehydes (e.g., vanillin) , benzaldehyde, anisaldehyde, etc.), lactones (e.g., ⁇ -undecalactone, ⁇ -nonalactone, etc.), animal fragrances (e.g., mus
  • sweeteners examples include, but are not limited to, sugar alcohols such as xylitol, maltitol, and erythritol; and acesulfame potassium, sucralose, and aspartame. Sugar alcohols are preferred from the viewpoint of taste adjustment.
  • sugar alcohols such as xylitol, maltitol, and erythritol
  • acesulfame potassium, sucralose, and aspartame Sugar alcohols are preferred from the viewpoint of taste adjustment.
  • One type of sweetener may be used alone, or two or more types may be used in combination in any ratio.
  • the type of sugar alcohol is not particularly limited, and examples include xylitol, maltitol, erythritol, sorbitol, mannitol, and lactitol. Among these, maltitol is preferred from the viewpoint of imparting good flavor.
  • One type of these substances may be used alone, or two or more types may be used in combination in any ratio.
  • the content of sugar alcohols in the composition is not limited, but from the perspective of flavor adjustment, it is usually 1% by weight or more, and the amount of % or more, more preferably 10% by weight or more. Further, the upper limit thereof is usually 80% by weight or less, preferably 70% by weight or less, and more preferably 60% by weight or less.
  • bitter taste suppressor is not limited, but includes, for example, soybean lecithin. Soybean lecithin is a phospholipid, and specific examples include phosphatidylcholine, phosphatidylethanolamine, and phosphatidic acid. As a bitter taste suppressant, one type may be used alone, or two or more types may be used in combination in any ratio.
  • Moisturizer Moisturizers are not limited, but include, for example, polyhydric alcohols such as glycerin and propylene glycol. From the viewpoint of product preservability, glycerin is preferred. As a humectant, one type may be used alone, or two or more types may be used in combination in any ratio.
  • Emulsifier, surfactant Emulsifiers are not limited, but examples include emulsifiers added to foods.
  • the emulsifier include one or more selected from the group consisting of sucrose fatty acid ester, organic acid glycerin fatty acid ester, polyglycerin fatty acid ester, and lecithin.
  • sucrose fatty acid esters include sucrose palmitate and sucrose stearate.
  • the organic acid glycerin fatty acid ester include succinic acid glycerin fatty acid ester and diacetyl tartrate glycerin fatty acid ester.
  • the polyglycerin fatty acid ester decaglycerin fatty acid ester can be mentioned.
  • the content of the emulsifier in the composition is preferably such that the total content of the emulsifier and the aforementioned polyglycerol fatty acid ester falls within the range described above as the content of the polyglycerol fatty acid ester.
  • the degree of polymerization of glycerin in the polyglycerin fatty acid ester is preferably 2 to 10.
  • Polyglycerol fatty acid ester functions as an emulsifier. Therefore, by containing the polyglycerol fatty acid ester, the components of the composition can be kept in a uniformly mixed state, and the flavor components can be kept stable, so that the flavor of the composition can be improved.
  • the polyglycerin fatty acid ester can impart appropriate viscosity to the composition and bind each component together, so it can suppress the dryness of the composition and improve the feeling of use, flavor, etc. can.
  • the composition is a dry type with a low water content (moisture content)
  • moisture content moisture content
  • production efficiency such as work efficiency and yield in producing oral products can be improved.
  • Polyglycerin fatty acid ester is a fatty acid ester of a dehydrated condensate of glycerin, and the degree of polymerization of glycerin is usually 2 or more, and may be 3 or more, and is usually 10 or less, and 8 or less. good.
  • the fatty acid ester group (RCOO- group) of polyglycerin fatty acid ester is derived from a fatty acid.
  • the fatty acid is not limited and may be a saturated fatty acid or an unsaturated fatty acid.
  • the number of carbon atoms in the fatty acid is usually 10 or more, preferably 12 or more, more preferably 14 or more, and even more preferably 16 or more.
  • it is usually 30 or less, preferably 26 or less, more preferably 22 or less, and even more preferably 20 or less.
  • the fatty acid may have a substituent or may be unsubstituted.
  • the number of fatty acid ester groups that one molecule of polyglycerol fatty acid ester has is not limited as long as the polyglycerol fatty acid ester has a structure that can function as an emulsifier, and depends on the degree of polymerization of glycerin and the number of hydroxyl groups derived from glycerin. It can be selected as appropriate.
  • a structure that can function as an emulsifier is a structure that has both a fatty acid moiety that serves as a lipophilic group and a polyhydric alcohol moiety that serves as a hydrophilic group.
  • the number of fatty acid ester groups per molecule of polyglycerin fatty acid ester should normally be one or more.
  • the number of hydroxyl groups derived from glycerin may be one or more.
  • the degree of polymerization of glycerin and the type and number of fatty acid ester groups in the polyglycerin fatty acid ester can be arbitrarily combined as described above. More specifically, the alcohol component of the polyglycerin fatty acid ester may be diglycerin, triglycerin, tetraglycerin, pentaglycerin, hexaglycerin, heptaglycerin, octaglycerin, nonaglycerin, or decaglycerin.
  • the acid component of the polyglycerol fatty acid ester may be a fatty acid such as lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, ⁇ -linolenic acid, and the like. Further, the polyglycerin fatty acid ester may be a monoester, diester, triester, tetraester, pentaester, or the like. As the polyglycerol fatty acid ester, one type may be used alone, or two or more types may be used in combination in any ratio.
  • the polyglycerin fatty acid ester is preferably one or more selected from diglycerin monofatty acid ester and decaglycerin fatty acid ester.
  • the diglycerin monofatty acid ester is preferably selected from the group consisting of diglycerin monolaurate, diglycerin monomyristate, diglycerin monopalmitate, diglycerin monostearate and diglycerin monooleate; More preferred is oleate.
  • the decaglycerin fatty acid ester is preferably selected from the group consisting of decaglycerin laurate, decaglycerin myristate, decaglycerin palmitate, decaglycerin stearate and decaglycerin oleate; More preferably it is selected from the group consisting of myristate, decaglycerin monopalmitate, decaglycerin monostearate and decaglycerin monooleate.
  • the content of polyglycerol fatty acid esters in the composition is not limited, but from the viewpoint of obtaining good flavor and improving production efficiency. , usually at least 0.1% by weight, preferably at least 0.2% by weight, more preferably at least 0.3% by weight, even more preferably at least 0.5% by weight. Further, the content of the polyglycerol fatty acid ester is usually 20.0% by weight or less, preferably 15.0% by weight or less, and 10.0% by weight or less, preferably 15.0% by weight or less, from the viewpoint of imparting appropriate viscosity to the composition. It is more preferably at most 8.0% by weight, even more preferably at most 8.0% by weight.
  • the HLB value of the polyglycerol fatty acid ester is not limited, but from the viewpoint of obtaining good flavor and improving production efficiency, it is usually 6.0 or more, preferably 7.0 or more, and usually 20.0 or less, preferably It is 18.0 or less, more preferably 16.0 or less.
  • the taste component may further include a compound exhibiting salty, bitter, sour, umami, or the like.
  • suitable flavoring ingredients include sodium chloride, potassium chloride, ammonium chloride, peptides, citric acid, ascorbic acid, sodium glutamate, arginine, gingerol, gymnema, and the like.
  • the taste component to be blended is preferably a ligand for a taste receptor. When these taste components are received by taste receptors in the oral cavity, they can impart a flavor effect to the product's taste due to fragrances, etc., and contribute to improving the taste and palatability of the product. Typical amounts of these taste components in the composition are usually 0.5% by weight or more and 10% by weight or less, more preferably 2% by weight or more and 8% by weight or less, and even more preferably , 3% by weight or more and 5% by weight or less.
  • composition 1 Characteristics of composition 1
  • pH The pH of the composition is not limited, but from the viewpoint of influence on taste, it is usually 7.0 or higher, preferably 7.5 or higher, more preferably 8.0 or higher, and usually 10 or higher. .0 or less, preferably 9.5 or less, and more preferably 9.0 or less.
  • the pH is a measured value at 25°C.
  • the pH of the composition at a measurement temperature of 25°C is determined using a pH analyzer (for example, LAQUA F-72 flat ISFET pH electrode manufactured by Horiba), and 20 mL of water is added to 2 g of the composition, shaken for 10 minutes, It can be measured by measuring the supernatant liquid.
  • a pH analyzer for example, LAQUA F-72 flat ISFET pH electrode manufactured by Horiba
  • 20 mL of water is added to 2 g of the composition, shaken for 10 minutes, It can be measured by measuring the supernatant liquid.
  • calibrate the equipment using phthalate pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all manufactured by Wako Pure Chemical Industries). It is preferable to perform three-point calibration using
  • Moisture adsorption/desorption isotherm The ease with which water oozes out during storage can be evaluated by measuring the moisture adsorption/desorption isotherm of the composition. Specifically, a composition that has high water adsorption performance in a high-humidity environment is less likely to seep out water during storage and has excellent storage stability. Since the base material has a large contribution to this property, it can be evaluated by measuring the moisture adsorption/desorption isotherm of the base material. The moisture adsorption/desorption isotherm is measured as follows.
  • a known device can be used, and for example, BELSORP MAX II from Microtrac BEL (Microtrac Bell Co., Ltd.) can be used.
  • the sample is preferably vacuum-dried at 105° C. until the leakage is 1 Pa/min or less.
  • the adsorption isothermal behavior is measured at relative pressure intervals of 0.025 from 0.025 to 0.3 and at intervals of 0.05 relative pressure from 0.3 to 0.95. After the relative pressure reaches 0.95, the desorption isothermal behavior is measured at the same relative pressure intervals as above until the relative pressure reaches 0.1, and an adsorption/desorption isotherm is created.
  • the equilibration conditions are that when the relative pressure is 0.9 or less, the pressure change is 0.3% or less in 300 seconds, and when the relative pressure is 0.9 or more, the pressure change is 0.3 Pa or less in 300 seconds.
  • composition can be produced by any method, but it is preferably produced through a step of mixing the base material, nicotine, and, if necessary, the above-mentioned components. Mixing can be performed by charging all raw materials into a mixer and mixing them.
  • the base material, nicotine, and optionally water and other substances are mixed to obtain a first mixture.
  • heating may be applied.
  • each raw material is not limited, and they may be mixed in any order or at the same time by being added to the mixer, or solid raw materials may be mixed uniformly, then liquid raw materials may be added and further mixed. good. From the viewpoint of workability, the latter embodiment is preferable.
  • an aqueous solution containing a pH adjuster, a sweetener such as acesulfame potassium, a flavoring agent such as menthol, a bitterness suppressant such as soybean lecithin, and a humectant such as glycerin are added as necessary (additives addition step).
  • the above additives may be added in solid form or as an aqueous solution dissolved in water. When added in an aqueous solution, it may be added in advance by dissolving it in a predetermined amount of water to achieve the final moisture content of the oral product.
  • Oral pouch products are compositions that contain a composition (also called the main material or filler) within a sealed water-insoluble packaging material (also called a pouch), and saliva penetrates through the pouch and is contained within the pouch.
  • Pouch Pouches are not limited to known pouches as long as they can package the filling, do not dissolve in water, and can permeate liquids (water, saliva, etc.) and water-soluble components in the filling. Can be used. Examples of the material for the pouch include cellulose nonwoven fabric, and commercially available nonwoven fabrics may also be used.
  • a pouch product can be produced by forming a sheet made of such a material into a bag shape, filling the bag with a filler, and sealing the bag by means such as heat sealing.
  • the basis weight of the sheet is not particularly limited, and is usually 12 gsm (g/m 2 ) or more and 54 gsm or less, preferably 24 gsm or more and 30 gsm or less.
  • the thickness of the sheet is not particularly limited, and is usually 100 ⁇ m or more and 300 ⁇ m or less, preferably 175 ⁇ m or more and 215 ⁇ m or less.
  • At least one of the inner and outer surfaces of the pouch may be partially coated with a water-repellent material.
  • a water-repellent fluororesin is suitable as the water-repellent material.
  • this type of water-repellent fluororesin includes Asahi Guard (registered trademark) manufactured by Asahi Glass Co., Ltd.
  • Water-repellent fluororesins are applied to packaging materials for foods and products containing fats and oils, such as confectionery, dairy products, prepared foods, fast food, and pet food. Therefore, this type of water-repellent fluororesin is safe even when applied to pouches placed in the oral cavity.
  • the water-repellent material is not limited to fluororesin, and may be a water-repellent material such as paraffin resin, silicone resin, or epoxy resin.
  • the pouch may contain any ingredients.
  • examples of such components include raw materials that adjust aroma and taste, fragrances, additives, tobacco extracts, and pigments.
  • the manner in which these components are contained is not limited, and examples include methods in which they are applied to the surface of the pouch, impregnated, and in the case of fibers, they are contained in the fibers.
  • the appearance of the pouch is also not limited. Pouches may be non-transparent, translucent, or transparent. If the pouch is translucent or transparent, the filling can be seen through.
  • the size of the oral pouch product is not limited.
  • the size of the product before use may be such that the lower limit of the long side is 25 mm or more, 28 mm or more, 35 mm or more, or 38 mm or more.
  • the upper limit may be 40 mm or less.
  • the lower limit of the short side may be 10 mm or more or 14 mm or more.
  • the upper limit may be 20 mm or less or 18 mm or less.
  • the ratio of the weight of the filler to the total weight of the oral pouch product is not limited, but is usually 80% by weight or more, preferably 85% by weight or more, more preferably 90% by weight or more, and , usually 99% by weight or less, preferably 97% by weight or less, more preferably 95% by weight or less.
  • the oral pouch product is filled with the composition as a filler.
  • the amount of filler per oral pouch product is preferably between 0.4 and 1.5 g.
  • Oral pouch products can be manufactured by packaging the composition with an exterior material (packaging process).
  • the packaging method is not limited, and any known method can be applied.
  • a known method can be used, such as a method in which the composition is poured into a bag-shaped nonwoven fabric and then sealed.
  • desired additional water may be added after sealing (water addition process). For example, if the final composition has a water content of 50% by weight and the filled composition has a water content of 15% by weight, the remaining 35% by weight of water is added.
  • Aspect 1 an inorganic porous material having an average particle size of 60 ⁇ m or more as a base material; Contains nicotine and In the inorganic porous material, the pore volume of pores with a pore diameter of less than 2 nm measured by a nitrogen adsorption method and calculated using the HK method is 0.10 cm 3 /g or more, Oral composition.
  • Aspect 2 the inorganic porous material is selected from the group consisting of silica, silicate, alumina, zeolite, hydroxyapatite, hydrotalcite, and combinations thereof; The oral composition according to aspect 1.
  • Aspect 3 The inorganic porous material has a BET specific surface area of 200 to 1200 m 2 /g.
  • Aspect 4 The pore volume of pores with a pore diameter of less than 2 nm measured by the nitrogen adsorption method and calculated using the HK method is V1, The pore volume of pores with a pore diameter of 2 nm or more and less than 50 nm, measured by the nitrogen adsorption method and calculated using the BJH method, is V2, When the pore volume of pores with a pore diameter of 50 nm or more measured by mercury intrusion method is V3, V1/(V1+V2+V3) ⁇ 5% by volume, The oral composition according to any one of aspects 1 to 3.
  • Aspect 5 The oral composition according to any one of aspects 1 to 4, having a water content of 10% by weight or more.
  • Aspect 6 The oral cavity composition according to any one of aspects 1 to 5, comprising 6% by weight or more of the inorganic porous material.
  • Aspect 7 The oral composition according to any one of aspects 1 to 6, A packaging material for packaging the oral composition;
  • An oral pouch product comprising:
  • Example 1 Production of oral composition
  • a base material 100.0 g of silica (manufactured by Evonic, SIPERNAT2200), 3.87 g of nicotine, 45.1 g of anhydrous sodium phosphate aqueous solution, 4.79 g of anhydrous citric acid aqueous solution, 14.03 g of a sodium chloride aqueous solution and 23.4 g of an acesulfame K aqueous solution were added and mixed until homogeneous to obtain a mixture A.
  • the obtained mixture A was subjected to jacket heating (can wall temperature: 100° C.). Thereafter, the mixture was cooled for 30 minutes at an ambient temperature of 20° C. to obtain a mixture B (11% water content after cooling).
  • Example 2 An oral composition was produced in the same manner as in Example 1, except that 36.0 g of powdered cellulose (VITACEL L00, manufactured by Rettenmeyer) and 66.0 g of the silica were mixed and used as a base material.
  • VITACEL L00 powdered cellulose
  • 66.0 g of the silica were mixed and used as a base material.
  • Example 3 An oral composition was produced in the same manner as in Example 1, except that 40.0 g of powdered cellulose (VITACEL L00, manufactured by Rettenmeyer) and 60.0 g of the silica were mixed and used as a base material.
  • VITACEL L00 powdered cellulose
  • 60.0 g of the silica were mixed and used as a base material.
  • Example 4 An oral composition was produced in the same manner as in Example 1, except that 30.0 g of powdered cellulose (VITACEL L00, manufactured by Rettenmeyer) and 70.0 g of the silica were mixed and used as a base material.
  • VITACEL L00 powdered cellulose
  • Example 1 An oral composition was produced in the same manner as in Example 1, except that 100.0 g of microcrystalline cellulose (VIVAPUR200, manufactured by Rettenmeyer) was used as the base material. Table 1 shows the composition, and Table 2 shows the physical properties of the base material.
  • VIVAPUR200 microcrystalline cellulose
  • Figure 1 shows the moisture adsorption/desorption isotherms of each material.
  • the silica used in the examples has a higher ability to adsorb water, especially in high-humidity environments, than cellulose-based base materials, and it can be said that the product is less likely to be denatured by the storage environment, that is, water seepage is reduced. .
  • the average particle size of each material means the particle size (D50) at 50% cumulative volume based on the particle size distribution determined by laser diffraction particle size distribution measurement.
  • Laser diffraction particle size distribution was measured using Mastersizer 3000 (manufactured by Malvern Panalytical).
  • ⁇ Micropore analysis using nitrogen adsorption method> Pretreatment was performed under the following conditions. Silica: Heated at 250°C for 2 hours Cellulose: Heated at 105°C for 1 hour Next, a nitrogen adsorption isotherm was obtained and the micropore volume was determined by the HK method. The measurement was performed using a gas adsorption amount measuring device AutoSorb-1 (manufactured by Quantachrome).
  • ⁇ pH> Using a pH analyzer (manufactured by Horiba, Ltd.: LAQUA F-72 flat ISFET pH electrode), 20 ml of water was added to 2 g of the composition, shaken for 10 minutes, and the supernatant liquid was measured. For example, calibrate the equipment using phthalate pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all manufactured by Wako Pure Chemical Industries). This was done using a three-point calibration.
  • phthalate pH standard solution pH 4.01
  • neutral phosphate pH standard solution pH 6.86
  • borate pH standard solution pH 9.18
  • Measuring device BELSORP MAX II from MicrotracBEL (Microtrac Bell Co., Ltd.) was used. As a pretreatment, the sample was vacuum dried at 105° C. until the leakage was 1 Pa/min or less. The measurement conditions are: from relative pressure (humidity) from 0.025 to 0.3, adsorption isotherms are measured at relative pressure intervals of 0.025; from 0.3 to 0.95, adsorption isotherms are measured at relative pressure intervals of 0.05; Once a relative pressure of 0.95 was reached, the desorption isotherm was measured at the same relative pressure interval up to a relative pressure of 0.1.

Abstract

An oral composition containing an inorganic porous material having an average grain size of 60 µm or greater as a base material, and also containing nicotine, the pore volume of pores having a pore diameter of less than 2 nm, measured through nitrogen adsorption and calculated using the HK method, in the inorganic porous material being 0.10 cm3/g or greater.

Description

無機多孔質材料を含む口腔用組成物Oral composition containing inorganic porous material
 本発明は無機多孔質材料を含む口腔用組成物に関する。 The present invention relates to an oral composition containing an inorganic porous material.
 口腔用パウチ製品の充填物である口腔用組成物は水分を含む。しかし、水分含有量の高い製品においては、蔵置中の湿度変化等の影響により、水分の染み出し等が生じる可能性があった。 The oral composition that is the filler of the oral pouch product contains water. However, in products with high moisture content, moisture may seep out due to changes in humidity during storage.
 ところで、多孔質シリカ材料はその細孔の特性を活かして医薬品のキャリア等に使用される(特許文献1、2参照)。しかし当該特許文献には、多孔質シリカ材料を、ニコチンを含む口腔用組成物に用いることは開示されていない。 Incidentally, porous silica materials are used as carriers for pharmaceuticals and the like by taking advantage of the characteristics of their pores (see Patent Documents 1 and 2). However, this patent document does not disclose the use of porous silica materials in oral compositions containing nicotine.
特表2015-536939号公報Special Publication No. 2015-536939 特表2006-518761号公報Special Publication No. 2006-518761
 本発明は水の染み出しを抑制した口腔用組成物および口腔用パウチ製品を提供することを課題とする。 An object of the present invention is to provide an oral composition and an oral pouch product that suppress water seepage.
 前記課題は以下の本発明によって解決される。
態様1
 基材として平均粒径が60μm以上である無機多孔質材料と、
 ニコチンと、を含み、
 前記無機多孔質材料における、窒素吸着法で測定しHK法を用いて算出された細孔直径が2nm未満である細孔の細孔容積が0.10cm/g以上である、
口腔用組成物。
態様2
 前記無機多孔質材料が、シリカ、ケイ酸塩、アルミナ、ゼオライト、ヒドロキシアパタイト、ハイドロタルサイト、およびこれらの組合せからなる群から選択される、
態様1に記載の口腔用組成物。
態様3
 前記無機多孔質材料のBET比表面積が200~1200m/gである、
態様1または2に記載の口腔用組成物。
態様4
 前記窒素吸着法で測定し、HK法を用いて算出された細孔直径2nm未満である細孔の細孔容積をV1、
 窒素吸着法で測定し、BJH法を用いて算出された細孔直径2nm以上50nm未満である細孔の細孔容積をV2、
 水銀圧入法で測定された細孔直径50nm以上である細孔の細孔容積をV3とするとき、
 V1/(V1+V2+V3)≧5体積%である、
態様1~3のいずれかに記載の口腔用組成物。
態様5
 水の含有率が10重量%以上である、態様1~4のいずれかに記載の口腔用組成物。
態様6
 前記無機多孔質材料を6重量%以上含む、態様1~5のいずれに記載の口腔用組成物。
態様7
 態様1~6のいずれかに記載の口腔用組成物と、
 前記口腔用組成物を包装する包装材と、
を備える口腔用パウチ製品。
The above problem is solved by the present invention as described below.
Aspect 1
an inorganic porous material having an average particle size of 60 μm or more as a base material;
Contains nicotine and
In the inorganic porous material, the pore volume of pores with a pore diameter of less than 2 nm measured by a nitrogen adsorption method and calculated using the HK method is 0.10 cm 3 /g or more,
Oral composition.
Aspect 2
the inorganic porous material is selected from the group consisting of silica, silicate, alumina, zeolite, hydroxyapatite, hydrotalcite, and combinations thereof;
The oral composition according to aspect 1.
Aspect 3
The inorganic porous material has a BET specific surface area of 200 to 1200 m 2 /g.
The oral composition according to aspect 1 or 2.
Aspect 4
The pore volume of pores with a pore diameter of less than 2 nm measured by the nitrogen adsorption method and calculated using the HK method is V1,
The pore volume of pores with a pore diameter of 2 nm or more and less than 50 nm, measured by the nitrogen adsorption method and calculated using the BJH method, is V2,
When the pore volume of pores with a pore diameter of 50 nm or more measured by mercury intrusion method is V3,
V1/(V1+V2+V3)≧5% by volume,
The oral composition according to any one of aspects 1 to 3.
Aspect 5
The oral composition according to any one of aspects 1 to 4, wherein the water content is 10% by weight or more.
Aspect 6
The oral cavity composition according to any one of aspects 1 to 5, comprising 6% by weight or more of the inorganic porous material.
Aspect 7
The oral composition according to any one of aspects 1 to 6,
A packaging material for packaging the oral composition;
An oral pouch product comprising:
 本発明によって水の染み出しを抑制した口腔用組成物および口腔用パウチ製品を提供できる。 The present invention can provide oral compositions and oral pouch products that suppress water seepage.
材料の吸脱着等温線Adsorption/desorption isotherms of materials
 以下、本発明を詳細に説明する。「X~Y」は、その端値であるXおよびYを含む。口腔用製品とは、口腔に製品を含んだ状態で、唾液を介し有効成分を口腔粘膜より摂取する製品である。口腔用組成物とは口腔用製品に使用される組成物である。 Hereinafter, the present invention will be explained in detail. “X~Y” includes the end values of X and Y. Oral products are products that are contained in the oral cavity and the active ingredients are ingested through the oral mucosa through saliva. Oral compositions are compositions used in oral products.
1.口腔用組成物
 本実施態様にかかる口腔用組成物(以下単に「組成物」ともいう)は、基材として特定の無機多孔質材料と、ニコチンとを含む。基材とは、組成物のマトリックスを構成する材料であり、賦形剤ともいう。
1. Oral Composition The oral composition (hereinafter also simply referred to as "composition") according to this embodiment contains a specific inorganic porous material as a base material and nicotine. The base material is a material that constitutes the matrix of the composition, and is also referred to as an excipient.
(1)無機多孔質材料
 当該無機多孔質材料は、細孔直径が2nm未満である細孔(以下「マイクロ孔」ともいう)を有し、かつ当該細孔の細孔容積が0.10cm/g以上である。当該細孔の細孔容積は、窒素吸着法で測定し得られた窒素吸着等温線へHK法を適用し算出される。具体的に、無機多孔質材料の窒素ガス吸着等温線を求め、これにHK法を適用し解析された所定の細孔直径の範囲の細孔容積を累積することで、前記細孔容積(以下「マイクロ孔容積」ともいう)を求めることができる。HK法は、マイクロ孔の測定に使用される方法であり、吸着分子同士の相互作用や吸着分子と細孔壁原子の相互作用の計算から細孔径分布を求める方法である。窒素吸着法は公知のとおりに実施できるが、当該測定の前に無機多孔質材料を前処理することが好ましい。前処理は、シリカに対しては200~250℃で2時間加熱する、セルロースに対しては105℃で1時間加熱すること等が挙げられる。
(1) Inorganic porous material The inorganic porous material has pores with a pore diameter of less than 2 nm (hereinafter also referred to as "micropores"), and the pore volume of the pores is 0.10 cm 3 /g or more. The pore volume of the pores is calculated by applying the HK method to the nitrogen adsorption isotherm obtained by measurement using the nitrogen adsorption method. Specifically, the pore volume (hereinafter referred to as (also referred to as "micropore volume") can be determined. The HK method is a method used to measure micropores, and is a method for determining pore size distribution from calculations of interactions between adsorbed molecules and interactions between adsorbed molecules and pore wall atoms. Although the nitrogen adsorption method can be performed as known, it is preferable to pre-treat the inorganic porous material before the measurement. Examples of pretreatment include heating at 200 to 250°C for 2 hours for silica, and heating at 105°C for 1 hour for cellulose.
 マイクロ孔容積が前記範囲である無機多孔質材料は、図1の吸脱着等温線に示すとおり、高湿度環境下での水の吸着性能が高い。したがって当該無機多孔質材料を含む口腔用組成物は、保管時の変性が生じにくく、特に保存時に水の染み出し等が低減される。かかる観点から、マイクロ孔容積の下限値は、好ましくは0.10cm/g以上である。その上限値は限定されないが、好ましくは1.0cm/g以下である。 An inorganic porous material having a micropore volume within the above range has high water adsorption performance in a high humidity environment, as shown by the adsorption/desorption isotherm in FIG. Therefore, the oral composition containing the inorganic porous material is less likely to be denatured during storage, and particularly water seepage during storage is reduced. From this viewpoint, the lower limit of the micropore volume is preferably 0.10 cm 3 /g or more. The upper limit is not limited, but is preferably 1.0 cm 3 /g or less.
 無機多孔質材料のBET比表面積は好ましくは200~1200m/gである。BET比表面積がこの範囲であると香料や甘味料をはじめとした口腔用組成物中に含まれる液体成分を効率よく吸着し、製品の呈味性を維持するという効果が発現する。かかる観点から、BET比表面積はより好ましくは200~500m/gである。 The BET specific surface area of the inorganic porous material is preferably 200 to 1200 m 2 /g. When the BET specific surface area is within this range, the effect of efficiently adsorbing liquid components contained in the oral composition, such as fragrances and sweeteners, and maintaining the taste of the product is exhibited. From this viewpoint, the BET specific surface area is more preferably 200 to 500 m 2 /g.
 前記窒素吸着法で測定し、HK法を用いて算出された細孔直径が2nm未満であるマイクロ孔容積をV1、窒素吸着法で測定し、BJH法を用いて算出された細孔直径が2nm以上50nm未満であるメソ孔の細孔容積をV2、水銀圧入法で測定された細孔直径が50nm以上であるマクロ孔の細孔容積をV3とするとき、以下の関係を満たすことが好ましい。
 V1/(V1+V2+V3)≧5体積%
 当該体積分率がこの範囲であると、細孔中に吸着された水分が蔵置中に蒸発しづらくなり、製品の水分設計を長期間安定的に保たせるという効果が発現する。製品中に保存された水分が保存されると、製品を口腔に入れた際の口当たりがしっとりし、使用者に好ましい印象を与えるという効果も期待される。かかる観点から、当該体積分率はより好ましくは5~25体積%である。
The micropore volume measured by the nitrogen adsorption method and the pore diameter calculated using the HK method is less than 2 nm is V1, and the pore diameter measured by the nitrogen adsorption method and calculated using the BJH method is 2 nm. When the pore volume of mesopores with a diameter of 50 nm or more is V2, and the pore volume of macropores with a pore diameter of 50 nm or more measured by mercury intrusion porosimetry is V3, it is preferable that the following relationship is satisfied.
V1/(V1+V2+V3)≧5% by volume
When the volume fraction is within this range, the moisture adsorbed in the pores becomes difficult to evaporate during storage, resulting in the effect of maintaining the moisture content of the product stably for a long period of time. If the moisture stored in the product is preserved, it is expected that the product will have a moist mouthfeel when placed in the oral cavity, giving a favorable impression to the user. From this point of view, the volume fraction is more preferably 5 to 25% by volume.
 BJH法とは、Kelvinの毛細管凝縮理論に基づきメソ孔がシリンダー形状であると仮定した解析法である。水銀圧入法とは、水銀を固体表面の細孔の中に圧入し、その時に加えた圧力と押し込まれた水銀容積との関係から細孔分布および細孔容積を求める方法である。 The BJH method is an analysis method based on Kelvin's capillary condensation theory, which assumes that mesopores have a cylindrical shape. The mercury intrusion method is a method in which mercury is injected into the pores of a solid surface, and the pore distribution and pore volume are determined from the relationship between the pressure applied at that time and the injected mercury volume.
 無機多孔質材料は、好ましくはシリカ、ケイ酸塩、アルミナ、ゼオライト、ヒドロキシアパタイト、ハイドロタルサイト、およびこれらの組合せからなる群から選択される。中でも、入手容易性、および香味への影響が少ない等の観点からシリカが好ましい。 The inorganic porous material is preferably selected from the group consisting of silica, silicates, alumina, zeolites, hydroxyapatites, hydrotalcites, and combinations thereof. Among these, silica is preferred from the viewpoints of easy availability and less influence on flavor.
 組成物中、無機多孔質材料の含有量は6重量%以上であることが好ましい。含有量は、特に断りがない限り、絶乾状態での量をいう。前記含有量の下限値は、好ましくは10重量%以上、より好ましくは15重量%以上である。前記含有率の上限は限定されないが、その他の原料を配合できる限界の観点から、通常70重量%以下であり、好ましくは68重量%以下、より好ましくは65重量%以下である。 The content of the inorganic porous material in the composition is preferably 6% by weight or more. Unless otherwise specified, the content refers to the amount in an absolutely dry state. The lower limit of the content is preferably 10% by weight or more, more preferably 15% by weight or more. The upper limit of the content is not limited, but from the viewpoint of the limit to which other raw materials can be blended, it is usually 70% by weight or less, preferably 68% by weight or less, more preferably 65% by weight or less.
 無機多孔質材料の平均粒径は60μm以上である。各材料の平均粒径は、レーザー回折粒度分布測定により求めた粒度分布における体積基準累積50%での粒径(D50)である。レーザー回折粒度分布測定には、例えばマスターサイザー3000(マルバーン・パナリティカル社製)を用いて測定できる。平均粒径は、特段の断りがない限り、粒度分布において体積積算値が50%となる粒径(D50)を意味する。平均粒径が前記下限値未満であると、口腔用組成物の流動性が低下する。また、平均粒径が過度に高いと前記無機多孔質材料の粒子によるざらつきをユーザーが知覚しやすくなり、製品の口当たりを不快に感じる要因となりうる。かかる観点から、平均粒径の下限値は、好ましくは60μm以上であり、より好ましくは100μm以下であり、その上限値は、好ましくは500μm以下であり、より好ましくは300μm以下である。 The average particle size of the inorganic porous material is 60 μm or more. The average particle size of each material is the particle size (D50) at 50% cumulative volume based on the particle size distribution determined by laser diffraction particle size distribution measurement. Laser diffraction particle size distribution measurement can be performed using, for example, Mastersizer 3000 (manufactured by Malvern Panalytical). Unless otherwise specified, the average particle size means the particle size (D50) at which the volume integrated value is 50% in the particle size distribution. If the average particle size is less than the lower limit, the fluidity of the oral composition will decrease. Furthermore, if the average particle size is too high, the user will be more likely to perceive roughness due to the particles of the inorganic porous material, which may cause the product to feel unpleasant to the mouth. From this viewpoint, the lower limit of the average particle diameter is preferably 60 μm or more, more preferably 100 μm or less, and the upper limit is preferably 500 μm or less, more preferably 300 μm or less.
(2)ニコチン
 組成物はニコチンを含む。ニコチンは、ニコチン単体の形態で含有されてもよいし、ニコチン含有原料の形態で含有されていてもよい。ニコチン含有原料とは、ニコチン塩や安定化させたニコチン等のニコチンを含む原料をいう。安定化させたニコチンとしては、例えばイオン交換樹脂に担持させたニコチン等のニコチン担持物質が挙げられる。イオン交換樹脂として、弱酸性陽イオン交換樹脂を挙げることができる。ニコチンが担持されたイオン交換樹脂として、具体的にニコチンポラクリレックスと呼ばれる、例えば10重量%以上、20重量%以下のニコチンを含有する樹脂複合体を用いることができる。ニコチンポラクリレックスで用いられるイオン交換樹脂は弱酸性陽イオン交換樹脂である。ニコチンポラクリレックスを用いる場合、口腔用組成物に対する添加量は、通常0.5重量%以上であり、1.0重量%以上であることが好ましく、2.0重量%以上であることがより好ましい。一方、風味の観点から、組成物に対するニコチンポラクリレックスの添加量は、通常15.0重量%以下であり、12.0重量%以下であることが好ましく、10.0重量%以下であることがより好ましい。
(2) Nicotine The composition contains nicotine. Nicotine may be contained in the form of nicotine alone or in the form of a nicotine-containing raw material. Nicotine-containing raw materials refer to raw materials containing nicotine, such as nicotine salts and stabilized nicotine. Examples of stabilized nicotine include nicotine-carrying substances such as nicotine supported on an ion exchange resin. Examples of ion exchange resins include weakly acidic cation exchange resins. As the ion exchange resin on which nicotine is supported, a resin composite specifically called nicotine placrilex containing, for example, 10% by weight or more and 20% by weight or less of nicotine can be used. The ion exchange resin used in Nicotine Puracrilex is a weakly acidic cation exchange resin. When using nicotine Puracrilex, the amount added to the oral composition is usually 0.5% by weight or more, preferably 1.0% by weight or more, and more preferably 2.0% by weight or more. preferable. On the other hand, from the viewpoint of flavor, the amount of nicotine puracrilex added to the composition is usually 15.0% by weight or less, preferably 12.0% by weight or less, and 10.0% by weight or less. is more preferable.
 また、ニコチン含有原料は、例えばたばこ葉を粉砕したたばこ粉末を含むたばこ材料であってもよい。たばこ粉末は、乾燥したたばこ葉のラミナの刻み、微粉、または繊維等を含んでもよく、例えば後述する方法によって調製される。たばこ葉は、葉肉(ラミナ)、葉脈(ステム)、または根を含んでもよい。前記たばこ材料は、基本的にたばこ葉のラミナから得られるたばこ粉末の他に、たばこ葉の中骨や根に由来する要素を含んでいてもよい。 Furthermore, the nicotine-containing raw material may be a tobacco material containing, for example, tobacco powder obtained by crushing tobacco leaves. Tobacco powder may include shredded dried tobacco leaf lamina, fine powder, fibers, etc., and is prepared, for example, by the method described below. Tobacco leaves may include mesophylls (lamina), veins (stem), or roots. The tobacco material may contain elements derived from the midribs and roots of tobacco leaves, in addition to tobacco powder that is basically obtained from the lamina of tobacco leaves.
 たばこ粉末の粒径は限定されないが、口腔内でのなじみを良好にして使用感を高めることと、たばこ粉末に含まれる香味成分の口腔内への放出を良好にする観点から、1.2mmのメッシュを通過したものであることが好ましく、1.0mmのメッシュを通過したものであることがより好ましい。 The particle size of the tobacco powder is not limited, but from the viewpoint of improving its familiarity in the oral cavity and enhancing the feeling of use, and the release of the flavor components contained in the tobacco powder into the oral cavity, a diameter of 1.2 mm is preferred. It is preferable to pass through a mesh, and more preferably to pass through a 1.0 mm mesh.
 たばこ粉末の原料となるたばこ種は特に限定されず、例えばニコチアナ属であり、ニコチアナ・タバカムの黄色種、バーレー種、ニコチアナ・ルスチカのブラジリア種などを例示できる。後述するたばこ材料およびたばこ葉についてもこれらと同じ種を使用できる。 The tobacco species used as a raw material for tobacco powder is not particularly limited, and examples thereof include the Nicotiana genus, such as the yellow variety of Nicotiana tabacum, the Burley variety, and the Brasilia variety of Nicotiana rustica. The same species can be used for tobacco materials and tobacco leaves that will be described later.
 たばこ粉末は以下のようにして調製されることが好ましい。まず、たばこ葉を粉砕して得たたばこ粉末に対して、塩基を添加して混合する。添加する塩基としては炭酸カリウムまたは炭酸ナトリウムを挙げることでき、水溶液として添加することが好ましい。また、例えば口腔用パウチ製品製造時のニコチン安定化のため、リン酸二水素ナトリウムのようなpH調整剤を添加してもよい。塩基の添加後の混合物のpHは8.0~9.0に調整されることが好ましい。この混合物における、たばこ粉末の含有率は、60~90重量%であることが好ましい。 The tobacco powder is preferably prepared as follows. First, a base is added to tobacco powder obtained by crushing tobacco leaves and mixed. The base to be added may include potassium carbonate or sodium carbonate, and is preferably added as an aqueous solution. Additionally, a pH adjuster such as sodium dihydrogen phosphate may be added, for example, to stabilize nicotine during the production of oral pouch products. The pH of the mixture after addition of the base is preferably adjusted to 8.0 to 9.0. The content of tobacco powder in this mixture is preferably 60 to 90% by weight.
 塩基を添加した後、例えば品温が65~90℃、好ましくは品温が70~80℃となる条件で、例えば0.5~3時間、好ましくは0.8~2時間加熱を行う。これにより、たばこ粉末の殺菌が行われる。加熱は、蒸気注入による加熱と、ジャケットによる加熱のどちらか一方または両方により行うことができる。加熱後の混合物のpHは8.0~9.0であることが好ましく、加熱後の混合物の含水率は10~50重量%であることが好ましい。 After adding the base, heating is performed for example for 0.5 to 3 hours, preferably for 0.8 to 2 hours, under conditions such that the product temperature is 65 to 90°C, preferably 70 to 80°C. This sterilizes the tobacco powder. Heating can be performed by either or both of heating by steam injection and heating by a jacket. The pH of the mixture after heating is preferably 8.0 to 9.0, and the water content of the mixture after heating is preferably 10 to 50% by weight.
 加熱後、得られた処理たばこ粉末に対して必要に応じて蒸気注入を止めてジャケットのみの加熱を行ない、乾燥処理を行う。その後、15~25℃程度で1時間程度、冷却する態様を挙げることができる。 After heating, the obtained treated tobacco powder is dried by stopping the steam injection and heating only the jacket, if necessary. Thereafter, it may be cooled at about 15 to 25° C. for about 1 hour.
 たばこ粉末を含むたばこ材料を用いる場合、口腔用組成物に対するその添加量は、通常0.001重量%以上であり、0.01重量%以上であることが好ましく、0.05重量%以上であることがより好ましい。一方、風味の観点から、前記組成物に対するその添加量は、通常90重量%以下であり、好ましくは80重量%以下、70重量%以下、45重量%以下、40重量%以下、または30重量%以下である。 When using a tobacco material containing tobacco powder, the amount added to the oral composition is usually 0.001% by weight or more, preferably 0.01% by weight or more, and 0.05% by weight or more. It is more preferable. On the other hand, from the viewpoint of flavor, the amount added to the composition is usually 90% by weight or less, preferably 80% by weight or less, 70% by weight or less, 45% by weight or less, 40% by weight or less, or 30% by weight. It is as follows.
 ニコチン含有原料は、たばこ葉等のニコチン含有物質を抽出することにより得られるニコチン含有抽出液であってもよい。 The nicotine-containing raw material may be a nicotine-containing extract obtained by extracting nicotine-containing substances such as tobacco leaves.
 上記の態様の中でも、的確なニコチンの供給や、取扱い易さの観点から、ニコチン担持物質を用いることが好ましい。また、通常、たばこ粉末を添加した場合、口腔用組成物や口腔用製品の色がたばこ葉の色となる傾向がある。一方で、無色のニコチン含有化合物を用いた場合、白色の組成物や口腔用製品を提供することが可能となる。白色の口腔用製品を好む使用者にとって、このような態様は利点である。上記の原料は、1種を用いてもよいし、2種以上を併用してもよい。 Among the above embodiments, it is preferable to use a nicotine-carrying substance from the viewpoint of accurate nicotine supply and ease of handling. Additionally, when tobacco powder is added, the color of the oral composition or oral product tends to be the color of tobacco leaves. On the other hand, when a colorless nicotine-containing compound is used, it is possible to provide white compositions and oral products. Such an embodiment is an advantage for users who prefer white oral products. The above raw materials may be used alone or in combination of two or more.
 組成物中の総ニコチンの含有率は限定されないが、ユーザーの嗜好性の観点から、通常0.1~5.0重量%である。組成物中の総ニコチンの含有率は、通常0.1重量%以上であり、1.0重量%以上であることが好ましく、2.0重量%以上であることがより好ましい。一方、風味の観点から、組成物中の総ニコチンの含有率は、通常5.0重量%以下であり、4.0重量%以下であることが好ましく、3.0重量%以下であることがより好ましい。したがって植物由来アルカロイドとしてニコチン含有原料を用いる場合は、総ニコチン含有率がこの範囲になるように当該原料の量は調整される。ニコチンがイオンとして存在する場合、上記の含有率は、ニコチンイオンとしての含有率である。前記組成物中のニコチンの含有率は、ガスクロマトグラフィー質量分析計(GC-MS)、液体クロマトグラフィー(LC、UV検出)等で測定することができる。 The total nicotine content in the composition is not limited, but from the viewpoint of user preference, it is usually 0.1 to 5.0% by weight. The total nicotine content in the composition is usually 0.1% by weight or more, preferably 1.0% by weight or more, and more preferably 2.0% by weight or more. On the other hand, from the viewpoint of flavor, the total nicotine content in the composition is usually 5.0% by weight or less, preferably 4.0% by weight or less, and preferably 3.0% by weight or less. More preferred. Therefore, when using a nicotine-containing raw material as a plant-derived alkaloid, the amount of the raw material is adjusted so that the total nicotine content falls within this range. When nicotine exists as an ion, the above content rate is the content rate as a nicotine ion. The nicotine content in the composition can be measured using a gas chromatography mass spectrometer (GC-MS), liquid chromatography (LC, UV detection), or the like.
(3)pH調整剤
 組成物はpH調整剤を含む。pH調整剤は限定されず、食品に添加されることが許容されているものが好ましい。例えば、炭酸ナトリウム、炭酸水素ナトリウム、炭酸カリウム、炭酸水素カリウム、リン酸カリウム、無水リン酸ナトリウム、リン酸二水素ナトリウム、およびクエン酸ナトリウム等が挙げられる。中でも、製品の呈味および保存中の製品安定性への影響の観点から、リン酸ナトリウム、炭酸カリウム、またはリン酸二水素ナトリウムが好ましい。pH調整剤として1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。
(3) pH adjuster The composition includes a pH adjuster. The pH adjuster is not limited, and those that are allowed to be added to foods are preferred. Examples include sodium carbonate, sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate, potassium phosphate, anhydrous sodium phosphate, sodium dihydrogen phosphate, and sodium citrate. Among these, sodium phosphate, potassium carbonate, or sodium dihydrogen phosphate is preferred from the viewpoint of influence on product taste and product stability during storage. One type of pH adjuster may be used alone, or two or more types may be used in combination in any ratio.
(4)ゲル化剤、ゲル化補助剤
 組成物は、公知のゲル化剤等を含んでいてもよい。ゲル化剤は、製品を口腔に服用した際、特に服用初期時点での不織布等による異物感を緩和し、使用者に好ましい印象を与える。当該ゲル化剤としては、官能基としてカルボキシル基を有する多糖類が好ましく、例えば、カラギーナン、ペクチン、アラビアガム、キサンタン、ジェランガム、トラガントガムが好ましい。さらに、カルシウムイオンの存在下でゲル化しやすく、カルボキシル基と陽イオンでジャンクションゾーンを作り架橋構造を形成することができる観点から、カラギーナン、ペクチン、ジェランガムが好ましい。これらは、1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。
(4) Gelling agent, gelling aid The composition may contain a known gelling agent and the like. When the product is taken into the oral cavity, the gelling agent alleviates the foreign body sensation caused by the nonwoven fabric, especially at the initial stage of taking the product, and gives a favorable impression to the user. The gelling agent is preferably a polysaccharide having a carboxyl group as a functional group, such as carrageenan, pectin, gum arabic, xanthan, gellan gum, or gum tragacanth. Furthermore, carrageenan, pectin, and gellan gum are preferred from the viewpoint of being easily gelled in the presence of calcium ions and being able to form a crosslinked structure by creating a junction zone with carboxyl groups and cations. One type of these may be used alone, or two or more types may be used in combination in any ratio.
 ゲル化補助成分としては、例えばカルシウムイオンが挙げられ、その供給源(ゲル化補助剤)は、は限定されないが、例えば、カルシウムのハロゲン酸塩(塩化物等)、クエン酸、炭酸塩、硫酸塩、リン酸塩、および乳酸塩等が挙げられる。これらのうち、味への影響が少ない、溶解性が高い、および溶解後のpHの観点から、乳酸カルシウム、塩化カルシウム、またはリン酸カルシウムが好ましく、特に、乳酸カルシウムが好ましい。これらは1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。 Examples of gelation auxiliary components include calcium ions, and the source thereof (gelation auxiliary agent) is not limited, but includes, for example, calcium halogenates (chlorides, etc.), citric acid, carbonates, sulfuric acid, etc. Examples include salts, phosphates, lactates, and the like. Among these, calcium lactate, calcium chloride, or calcium phosphate is preferable from the viewpoint of having little influence on taste, high solubility, and pH after dissolution, and calcium lactate is particularly preferable. One type of these may be used alone, or two or more types may be used in combination in any ratio.
 カルシウムイオン以外のゲル化補助成分としては、例えば、カルシウムイオンと同様にゲル化剤をイオン結合で結合させることができるマグネシウム、銀、亜鉛、銅、金、アルミニウム等の金属イオン、およびカチオン性高分子のイオン等が挙げられる。これらの供給源(その他のゲル化補助剤)としては、例えば、これらの金属イオンのハロゲン酸塩(塩化物等)、クエン酸、炭酸塩、硫酸塩、リン酸塩、およびカチオン性高分子等が挙げられる。これらは1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。 Examples of gelling auxiliary ingredients other than calcium ions include metal ions such as magnesium, silver, zinc, copper, gold, and aluminum, which can bind the gelling agent through ionic bonds in the same way as calcium ions, and highly cationic ions. Examples include molecular ions. Sources of these (other gelling aids) include, for example, halogenates (chlorides, etc.) of these metal ions, citric acid, carbonates, sulfates, phosphates, and cationic polymers. can be mentioned. One type of these may be used alone, or two or more types may be used in combination in any ratio.
(5)離型剤
 組成物は公知の離型剤を含んでいてもよい。しかしながら前記無機多孔質材料、特にシリカは離型剤としての機能を兼ね備えるので、当該無機多孔質材料以外の離型剤を含んでいなくてもよい。
(5) Mold release agent The composition may contain a known mold release agent. However, since the inorganic porous material, especially silica, also functions as a mold release agent, it is not necessary to contain any mold release agent other than the inorganic porous material.
(6)水
 組成物中の水の含有率(含水率)は、当該組成物の製造容易性の観点から、10重量%以上である。さらに、組成物の製造効率向上、耐ケーキング性向上、べたつき抑制等の観点から、水の含有率の下限は30重量%以上であることが好ましく、45重量%以上であることがより好ましく、その上限は通常60重量%以下であり、50重量%以下であることが好ましい。また、水の含有率は40重量%以下であってもよく、30重量%以下であってもよく、20重量%以下であってもよい。水の含有率は、添加する水の量を調整したり、製造段階で加熱処理や乾燥処理を設けたりすることによって調整することができる。前記組成物の水の含有率は、製品のタイプ(モイストまたはドライ)に応じて適宜調整される。例えばモイストタイプの場合、水の含有率は通常20~60重量%であり、好ましくは30~50重量%である。一方、ドライタイプの場合、水の含有率は通常5~20重量%であり、好ましくは10~15重量%である。
(6) Water The water content (water content) in the composition is 10% by weight or more from the viewpoint of ease of manufacturing the composition. Furthermore, from the viewpoint of improving production efficiency, improving caking resistance, and suppressing stickiness of the composition, the lower limit of the water content is preferably 30% by weight or more, more preferably 45% by weight or more; The upper limit is usually 60% by weight or less, preferably 50% by weight or less. Further, the water content may be 40% by weight or less, 30% by weight or less, or 20% by weight or less. The water content can be adjusted by adjusting the amount of water added or by providing heat treatment or drying treatment at the manufacturing stage. The water content of the composition is appropriately adjusted depending on the type of product (moist or dry). For example, in the case of a moist type, the water content is usually 20 to 60% by weight, preferably 30 to 50% by weight. On the other hand, in the case of a dry type, the water content is usually 5 to 20% by weight, preferably 10 to 15% by weight.
 組成物の水の含有率(含水率)は、加熱乾燥式水分計(例えば、METTER TOLEDO社製:HB 43-S)を用いて測定することができる。測定に際し、試料を所定容器に投入し到達温度100℃まで加熱する。測定は60秒間で1mg以下の変化量となった時点で終了し、加熱前後の秤量値より含水率を算出する。 The water content (moisture content) of the composition can be measured using a heat-drying moisture meter (for example, METTER manufactured by TOLEDO: HB 43-S). For measurement, a sample is placed in a predetermined container and heated to an ultimate temperature of 100°C. The measurement ends when the amount of change becomes 1 mg or less in 60 seconds, and the moisture content is calculated from the weighed values before and after heating.
(7)その他
 組成物は、上記以外に他の物質を含んでいてもよい。その他の物質としては、例えば、香料、甘味料、保湿剤、苦味抑制剤、および乳化剤等が挙げられる。当該物質の含有率は、限定されず、製品設計に応じて適宜配合を調整することができる。
(7) Others The composition may contain other substances in addition to the above. Other substances include, for example, fragrances, sweeteners, humectants, bitterness suppressants, emulsifiers, and the like. The content of the substance is not limited, and the formulation can be adjusted as appropriate depending on the product design.
 1)香料
 香料は限定されず、例えば、メンソール、葉たばこ抽出エキス、天然植物性香料(例えば、シナモン、セージ、ハーブ、カモミール、葛草、甘茶、クローブ、ラベンダー、カルダモン、チョウジ、ナツメグ、ベルガモット、ゼラニウム、蜂蜜エッセンス、ローズ油、レモン、オレンジ、ケイ皮、キャラウェー、ジャスミン、ジンジャー、コリアンダー、バニラエキス、スペアミント、ペパーミント、カシア、コーヒー、セロリー、カスカリラ、サンダルウッド、ココア、イランイラン、フェンネル、アニス、リコリス、セントジョンズブレッド、スモモエキス、ピーチエキス等)、糖類(例えば、グルコース、フルクトース、異性化糖、カラメル、蜂蜜、糖蜜等)、ココア類(パウダー、エキス等)、エステル類(例えば、酢酸イソアミル、酢酸リナリル、プロピオン酸イソアミル、酪酸リナリル等)、ケトン類(例えば、メントン、イオノン、ダマセノン、エチルマルトール等)、アルコール類(例えば、ゲラニオール、リナロール、アネトール、オイゲノール等)、アルデヒド類(例えば、バニリン、ベンズアルデヒド、アニスアルデヒド等)、ラクトン類(例えば、γ-ウンデカラクトン、γ-ノナラクトン等)、動物性香料(例えば、ムスク、アンバーグリス、シベット、カストリウム等)、および炭化水素類(例えば、リモネン、ピネン等)が挙げられる。香料として1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。
1) Flavors Flavors are not limited, and examples include menthol, leaf tobacco extract, natural plant flavors (for example, cinnamon, sage, herbs, chamomile, kudzu grass, sweet tea, cloves, lavender, cardamom, cloves, nutmeg, bergamot, and geranium). , honey essence, rose oil, lemon, orange, cinnamon bark, caraway, jasmine, ginger, coriander, vanilla extract, spearmint, peppermint, cassia, coffee, celery, cascarilla, sandalwood, cocoa, ylang ylang, fennel, anise, licorice, St. John's bread, plum extract, peach extract, etc.), sugars (e.g., glucose, fructose, isomerized sugar, caramel, honey, molasses, etc.), cocoa (powder, extract, etc.), esters (e.g., isoamyl acetate) , linalyl acetate, isoamyl propionate, linalyl butyrate, etc.), ketones (e.g., menthone, ionone, damascenone, ethylmaltol, etc.), alcohols (e.g., geraniol, linalool, anethole, eugenol, etc.), aldehydes (e.g., vanillin) , benzaldehyde, anisaldehyde, etc.), lactones (e.g., γ-undecalactone, γ-nonalactone, etc.), animal fragrances (e.g., musk, ambergris, civet, castoreum, etc.), and hydrocarbons (e.g., limonene, etc.). , pinene, etc.). One type of fragrance may be used alone, or two or more types may be used in combination in any ratio.
 2)甘味料
 甘味料としては、限定されないが、例えばキシリトール、マルチトール、エリスリトール等の糖アルコール;およびアセスルファムカリウム、スクラロース、アスパルテーム等が挙げられる。味の調節の観点から糖アルコールが好ましい。甘味料は、1種類を単独で用いてもよく、また、2種類以上を任意の比率で併用してもよい。
2) Sweeteners Examples of sweeteners include, but are not limited to, sugar alcohols such as xylitol, maltitol, and erythritol; and acesulfame potassium, sucralose, and aspartame. Sugar alcohols are preferred from the viewpoint of taste adjustment. One type of sweetener may be used alone, or two or more types may be used in combination in any ratio.
 糖アルコールの種類は特に限定されず、例えば、キシリトール、マルチトール、エリスリトール、ソルビトール、マンニトール、およびラクチトール等を挙げることができる。これらのうち、良好な風味を付与する観点から、マルチトールが好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の比率で併用してもよい。 The type of sugar alcohol is not particularly limited, and examples include xylitol, maltitol, erythritol, sorbitol, mannitol, and lactitol. Among these, maltitol is preferred from the viewpoint of imparting good flavor. One type of these substances may be used alone, or two or more types may be used in combination in any ratio.
 組成物中の糖アルコールの含有率(糖アルコールを2種類以上含有する場合は、それらの総含有率)は、限定されないが、風味の調節の観点から、通常1重量%以上であり、5量%以上であることが好ましく、10重量%以上であることがより好ましい。また、その上限は、通常80重量%以下であり、70重量%以下であることが好ましく、60重量%以下であることがより好ましい。 The content of sugar alcohols in the composition (if it contains two or more types of sugar alcohols, their total content) is not limited, but from the perspective of flavor adjustment, it is usually 1% by weight or more, and the amount of % or more, more preferably 10% by weight or more. Further, the upper limit thereof is usually 80% by weight or less, preferably 70% by weight or less, and more preferably 60% by weight or less.
 3)苦味抑制剤
 苦味抑制剤は限定されないが、例えば、大豆レシチンが挙げられる。大豆レシチンとはリン脂質であり、具体的にホスファチジルコリン、ホスファチジルエタノールアミン、およびホスファチジン酸等が挙げられる。苦味抑制剤として1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。
3) Bitter taste suppressor The bitter taste suppressor is not limited, but includes, for example, soybean lecithin. Soybean lecithin is a phospholipid, and specific examples include phosphatidylcholine, phosphatidylethanolamine, and phosphatidic acid. As a bitter taste suppressant, one type may be used alone, or two or more types may be used in combination in any ratio.
 4)保湿剤
 保湿剤は限定されないが、例えば、グリセリンおよびプロピレングリコール等の多価アルコールが挙げられる。製品保存性の観点から、グリセリンが好ましい。保湿剤として1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。
4) Moisturizer Moisturizers are not limited, but include, for example, polyhydric alcohols such as glycerin and propylene glycol. From the viewpoint of product preservability, glycerin is preferred. As a humectant, one type may be used alone, or two or more types may be used in combination in any ratio.
 5)乳化剤、界面活性剤
 乳化剤は限定されないが、例えば、食品に添加される乳化剤を挙げることができる。乳化剤としては、ショ糖脂肪酸エステル、有機酸グリセリン脂肪酸エステル、ポリグリセリン脂肪酸エステルおよびレシチンからなる群から選ばれる一種以上を挙げることができる。ショ糖脂肪酸エステルとして、ショ糖パルミチン酸エステルおよびショ糖ステアリン酸エステルを挙げることができる。有機酸グリセリン脂肪酸エステルとして、コハク酸グリセリン脂肪酸エステルおよびジアセチル酒石酸グリセリン脂肪酸エステルを挙げることができる。ポリグリセリン脂肪酸エステルとして、デカグリセリン脂肪酸エステルを挙げることができる。前記組成物における乳化剤の含有率は、前述のポリグリセリン脂肪酸エステルとの合計含有率が、ポリグリセリン脂肪酸エステルの含有率として上述した範囲内となる量であることが好ましい。
5) Emulsifier, surfactant Emulsifiers are not limited, but examples include emulsifiers added to foods. Examples of the emulsifier include one or more selected from the group consisting of sucrose fatty acid ester, organic acid glycerin fatty acid ester, polyglycerin fatty acid ester, and lecithin. Examples of sucrose fatty acid esters include sucrose palmitate and sucrose stearate. Examples of the organic acid glycerin fatty acid ester include succinic acid glycerin fatty acid ester and diacetyl tartrate glycerin fatty acid ester. As the polyglycerin fatty acid ester, decaglycerin fatty acid ester can be mentioned. The content of the emulsifier in the composition is preferably such that the total content of the emulsifier and the aforementioned polyglycerol fatty acid ester falls within the range described above as the content of the polyglycerol fatty acid ester.
 ポリグリセリン脂肪酸エステルにおけるグリセリンの重合度は2~10であることが好ましい。ポリグリセリン脂肪酸エステルは、乳化剤として機能する。そのため、ポリグリセリン脂肪酸エステルを含有することにより、組成物の各成分の均一な混合状態が保持され、香味成分を安定に保つことができるため、当該組成物の香味を良好にすることができる。また、ポリグリセリン脂肪酸エステルは、組成物に適度な粘性を付与し、各成分を一体に結着させることができるため、当該組成物のぱさつきを抑え、使用感、香味等を良好にすることができる。加えて、組成物が水の含有量(含水率)の少ないドライタイプの場合でも、当該組成物をパウチ等の外装材に充填する際に、当該組成物が飛散することを抑制できる。このように、前記組成物にポリグリセリン脂肪酸エステルを含有させることで、口腔用製品の製造における作業効率、歩留まり等の製造効率を向上することができる。 The degree of polymerization of glycerin in the polyglycerin fatty acid ester is preferably 2 to 10. Polyglycerol fatty acid ester functions as an emulsifier. Therefore, by containing the polyglycerol fatty acid ester, the components of the composition can be kept in a uniformly mixed state, and the flavor components can be kept stable, so that the flavor of the composition can be improved. In addition, the polyglycerin fatty acid ester can impart appropriate viscosity to the composition and bind each component together, so it can suppress the dryness of the composition and improve the feeling of use, flavor, etc. can. In addition, even if the composition is a dry type with a low water content (moisture content), it is possible to prevent the composition from scattering when filling an exterior material such as a pouch with the composition. In this way, by including the polyglycerol fatty acid ester in the composition, production efficiency such as work efficiency and yield in producing oral products can be improved.
 ポリグリセリン脂肪酸エステルは、グリセリンの脱水縮合体の脂肪酸エステルであり、グリセリンの重合度は、通常2以上であり、3以上であってもよく、また、通常10以下であり、8以下であってよい。 Polyglycerin fatty acid ester is a fatty acid ester of a dehydrated condensate of glycerin, and the degree of polymerization of glycerin is usually 2 or more, and may be 3 or more, and is usually 10 or less, and 8 or less. good.
 ポリグリセリン脂肪酸エステルの脂肪酸エステル基(RCOO-基)は、脂肪酸に由来する。当該脂肪酸は限定されず、飽和脂肪酸であってもよく、不飽和脂肪酸であってもよい。また、当該脂肪酸の炭素数は、良好な香味および製造効率の観点から、通常10以上であり、12以上であることが好ましく、14以上であることがより好ましく、16以上であることがさらに好ましく、また、通常30以下であり、26以下であることが好ましく、22以下であることがより好ましく、20以下であることがさらに好ましい。当該脂肪酸は、置換基を有していてもよく、無置換であってもよい。 The fatty acid ester group (RCOO- group) of polyglycerin fatty acid ester is derived from a fatty acid. The fatty acid is not limited and may be a saturated fatty acid or an unsaturated fatty acid. In addition, from the viewpoint of good flavor and production efficiency, the number of carbon atoms in the fatty acid is usually 10 or more, preferably 12 or more, more preferably 14 or more, and even more preferably 16 or more. Moreover, it is usually 30 or less, preferably 26 or less, more preferably 22 or less, and even more preferably 20 or less. The fatty acid may have a substituent or may be unsubstituted.
 また、ポリグリセリン脂肪酸エステル一分子が有する脂肪酸エステル基の数は、ポリグリセリン脂肪酸エステルが乳化剤としての機能を発揮し得る構造であれば限定されず、グリセリンの重合度およびグリセリン由来の水酸基の数に応じて適宜選択することができる。乳化剤としての機能を発揮し得る構造とは、親油基となる脂肪酸部位および親水基となる多価アルコール部位の両方を有する構造である。具体的には、ポリグリセリン脂肪酸エステル一分子あたりの脂肪酸エステル基の数は、通常1以上であればよい。また、グリセリン由来の水酸基の数は、1以上であればよい。 In addition, the number of fatty acid ester groups that one molecule of polyglycerol fatty acid ester has is not limited as long as the polyglycerol fatty acid ester has a structure that can function as an emulsifier, and depends on the degree of polymerization of glycerin and the number of hydroxyl groups derived from glycerin. It can be selected as appropriate. A structure that can function as an emulsifier is a structure that has both a fatty acid moiety that serves as a lipophilic group and a polyhydric alcohol moiety that serves as a hydrophilic group. Specifically, the number of fatty acid ester groups per molecule of polyglycerin fatty acid ester should normally be one or more. Further, the number of hydroxyl groups derived from glycerin may be one or more.
 ポリグリセリン脂肪酸エステルにおけるグリセリンの重合度、ならびに脂肪酸エステル基の種類および数は、上述したものを任意に組み合わせることができる。より具体的には、ポリグリセリン脂肪酸エステルのアルコール成分は、ジグリセリン、トリグリセリン、テトラグリセリン、ペンタグリセリン、ヘキサグリセリン、ヘプタグリセリン、オクタグリセリン、ノナグリセリン、またはデカグリセリンであってよい。ポリグリセリン脂肪酸エステルの酸成分は、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸、リノール酸、α-リノレン酸等の脂肪酸であってよい。また、ポリグリセリン脂肪酸エステルは、モノエステル、ジエステル、トリエステル、テトラエステル、ペンタエステル等であってよい。ポリグリセリン脂肪酸エステルとして、1種類を単独で用いてもよく、また2種類以上を任意の比率で併用してもよい。 The degree of polymerization of glycerin and the type and number of fatty acid ester groups in the polyglycerin fatty acid ester can be arbitrarily combined as described above. More specifically, the alcohol component of the polyglycerin fatty acid ester may be diglycerin, triglycerin, tetraglycerin, pentaglycerin, hexaglycerin, heptaglycerin, octaglycerin, nonaglycerin, or decaglycerin. The acid component of the polyglycerol fatty acid ester may be a fatty acid such as lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, α-linolenic acid, and the like. Further, the polyglycerin fatty acid ester may be a monoester, diester, triester, tetraester, pentaester, or the like. As the polyglycerol fatty acid ester, one type may be used alone, or two or more types may be used in combination in any ratio.
 ポリグリセリン脂肪酸エステルは、良好な香味および製造時の作業性の観点から、ジグリセリンモノ脂肪酸エステルおよびデカグリセリン脂肪酸エステルから選択される一種以上であることが好ましい。ジグリセリンモノ脂肪酸エステルは、ジグリセリンモノラウレート、ジグリセリンモノミリステート、ジグリセリンモノパルミテート、ジグリセリンモノステアレートおよびジグリセリンモノオレエートからなる群から選択されることが好ましく、ジグリセリンモノオレエートであることがより好ましい。デカグリセリン脂肪酸エステルは、デカグリセリンラウレート、デカグリセリンミリステート、デカグリセリンパルミテート、デカグリセリンステアレートおよびデカグリセリンオレエートからなる群から選択されることが好ましく、デカグリセリンモノラウレート、デカグリセリンモノミリステート、デカグリセリンモノパルミテート、デカグリセリンモノステアレートおよびデカグリセリンモノオレエートからなる群から選択されることがより好ましい。 From the viewpoint of good flavor and workability during production, the polyglycerin fatty acid ester is preferably one or more selected from diglycerin monofatty acid ester and decaglycerin fatty acid ester. The diglycerin monofatty acid ester is preferably selected from the group consisting of diglycerin monolaurate, diglycerin monomyristate, diglycerin monopalmitate, diglycerin monostearate and diglycerin monooleate; More preferred is oleate. The decaglycerin fatty acid ester is preferably selected from the group consisting of decaglycerin laurate, decaglycerin myristate, decaglycerin palmitate, decaglycerin stearate and decaglycerin oleate; More preferably it is selected from the group consisting of myristate, decaglycerin monopalmitate, decaglycerin monostearate and decaglycerin monooleate.
 組成物中のポリグリセリン脂肪酸エステルの含有率(ポリグリセリン脂肪酸エステルを2種類以上含有する場合は、それらの総含有率)は、限定されないが、良好な香味を得る観点および製造効率向上の観点から、通常0.1重量%以上であり、0.2量%以上であることが好ましく、0.3重量%以上であることがより好ましく、0.5重量%以上であることがさらに好ましい。また、前記ポリグリセリン脂肪酸エステルの含有率は、前記組成物に適度な粘性を付与する観点から、通常20.0重量%以下であり、15.0重量%以下であることが好ましく、10.0重量%以下であることがより好ましく、8.0重量%以下であることがさらに好ましい。 The content of polyglycerol fatty acid esters in the composition (if it contains two or more types of polyglycerol fatty acid esters, their total content) is not limited, but from the viewpoint of obtaining good flavor and improving production efficiency. , usually at least 0.1% by weight, preferably at least 0.2% by weight, more preferably at least 0.3% by weight, even more preferably at least 0.5% by weight. Further, the content of the polyglycerol fatty acid ester is usually 20.0% by weight or less, preferably 15.0% by weight or less, and 10.0% by weight or less, preferably 15.0% by weight or less, from the viewpoint of imparting appropriate viscosity to the composition. It is more preferably at most 8.0% by weight, even more preferably at most 8.0% by weight.
 ポリグリセリン脂肪酸エステルのHLB値は、限定されないが、良好な香味を得る観点および製造効率向上の観点から、通常6.0以上、好ましくは7.0以上、また、通常20.0以下、好ましくは18.0以下、より好ましくは16.0以下である。 The HLB value of the polyglycerol fatty acid ester is not limited, but from the viewpoint of obtaining good flavor and improving production efficiency, it is usually 6.0 or more, preferably 7.0 or more, and usually 20.0 or less, preferably It is 18.0 or less, more preferably 16.0 or less.
 6)呈味性成分
 呈味性成分として、塩味、苦味、酸味、うま味などを呈する化合物をさらに含んでもよい。適切な呈味性成分の非限定的な例としては、塩化ナトリウム、塩化カリウム、塩化アンモニウム、ペプチド、クエン酸、アスコルビン酸、グルタミン酸ナトリウム、アルギニン、ジンゲロール、ギムネマ等が挙げられる。配合される呈味成分は味覚受容体のリガンドが好ましい。これらの呈味性成分は口腔内の味覚受容体によって受容されることで、香料等による製品の喫味に呈味効果を付与し、喫味改善や嗜好性の向上に寄与しうる。これら呈味性成分の代表的な量は、組成物中、通常0.5重量%以上、10重量%以下であり、より好ましくは、2重量%以上、8重量%以下であり、さらに好ましくは、3重量%以上、5重量%以下である。
6) Taste component The taste component may further include a compound exhibiting salty, bitter, sour, umami, or the like. Non-limiting examples of suitable flavoring ingredients include sodium chloride, potassium chloride, ammonium chloride, peptides, citric acid, ascorbic acid, sodium glutamate, arginine, gingerol, gymnema, and the like. The taste component to be blended is preferably a ligand for a taste receptor. When these taste components are received by taste receptors in the oral cavity, they can impart a flavor effect to the product's taste due to fragrances, etc., and contribute to improving the taste and palatability of the product. Typical amounts of these taste components in the composition are usually 0.5% by weight or more and 10% by weight or less, more preferably 2% by weight or more and 8% by weight or less, and even more preferably , 3% by weight or more and 5% by weight or less.
(8)組成物の特性
 1)pH
 組成物のpHは限定されないが、味への影響の観点から、通常7.0以上であり、7.5以上であることが好ましく、8.0以上であることがより好ましく、また、通常10.0以下であり、9.5以下であることが好ましく、9.0以下であることがより好ましい。当該pHは25℃における測定値である。
(8) Characteristics of composition 1) pH
The pH of the composition is not limited, but from the viewpoint of influence on taste, it is usually 7.0 or higher, preferably 7.5 or higher, more preferably 8.0 or higher, and usually 10 or higher. .0 or less, preferably 9.5 or less, and more preferably 9.0 or less. The pH is a measured value at 25°C.
 測定温度25℃における組成物のpHは、pH分析計(例えば、堀場製作所製:LAQUA F-72 フラットISFET pH電極)を用い、組成物2gに対して、水20mL投入し10分間振とうし、その上清液を測定することで測定することができる。機器の校正は、例えば、フタル酸pH標準液(pH4.01)、中性リン酸塩pH標準液(pH6.86)、ほう酸塩pH標準液(pH9.18)(いずれも和光純薬工業)を用いた3点校正で行うことが好ましい。 The pH of the composition at a measurement temperature of 25°C is determined using a pH analyzer (for example, LAQUA F-72 flat ISFET pH electrode manufactured by Horiba), and 20 mL of water is added to 2 g of the composition, shaken for 10 minutes, It can be measured by measuring the supernatant liquid. For example, calibrate the equipment using phthalate pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all manufactured by Wako Pure Chemical Industries). It is preferable to perform three-point calibration using
 2)水分の吸脱着等温線
 保存中の水の染み出しやすさは、組成物に対して水分の吸脱着等温線を測定することで評価できる。具体的に、高湿度環境下での水の吸着性能が高い組成物は、保存中に水が染み出しにくく、保存安定性に優れる。この特性に対しては前記基材の寄与が大きいので、前記基材に対し水分の吸脱着等温線を測定することで評価が可能である。水分の吸脱着等温線は以下のように測定される。
2) Moisture adsorption/desorption isotherm The ease with which water oozes out during storage can be evaluated by measuring the moisture adsorption/desorption isotherm of the composition. Specifically, a composition that has high water adsorption performance in a high-humidity environment is less likely to seep out water during storage and has excellent storage stability. Since the base material has a large contribution to this property, it can be evaluated by measuring the moisture adsorption/desorption isotherm of the base material. The moisture adsorption/desorption isotherm is measured as follows.
 水分の吸脱着等温挙動を測定する装置としては公知のものを使用できるが、例えばMicrotracBEL(マイクロトラック・ベル株式会社)のBELSORP MAX IIを用いることができる。前処理として、サンプルを、リークが1Pa/min以下になるまで105℃にて真空乾燥することが好ましい。次いで、相対圧(湿度)が0.025から0.3までは相対圧0.025間隔で、0.3から0.95までは相対圧0.05間隔で吸着等温挙動を測定する。そして相対圧が0.95まで到達した以降は、前記と同じ相対圧の間隔にて、相対圧0.1まで脱着等温挙動を測定し、吸脱着等温線を作成する。平衡化条件は、相対圧0.9以下では300secで圧力変化が0.3%以下、相対圧が0.9以上では300secで圧力値0.3Pa以下の変動になることとする。 As a device for measuring the isothermal behavior of adsorption and desorption of moisture, a known device can be used, and for example, BELSORP MAX II from Microtrac BEL (Microtrac Bell Co., Ltd.) can be used. As a pretreatment, the sample is preferably vacuum-dried at 105° C. until the leakage is 1 Pa/min or less. Next, the adsorption isothermal behavior is measured at relative pressure intervals of 0.025 from 0.025 to 0.3 and at intervals of 0.05 relative pressure from 0.3 to 0.95. After the relative pressure reaches 0.95, the desorption isothermal behavior is measured at the same relative pressure intervals as above until the relative pressure reaches 0.1, and an adsorption/desorption isotherm is created. The equilibration conditions are that when the relative pressure is 0.9 or less, the pressure change is 0.3% or less in 300 seconds, and when the relative pressure is 0.9 or more, the pressure change is 0.3 Pa or less in 300 seconds.
(9)組成物の製造方法
 組成物は、任意の方法で製造されるが、基材、ニコチン、必要に応じて前記の成分を混合する工程を経て製造されることが好ましい。混合は、全原料をミキサーに投入して混合することで実施できる。
(9) Method for producing composition The composition can be produced by any method, but it is preferably produced through a step of mixing the base material, nicotine, and, if necessary, the above-mentioned components. Mixing can be performed by charging all raw materials into a mixer and mixing them.
 好ましい製造方法では、まず、基材、ニコチン、および必要に応じて水およびその他の物質(甘味料、香料、保湿剤等)を混合して第1の混合物を得る。このとき加熱を施してもよい。また、各原料の混合の順序は限定されず、任意の順序または同時にミキサーに投入して混合してもよく、固形の原料を均一に混合した後に液体の原料を添加してさらに混合してもよい。作業性の観点からは、後者の態様が好ましい。 In a preferred manufacturing method, first, the base material, nicotine, and optionally water and other substances (sweeteners, flavors, humectants, etc.) are mixed to obtain a first mixture. At this time, heating may be applied. Furthermore, the order of mixing each raw material is not limited, and they may be mixed in any order or at the same time by being added to the mixer, or solid raw materials may be mixed uniformly, then liquid raw materials may be added and further mixed. good. From the viewpoint of workability, the latter embodiment is preferable.
 上記のとおりに得た混合物に、必要に応じてpH調整剤を含む水溶液、アセスルファムカリウム等の甘味料、メンソール等の香料、大豆レシチン等の苦味抑制剤、グリセリン等の保湿剤を添加(添加剤添加工程)することができる。上記の添加物は、固体で添加してもよいし、水に溶解した水溶液として添加してもよい。水溶液で添加する場合は、口腔用製品の最終水分含量を達成できるように予め所定量の水に溶解して添加してもよい。 To the mixture obtained as above, an aqueous solution containing a pH adjuster, a sweetener such as acesulfame potassium, a flavoring agent such as menthol, a bitterness suppressant such as soybean lecithin, and a humectant such as glycerin are added as necessary (additives addition step). The above additives may be added in solid form or as an aqueous solution dissolved in water. When added in an aqueous solution, it may be added in advance by dissolving it in a predetermined amount of water to achieve the final moisture content of the oral product.
2.口腔用パウチ製品
 口腔用製品は、口中に含んで使用される。口腔用パウチ製品とはシールされた非水溶性包装材(パウチともいう)内に組成物(主材または充填物ともいう)を備え、唾液がパウチを通って浸透しパウチ内に包含された組成物中の成分を溶解し、その後、パウチを通り抜けて口腔中に運び出し得る製品をいう。
2. Oral Pouch Products Oral products are used by being placed in the mouth. Oral pouch products are compositions that contain a composition (also called the main material or filler) within a sealed water-insoluble packaging material (also called a pouch), and saliva penetrates through the pouch and is contained within the pouch. A product that dissolves the ingredients in the product and can then be passed through a pouch and transported into the oral cavity.
(1)パウチ
 パウチは、充填物を包装することができ、水に溶解せず、かつ、液体(水や唾液等)および充填物中の水溶性成分を透過できれば、限定されず公知のものを用いることができる。パウチの材料としては、例えば、セルロース系の不織布等が挙げられ、市販の不織布を用いてもよい。このような材料からなるシートを袋形状に成形し、その中に充填物を充填し、ヒートシール等の手段によりシールすることによりパウチ製品を作製することができる。
(1) Pouch Pouches are not limited to known pouches as long as they can package the filling, do not dissolve in water, and can permeate liquids (water, saliva, etc.) and water-soluble components in the filling. Can be used. Examples of the material for the pouch include cellulose nonwoven fabric, and commercially available nonwoven fabrics may also be used. A pouch product can be produced by forming a sheet made of such a material into a bag shape, filling the bag with a filler, and sealing the bag by means such as heat sealing.
 上記のシートの坪量は、特段制限されず、通常12gsm(g/m)以上、54gsm以下であり、24gsm以上、30gsm以下であることが好ましい。上記のシートの厚さは、特段制限されず、通常100μm以上、300μm以下であり、175μm以上、215μm以下であることが好ましい。 The basis weight of the sheet is not particularly limited, and is usually 12 gsm (g/m 2 ) or more and 54 gsm or less, preferably 24 gsm or more and 30 gsm or less. The thickness of the sheet is not particularly limited, and is usually 100 μm or more and 300 μm or less, preferably 175 μm or more and 215 μm or less.
 パウチの内面および外面の少なくとも一方に部分的に撥水材料が塗布されていてもよい。撥水材料としては撥水性フッ素系樹脂が好適である。具体的には、この種の撥水性フッ素系樹脂としては、旭硝子社製のアサヒガード(登録商標)が挙げられる。撥水性フッ素系樹脂は、例えば、菓子類、乳製品、惣菜、ファストフードやペットフードなどの油脂類を含んだ食品や製品のための包材に塗布されている。それ故、この種の撥水性フッ素系樹脂は、口腔内に置かれるパウチに塗布されても安全である。この撥水材料としてはフッ素系樹脂に限ることなく、例えば、パラフィン樹脂、シリコン系樹脂またはエポキシ系樹脂等の撥水作用を有する材料であってもよい。 At least one of the inner and outer surfaces of the pouch may be partially coated with a water-repellent material. A water-repellent fluororesin is suitable as the water-repellent material. Specifically, this type of water-repellent fluororesin includes Asahi Guard (registered trademark) manufactured by Asahi Glass Co., Ltd. Water-repellent fluororesins are applied to packaging materials for foods and products containing fats and oils, such as confectionery, dairy products, prepared foods, fast food, and pet food. Therefore, this type of water-repellent fluororesin is safe even when applied to pouches placed in the oral cavity. The water-repellent material is not limited to fluororesin, and may be a water-repellent material such as paraffin resin, silicone resin, or epoxy resin.
 パウチは、任意の成分を含んでいてよい。当該成分としては、例えば、香りや味を調節する原料や、香料、添加物、たばこ抽出液、および色素等が挙げられる。また、これらの成分を含有させる態様は限定されず、パウチ表面に塗布したり、しみこませたり、繊維からなる場合には該繊維に含有させる態様等が挙げられる。 The pouch may contain any ingredients. Examples of such components include raw materials that adjust aroma and taste, fragrances, additives, tobacco extracts, and pigments. Furthermore, the manner in which these components are contained is not limited, and examples include methods in which they are applied to the surface of the pouch, impregnated, and in the case of fibers, they are contained in the fibers.
 パウチの外観も限定されない。パウチは、非透明、半透明、または透明であってよい。パウチが半透明または透明であると充填物が透けてみえる。 The appearance of the pouch is also not limited. Pouches may be non-transparent, translucent, or transparent. If the pouch is translucent or transparent, the filling can be seen through.
 口腔用パウチ製品のサイズは限定されない。使用前の製品のサイズは、長辺の下限が25mm以上、28mm以上、35mm以上、または38mm以上であってよい。またその上限は40mm以下であってよい。短辺の下限は10mm以上または14mm以上であってよい。またその上限は、20mm以下または18mm以下であってよい。口腔用パウチ製品の全重量に対する充填物の重量の割合は、限定されないが、通常80重量%以上であり、85重量%以上であることが好ましく、90重量%以上であることがより好ましく、また、通常99重量%以下であり、97重量%以下であることが好ましく、95重量%以下であることがより好ましい。 The size of the oral pouch product is not limited. The size of the product before use may be such that the lower limit of the long side is 25 mm or more, 28 mm or more, 35 mm or more, or 38 mm or more. Moreover, the upper limit may be 40 mm or less. The lower limit of the short side may be 10 mm or more or 14 mm or more. Moreover, the upper limit may be 20 mm or less or 18 mm or less. The ratio of the weight of the filler to the total weight of the oral pouch product is not limited, but is usually 80% by weight or more, preferably 85% by weight or more, more preferably 90% by weight or more, and , usually 99% by weight or less, preferably 97% by weight or less, more preferably 95% by weight or less.
(2)充填物
 口腔用パウチ製品には充填物として前記組成物が充填される。口腔用パウチ製品1個当たりの充填物の量は、好ましくは0.4~1.5gである。
(2) Filler The oral pouch product is filled with the composition as a filler. The amount of filler per oral pouch product is preferably between 0.4 and 1.5 g.
(3)口腔用パウチ製品の製造方法
 組成物を外装材で包装することで口腔用パウチ製品を製造できる(包装工程)。包装する方法は限定されず、公知の方法を適用することができる。例えば、袋形状の不織布に前記組成物を投入した後シールする方法等、公知の方法を用いることができる。包装工程において、シール後に所望のさらに水を加えてもよい(水添加工程)。例えば、最終的な組成物の水の含有率が50重量%であり、充填された組成物の水の含有率が15重量%である場合は、残りの35重量%分の水を添加する。
(3) Method for manufacturing oral pouch products Oral pouch products can be manufactured by packaging the composition with an exterior material (packaging process). The packaging method is not limited, and any known method can be applied. For example, a known method can be used, such as a method in which the composition is poured into a bag-shaped nonwoven fabric and then sealed. In the packaging process, desired additional water may be added after sealing (water addition process). For example, if the final composition has a water content of 50% by weight and the filled composition has a water content of 15% by weight, the remaining 35% by weight of water is added.
 以下に実施態様を記載する。
態様1
 基材として平均粒径が60μm以上である無機多孔質材料と、
 ニコチンと、を含み、
 前記無機多孔質材料における、窒素吸着法で測定しHK法を用いて算出された細孔直径が2nm未満である細孔の細孔容積が0.10cm/g以上である、
口腔用組成物。
態様2
 前記無機多孔質材料が、シリカ、ケイ酸塩、アルミナ、ゼオライト、ヒドロキシアパタイト、ハイドロタルサイト、およびこれらの組合せからなる群から選択される、
態様1に記載の口腔用組成物。
態様3
 前記無機多孔質材料のBET比表面積が200~1200m/gである、
態様1または2に記載の口腔用組成物。
態様4
 前記窒素吸着法で測定し、HK法を用いて算出された細孔直径2nm未満である細孔の細孔容積をV1、
 窒素吸着法で測定し、BJH法を用いて算出された細孔直径2nm以上50nm未満である細孔の細孔容積をV2、
 水銀圧入法で測定された細孔直径50nm以上である細孔の細孔容積をV3とするとき、
 V1/(V1+V2+V3)≧5体積%である、
態様1~3のいずれかに記載の口腔用組成物。
態様5
 水分含有量が10重量%以上である、態様1~4のいずれかに記載の口腔用組成物。
態様6
 前記無機多孔質材料を6重量%以上含む、態様1~5のいずれに記載の口腔用組成物。
態様7
 態様1~6のいずれかに記載の口腔用組成物と、
 前記口腔用組成物を包装する包装材と、
を備える口腔用パウチ製品。
Embodiments are described below.
Aspect 1
an inorganic porous material having an average particle size of 60 μm or more as a base material;
Contains nicotine and
In the inorganic porous material, the pore volume of pores with a pore diameter of less than 2 nm measured by a nitrogen adsorption method and calculated using the HK method is 0.10 cm 3 /g or more,
Oral composition.
Aspect 2
the inorganic porous material is selected from the group consisting of silica, silicate, alumina, zeolite, hydroxyapatite, hydrotalcite, and combinations thereof;
The oral composition according to aspect 1.
Aspect 3
The inorganic porous material has a BET specific surface area of 200 to 1200 m 2 /g.
The oral composition according to aspect 1 or 2.
Aspect 4
The pore volume of pores with a pore diameter of less than 2 nm measured by the nitrogen adsorption method and calculated using the HK method is V1,
The pore volume of pores with a pore diameter of 2 nm or more and less than 50 nm, measured by the nitrogen adsorption method and calculated using the BJH method, is V2,
When the pore volume of pores with a pore diameter of 50 nm or more measured by mercury intrusion method is V3,
V1/(V1+V2+V3)≧5% by volume,
The oral composition according to any one of aspects 1 to 3.
Aspect 5
The oral composition according to any one of aspects 1 to 4, having a water content of 10% by weight or more.
Aspect 6
The oral cavity composition according to any one of aspects 1 to 5, comprising 6% by weight or more of the inorganic porous material.
Aspect 7
The oral composition according to any one of aspects 1 to 6,
A packaging material for packaging the oral composition;
An oral pouch product comprising:
[実施例1]口腔用組成物組成物の製造
 基材としてシリカ(Evonic社製、SIPERNAT2200)100.0g、ニコチン3.87g、無水リン酸ナトリウム水溶液45.1g、無水クエン酸水溶液4.79g、塩化ナトリウム水溶液14.03g、およびアセスルファムK水溶液23.4gを添加し、これらを均一になるまで混合し、混合物Aを得た。得られた混合物Aに、ジャケット加熱(缶壁温度100℃)を行った。その後、周囲温度が20℃となる条件下で30分間冷却し、混合物B(冷却後の水分11%)を得た。冷却後の混合物Bに、リン酸三カリウム水溶液67.7g、リン酸三ナトリウム水溶液28.5g、ジェランガム水溶液20g、および他の成分を添加し、口腔用組成物(含水率41.2重量%、pH8.51)263gを得た。
[Example 1] Production of oral composition As a base material, 100.0 g of silica (manufactured by Evonic, SIPERNAT2200), 3.87 g of nicotine, 45.1 g of anhydrous sodium phosphate aqueous solution, 4.79 g of anhydrous citric acid aqueous solution, 14.03 g of a sodium chloride aqueous solution and 23.4 g of an acesulfame K aqueous solution were added and mixed until homogeneous to obtain a mixture A. The obtained mixture A was subjected to jacket heating (can wall temperature: 100° C.). Thereafter, the mixture was cooled for 30 minutes at an ambient temperature of 20° C. to obtain a mixture B (11% water content after cooling). To the cooled mixture B, 67.7 g of tripotassium phosphate aqueous solution, 28.5 g of trisodium phosphate aqueous solution, 20 g of gellan gum aqueous solution, and other components were added to form an oral composition (water content 41.2% by weight, 263 g of pH 8.51) were obtained.
[実施例2]
 粉末セルロース(レッテンマイヤー社製、VITACEL L00)36.0gと前記シリカ66.0gを混合し基材として用いた以外は、実施例1と同じ方法で口腔用組成物を製造した。
[Example 2]
An oral composition was produced in the same manner as in Example 1, except that 36.0 g of powdered cellulose (VITACEL L00, manufactured by Rettenmeyer) and 66.0 g of the silica were mixed and used as a base material.
[実施例3]
 粉末セルロース(レッテンマイヤー社製、VITACEL L00)40.0gと前記シリカ60.0gを混合し基材として用いた以外は、実施例1と同じ方法で口腔用組成物を製造した。
[Example 3]
An oral composition was produced in the same manner as in Example 1, except that 40.0 g of powdered cellulose (VITACEL L00, manufactured by Rettenmeyer) and 60.0 g of the silica were mixed and used as a base material.
[実施例4]
 粉末セルロース(レッテンマイヤー社製、VITACEL L00)30.0gと前記シリカ70.0gを混合し基材として用いた以外は、実施例1と同じ方法で口腔用組成物を製造した。
[Example 4]
An oral composition was produced in the same manner as in Example 1, except that 30.0 g of powdered cellulose (VITACEL L00, manufactured by Rettenmeyer) and 70.0 g of the silica were mixed and used as a base material.
[比較例1]
 基材として微結晶セルロース(レッテンマイヤー社製、VIVAPUR200)100.0gを用いた以外は、実施例1と同じ方法で口腔用組成物を製造した。表1に組成を、表2に基材の物性を示した。
[Comparative example 1]
An oral composition was produced in the same manner as in Example 1, except that 100.0 g of microcrystalline cellulose (VIVAPUR200, manufactured by Rettenmeyer) was used as the base material. Table 1 shows the composition, and Table 2 shows the physical properties of the base material.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
 
Figure JPOXMLDOC01-appb-T000002
 
 図1に各材料の水分の吸脱着等温線を示した。実施例で用いたシリカは、セルロース系基材と比べ、特に高湿度環境下での水の吸着性能が高く、保管環境による製品の変性が起こりづらい、すなわち水の染み出しが低減されるといえる。 Figure 1 shows the moisture adsorption/desorption isotherms of each material. The silica used in the examples has a higher ability to adsorb water, especially in high-humidity environments, than cellulose-based base materials, and it can be said that the product is less likely to be denatured by the storage environment, that is, water seepage is reduced. .
 各種測定は以下のとおり実施した。
<平均粒径>
 各材料の平均粒径は、レーザー回折粒度分布測定により求めた粒度分布における体積基準累積50%での粒径(D50)を意味する。レーザー回折粒度分布測定には、マスターサイザー3000(マルバーン・パナリティカル社製)を用いて測定した。
Various measurements were carried out as follows.
<Average particle size>
The average particle size of each material means the particle size (D50) at 50% cumulative volume based on the particle size distribution determined by laser diffraction particle size distribution measurement. Laser diffraction particle size distribution was measured using Mastersizer 3000 (manufactured by Malvern Panalytical).
<水分量>
 加熱乾燥式水分計(METTER TOLEDO社製:HB 43-S)を用いて測定した。測定に際し、試料を所定容器に投入し到達温度100℃まで加熱した。測定は60秒間で1mg以下の変化量となった時点で終了し、加熱前後の秤量値より含水率を算出した。
<Water content>
It was measured using a heat drying moisture meter (METTER TOLEDO: HB 43-S). At the time of measurement, the sample was placed in a predetermined container and heated to an ultimate temperature of 100°C. The measurement was terminated when the amount of change became 1 mg or less in 60 seconds, and the water content was calculated from the weighed values before and after heating.
<窒素吸着法によるマイクロ孔解析>
 以下の条件で前処理を行った。
 シリカ:250℃、2時間加熱
 セルロース:105℃、1時間加熱
 次いで、窒素吸着等温線を得て、HK法によって、マイクロ孔容積を求めた。
 測定装置は、ガス吸着量測定装置AutoSorb-1(Quantachrome社製)を用いて取得した。
<Micropore analysis using nitrogen adsorption method>
Pretreatment was performed under the following conditions.
Silica: Heated at 250°C for 2 hours Cellulose: Heated at 105°C for 1 hour Next, a nitrogen adsorption isotherm was obtained and the micropore volume was determined by the HK method.
The measurement was performed using a gas adsorption amount measuring device AutoSorb-1 (manufactured by Quantachrome).
<pH>
 pH分析計(堀場製作所製:LAQUA F-72 フラットISFET pH電極)を用い、組成物2gに対して、水20ml投入し10分間振とう、その上清液を測定した。機器の校正は、例えば、フタル酸pH標準液(pH4.01)、中性リン酸塩pH標準液(pH6.86)、ほう酸塩pH標準液(pH9.18)(いずれも和光純薬工業)を用いた3点校正で行った。
<pH>
Using a pH analyzer (manufactured by Horiba, Ltd.: LAQUA F-72 flat ISFET pH electrode), 20 ml of water was added to 2 g of the composition, shaken for 10 minutes, and the supernatant liquid was measured. For example, calibrate the equipment using phthalate pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all manufactured by Wako Pure Chemical Industries). This was done using a three-point calibration.
<水分の吸脱着等温線>
 測定装置:MicrotracBEL(マイクロトラック・ベル株式会社)のBELSORP MAX IIを用いた。前処理として、サンプルを、リークが1Pa/min以下になるまで105℃にて真空乾燥した。測定条件は、相対圧(湿度)が0.025から0.3までは相対圧0.025間隔で、0.3から0.95までは相対圧0.05間隔で吸着等温線を測定し、相対圧0.95まで到達すると、同じ相対圧の間隔にて相対圧0.1まで脱着等温線を測定した。(TSPは測定時間が長く測定精度か低下するため相対圧訳0.5までとした。)平衡化条件は、相対圧0.9以下では300secで圧力変化が0.3%以下、相対圧が0.9以上では300secで圧力値0.3Pa以下の変動になることとした。
 
<Moisture adsorption/desorption isotherm>
Measuring device: BELSORP MAX II from MicrotracBEL (Microtrac Bell Co., Ltd.) was used. As a pretreatment, the sample was vacuum dried at 105° C. until the leakage was 1 Pa/min or less. The measurement conditions are: from relative pressure (humidity) from 0.025 to 0.3, adsorption isotherms are measured at relative pressure intervals of 0.025; from 0.3 to 0.95, adsorption isotherms are measured at relative pressure intervals of 0.05; Once a relative pressure of 0.95 was reached, the desorption isotherm was measured at the same relative pressure interval up to a relative pressure of 0.1. (For TSP, the measurement time is long and the measurement accuracy is reduced, so the relative pressure translation was limited to 0.5.) The equilibration conditions were that when the relative pressure was 0.9 or less, the pressure change was 0.3% or less in 300 seconds, and when the relative pressure was If the pressure is 0.9 or more, the pressure value will fluctuate to 0.3 Pa or less in 300 seconds.

Claims (7)

  1.  基材として平均粒径が60μm以上である無機多孔質材料と、
     ニコチンと、を含み、
     前記無機多孔質材料における、窒素吸着法で測定しHK法を用いて算出された細孔直径が2nm未満である細孔の細孔容積が0.10cm/g以上である、
    口腔用組成物。
    an inorganic porous material having an average particle size of 60 μm or more as a base material;
    Contains nicotine and
    In the inorganic porous material, the pore volume of pores with a pore diameter of less than 2 nm measured by a nitrogen adsorption method and calculated using the HK method is 0.10 cm 3 /g or more,
    Oral composition.
  2.  前記無機多孔質材料が、シリカ、ケイ酸塩、アルミナ、ゼオライト、ヒドロキシアパタイト、ハイドロタルサイト、およびこれらの組合せからなる群から選択される、
    請求項1に記載の口腔用組成物。
    the inorganic porous material is selected from the group consisting of silica, silicate, alumina, zeolite, hydroxyapatite, hydrotalcite, and combinations thereof;
    The oral composition according to claim 1.
  3.  前記無機多孔質材料のBET比表面積が200~1200m/gである、
    請求項1または2に記載の口腔用組成物。
    The inorganic porous material has a BET specific surface area of 200 to 1200 m 2 /g.
    The oral composition according to claim 1 or 2.
  4.  前記窒素吸着法で測定し、HK法を用いて算出された細孔直径2nm未満である細孔の細孔容積をV1、
     窒素吸着法で測定し、BJH法を用いて算出された細孔直径2nm以上50nm未満である細孔の細孔容積をV2、
     水銀圧入法で測定された細孔直径50nm以上である細孔の細孔容積をV3とするとき、
     V1/(V1+V2+V3)≧5体積%である、
    請求項1~3のいずれかに記載の口腔用組成物。
    The pore volume of pores with a pore diameter of less than 2 nm measured by the nitrogen adsorption method and calculated using the HK method is V1,
    The pore volume of pores with a pore diameter of 2 nm or more and less than 50 nm, measured by the nitrogen adsorption method and calculated using the BJH method, is V2,
    When the pore volume of pores with a pore diameter of 50 nm or more measured by mercury intrusion method is V3,
    V1/(V1+V2+V3)≧5% by volume,
    The oral composition according to any one of claims 1 to 3.
  5.  水の含有率が10重量%以上である、請求項1~4のいずれかに記載の口腔用組成物。 The oral composition according to any one of claims 1 to 4, wherein the water content is 10% by weight or more.
  6.  前記無機多孔質材料を6重量%以上含む、請求項1~5のいずれに記載の口腔用組成物。 The oral cavity composition according to any one of claims 1 to 5, comprising 6% by weight or more of the inorganic porous material.
  7.  請求項1~6のいずれかに記載の口腔用組成物と、
     前記口腔用組成物を包装する包装材と、
    を備える口腔用パウチ製品。
     
    The oral composition according to any one of claims 1 to 6,
    A packaging material for packaging the oral composition;
    An oral pouch product comprising:
PCT/JP2023/016876 2022-04-28 2023-04-28 Oral composition containing inorganic porous material WO2023210814A1 (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011529842A (en) * 2008-08-01 2011-12-15 エボニック デグサ ゲーエムベーハー A new class of precipitated silica for support applications.
WO2014159403A1 (en) * 2013-03-14 2014-10-02 Altria Client Services Inc. Smokeless tobacco article
JP2014237700A (en) * 2007-04-11 2014-12-18 ファーマシューティカル プロダクションズ, インコーポレイテッド Melatonin tablet and methods of preparation and use
WO2016014454A1 (en) * 2014-07-21 2016-01-28 Pharmaceutical Productions, Inc. Solid dosage form composition for buccal or sublingual administration of cannabinoids
JP2019512219A (en) * 2016-03-07 2019-05-16 ブリティッシュ アメリカン タバコ (インヴェストメンツ) リミテッドBritish American Tobacco (Investments) Limited Smokeless oral tobacco products and their preparation
US20190246686A1 (en) * 2018-02-15 2019-08-15 Altria Client Services Llc Alternative Nicotine Carriers for Solid Products
WO2021116866A1 (en) * 2019-12-09 2021-06-17 Nicoventures Trading Limited Pouched products with enhanced flavor stability

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014237700A (en) * 2007-04-11 2014-12-18 ファーマシューティカル プロダクションズ, インコーポレイテッド Melatonin tablet and methods of preparation and use
JP2011529842A (en) * 2008-08-01 2011-12-15 エボニック デグサ ゲーエムベーハー A new class of precipitated silica for support applications.
WO2014159403A1 (en) * 2013-03-14 2014-10-02 Altria Client Services Inc. Smokeless tobacco article
WO2016014454A1 (en) * 2014-07-21 2016-01-28 Pharmaceutical Productions, Inc. Solid dosage form composition for buccal or sublingual administration of cannabinoids
JP2019512219A (en) * 2016-03-07 2019-05-16 ブリティッシュ アメリカン タバコ (インヴェストメンツ) リミテッドBritish American Tobacco (Investments) Limited Smokeless oral tobacco products and their preparation
US20190246686A1 (en) * 2018-02-15 2019-08-15 Altria Client Services Llc Alternative Nicotine Carriers for Solid Products
WO2021116866A1 (en) * 2019-12-09 2021-06-17 Nicoventures Trading Limited Pouched products with enhanced flavor stability

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