WO2021220898A1 - Nicotine supply oral pouch product and production method therefor - Google Patents

Nicotine supply oral pouch product and production method therefor Download PDF

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Publication number
WO2021220898A1
WO2021220898A1 PCT/JP2021/016101 JP2021016101W WO2021220898A1 WO 2021220898 A1 WO2021220898 A1 WO 2021220898A1 JP 2021016101 W JP2021016101 W JP 2021016101W WO 2021220898 A1 WO2021220898 A1 WO 2021220898A1
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WIPO (PCT)
Prior art keywords
composition
nicotine
weight
water
supplied
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Application number
PCT/JP2021/016101
Other languages
French (fr)
Japanese (ja)
Inventor
雅之 古越
賢 住田
淳 桑原
正人 宮内
道徳 横井
圭祐 戸渡
敦 永井
慶 小林
真里那 八川
Original Assignee
日本たばこ産業株式会社
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Application filed by 日本たばこ産業株式会社 filed Critical 日本たばこ産業株式会社
Priority to EP21796154.9A priority Critical patent/EP4144231A1/en
Publication of WO2021220898A1 publication Critical patent/WO2021220898A1/en

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    • 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
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303Plant extracts other than tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/42Treatment of tobacco products or tobacco substitutes by chemical substances by organic and inorganic substances

Definitions

  • the present invention relates to a nicotine-supplied oral pouch product and a method for producing the same.
  • a nicotine-supplied oral pouch product such as an oral tobacco product is a package in which a composition containing nicotine is stored in a pouch (packaging material) formed of a material such as a non-woven fabric. Put it inside and use it.
  • a composition containing nicotine is stored in a pouch (packaging material) formed of a material such as a non-woven fabric. Put it inside and use it.
  • components such as nicotine in the composition exude to the outside of the packaging material, and the flavor component is delivered to the user.
  • Patent Documents In the nicotine-supplied oral pouch product, the feeling of use in the oral cavity at the time of use is important, and the technology for improving the mouthfeel and the technology for improving the familiarity between the product and saliva are known. For example, by reducing the sealing area and the amount of excess air in the product, it is possible to release the desired flavor during use, and the development of a technique for improving the palatability in the oral cavity (Patent Documents). 1) In addition, the development of technology that improves the compatibility between the product and saliva by containing a specific substance in the composition and promotes the rapid transmucosal transmission of the substance in the composition in the oral cavity is progressing. (Patent Document 2).
  • the present inventors have focused on the fluidity of the composition in the pouch during use and the adhesion between the materials constituting the composition.
  • the pouch product can be easily deformed in the direction perpendicular to the direction in which the pressure is applied to the pouch product, so that the user can easily shape the pouch product into a desired shape. It can be deformed and held in the oral cavity.
  • the pouch product can be easily deformed in the direction in which pressure is applied to the pouch product, so that the user can easily make an initial pouch product having a large thickness. It can be deformed thinly.
  • the above-mentioned improvement in fluidity is an improvement in usability between the time when the user puts the pouch product in the mouth and the saliva soaks into the mouth and the time when the user finishes using the product and takes it out of the mouth.
  • Patent Documents 1 and 2 do not disclose any of these characteristics.
  • the present inventors can solve the above problems by using a composition containing gel particles containing a specific substance and setting the water content in the composition to a specific value or more. And arrived at the present invention.
  • a nicotine-supplied oral pouch product comprising a composition containing gel particles and a pouch for packaging the composition.
  • the gel particles contain at least anionic natural polymer carbohydrates, calcium ions, and water.
  • the composition comprises nicotine The content of water in the composition is 15% by weight or more. Nicotine-supplied oral pouch products.
  • the anionic natural polymer carbohydrate is LM pectin.
  • the composition contains nicotine and A method for producing a nicotine-supplied oral pouch product, wherein the content of water in the composition is 15% by weight or more.
  • the nicotine-supplied oral pouch product according to the embodiment of the present invention is a nicotine-supplied oral pouch product having a composition containing gel particles and a pouch for packaging the composition.
  • the gel particles contain at least anionic natural polymer carbohydrates, calcium ions, and water.
  • the composition comprises nicotine The content of water in the composition is 15% by weight or more. It is a nicotine-supplied oral pouch product.
  • the composition in the pouch contains gel particles, and the gel particles have a structure in which at least anionic natural polymer carbohydrates are crosslinked with calcium ions and swollen with a dispersion medium containing water.
  • the content of water in the composition is 15% by weight or more, so that the fluidity and / or adhesiveness of the composition can be improved.
  • the fluidity and / and adhesion of anionic natural polymer carbohydrates that swell with water can be improved.
  • composition The composition of the composition is not particularly limited as long as it contains at least anionic natural polymer carbohydrates, calcium ions, and gel particles containing water, and nicotine.
  • the composition in the present invention is a general term for any substance contained in a pouch. Further, from the viewpoint of preventing the composition from leaking to the outside of the pouch, the composition is preferably not a liquid, and for example, it is preferably composed of only gel-like gel particles or a gel-like particles and a solid substance. Further, in order to satisfy the preferred embodiment of the particle size described later, it is preferable that the particles have a particle shape (plurality of particles) after drying.
  • Oral pouch products have compositions that include gel particles.
  • the gel particles contained in the composition are not particularly limited as long as they are particulate gels.
  • the term "particulate” means small particles, which do not have to be on a perfect sphere, and specifically, on a sphere, an ellipsoid, a rod, a plate, or in appearance. Includes similar shapes.
  • the “gel-like” refers to a state in which a sol-like decomposition product having fluidity is solidified and loses spontaneous fluidity while maintaining elasticity, and in such a state. A substance is called a "gel", and a substance consisting of a gel is called a "gel substance”.
  • the content of the gel particles in the composition is not particularly limited, but is usually 0.01% by weight or more, preferably 0.05% by weight or more, and more preferably 0.1% by weight or more. , 1.0% by weight or more, and usually 50.0% by weight or less, preferably 20.0% by weight or less, and more preferably 10.0% by weight or less. , 5.0% by weight or less, more preferably.
  • the gel particles are not particularly limited as long as they contain at least anionic natural polymer carbohydrates, calcium ions, and water.
  • the anionic natural polymer carbohydrate is a gelling agent, the type of which is not particularly limited, but a polysaccharide having a carboxyl group is preferable, for example, carrageenan, pectin, arabic gum, xanthan (xanthan gum), gellan (gellan gum), tragant gum, etc.
  • Alginic acid is preferable, and carrageenan, pectin, gellan gum, and alginic acid are preferable from the viewpoint that they are easily gelled in the presence of calcium ions and a junction zone can be formed by a carboxyl group and a cation to form a crosslinked structure. .. Among these, LM pectin is preferable for the reason described later.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • Pectin is a polysaccharide having galacturonic acid and galacturonic acid methyl ester as constituent units and ⁇ 1,4-bonded to them. In addition to galacturonic acid, it is known to contain several diverse sugars. Generally, pectin is classified into LM pectin having a degree of esterification of less than 50% and HM pectin having a degree of esterification of 50% or more. As described above, LM pectin is preferable in this embodiment. In particular, pectin gels in the presence of divalent cations such as calcium ions, and the carboxyl group of galacturonic acid in pectin and cations form a junction zone to form a gel.
  • divalent cations such as calcium ions
  • Pectin having a large number of junction zones that is, a pectin having a low degree of esterification, has a stronger gelling property.
  • the degree of esterification of pectin is preferably 20% or less, more preferably 12% or less, further preferably 10% or less, and it is not necessary to set a lower limit of the degree of esterification. , Usually 6% or more.
  • Gellan gum is known as a water-soluble polysaccharide synthesized by one of the eubacteria, Pseudomonas elodea. When cations are added to the aqueous solution, they are electrically neutralized and the water solubility of gellan gum decreases, resulting in gelation.
  • Gellan gum is a polymeric compound in which repeating units consisting of two D-glucose residues, one L-rhamnose residue and one D-glucuronic acid tetrasaccharide are linearly linked. The repeating structure of tetrasaccharides is as follows. [D-Glc ( ⁇ 1 ⁇ 4) D-GlcA ( ⁇ 1 ⁇ 4) D-Glc ( ⁇ 1 ⁇ 4) L-Rha ( ⁇ 1 ⁇ 3)] n
  • Carrageenan is a kind of linear sulfur-containing polysaccharide and is an anionic polymer compound composed of D-galactose (or 3,6-anhydro-D-galactose) and sulfuric acid.
  • Alginic acid is a type of polysaccharide mainly contained in brown algae. It has a structure in which ⁇ -L-gluuronic acid and ⁇ -D-mannuronic acid are pyranose-type and bound by a 1,4-glycosidic bond (CAS 9005-38-3). It has the property of gelling when cations are added.
  • Gum arabic is also called “gum arabic” or “resin arabic” and dries the secretions from the wounds of the bark of the legumes, Albizia subfamily, Acacia, or related plants of the same genus. It is a thing.
  • the main component is a polysaccharide (polyuronic acid), which is a mixture of arabinogalactan (75-94%), arabinogalactan-protein (5-20%), and glycoprotein (1-5%).
  • the structure of the polysaccharide has galactose in the main chain and galactose, arabinose, rhamnose, and glucuronic acid in the side chain. It is usually a calcium salt, unlike hemicellulose, which constitutes the cell wall, in that the carboxyl group is free.
  • Xanthan is a type of polysaccharide and is generally produced by fermenting corn sugar starch with bacteria. It has a repeating structure with two glucose molecules, two mannose molecules, and a glucuronic acid molecule as units (CAS 11138-66-2).
  • Tragant gum is a thickening polysaccharide obtained by drying the secretion of Tragant, a legume, and is a complex polysaccharide mixture consisting of arabinose, xylose, fucose, galactose, galacturonic acid, and the like.
  • the main components are two types of polysaccharides, acidic and neutral, but include starch, cellulose, minerals and the like.
  • the weight average molecular weight (Mw) of the anionic natural polymer carbohydrate measured by GPC (Gel Permeation Chromatography) and converted by the calibration curve of standard polystyrene may be, for example, 100,000 g / mol or more and 700,000 g / mol or less. , 140,000 g / mol or more and 300,000 g / mol or less, and is not limited to these ranges, as long as the minimum molecular weight at which gelation is achieved is guaranteed.
  • the weight average molecular weight can be increased by the addition of a divalent cation and can be decreased by the addition of an alkali.
  • the content of the anionic natural polymer carbohydrate in the composition is not particularly limited, but is usually 0.01% by weight or more, preferably 0.1% by weight or more, and preferably 1.0% by weight or more. More preferably, it is more preferably 2.0% by weight or more, and usually it is 50.0% by weight or less, preferably 20% by weight or less, and more preferably 10% by weight or less. It is more preferably 0% by weight or less.
  • the content of anionic natural polymer carbohydrates in the composition can be measured by various fraction separation methods and detection methods such as liquid chromatography and liquid chromatography mass spectrometer.
  • Calcium ion is a gelling auxiliary component, and its source (gelling auxiliary agent) is not particularly limited, but for example, calcium halide (chloride, etc.), citric acid, carbonate, sulfate, phosphorus. Examples thereof include acid salts and lactates, and among these, calcium lactate, calcium carbonate, and calcium phosphate are preferable from the viewpoint of less influence of taste on pouch products, high solubility, and pH after dissolution, and in particular, Calcium lactate is preferred.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the content of calcium ions in the composition is not particularly limited, but from the viewpoint of ensuring good fluidity and adhesiveness, the molar ratio to the weight of the composition is usually 0.00023 mol / kg or more, and 0. It is preferably 0023mol / kg or more, more preferably 0.023 mol / kg or more, further preferably 0.046 mol / kg or more, and usually 1.15 mol / kg or less, 0. It is preferably 46 mol / kg or less, more preferably 0.23 mol / kg or less, and even more preferably 0.11 mol / kg or less.
  • the content of calcium ions in the composition can usually be measured by atomic absorption spectrometry.
  • the anionic natural polymer carbohydrate constituting the above-mentioned gelling agent tends to gel in the presence of divalent cations, and the junction zone is formed by the carboxyl group and the cations. To form a gel. If a junction zone is present in the gel, the composition containing the gel will have a network structure. It is desirable that a compound containing a carboxyl group and a divalent cation which is a gelation promoting component is efficiently gelled, and both are present in a number ratio of 2: 1.
  • the ratio of the total number of carboxyl groups of the anionic natural polymer carbohydrate to the total number of calcium ions is preferably 100: 1 to 2: 1, 50: 1 to 2: 1, 10: 1 to 2: 1. The range.
  • the composition may contain a gelling auxiliary component other than calcium ions, for example, magnesium, silver, zinc, copper, gold, aluminum, etc., to which a gelling agent can be bonded by an ionic bond like calcium ions.
  • a gelling auxiliary component other than calcium ions for example, magnesium, silver, zinc, copper, gold, aluminum, etc., to which a gelling agent can be bonded by an ionic bond like calcium ions.
  • Metal ions, cationic polymer ions, etc., and examples of these sources (other gelling aids) include halides (chlorides, etc.), citric acid, and carbonic acid of these metal ions. Examples thereof include salts, sulfates, phosphates and cationic polymers. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the type of water contained in the composition is not particularly limited.
  • the water content (moisture content) in the composition is 15% by weight or more. If the water content is less than 15% by weight, the texture becomes rough and the composition becomes difficult to produce. Further, from the viewpoint of ensuring good fluidity and adhesiveness of the composition and easiness of producing the composition, it is preferably 30% by weight or more, more preferably 45% by weight or more, and usually. It is 55% by weight or less, and preferably 50% by weight or less.
  • the water content can be adjusted by adjusting the amount of water to be added, or by providing a heat treatment or a drying treatment at the production stage.
  • the water content (moisture content) of the above composition is measured using a heat-drying moisture meter (for example, manufactured by METTER TOLEDO: HB 43-S). At the time of measurement, the sample is put into a predetermined container and heated to an ultimate temperature of 100 ° C. The measurement is completed when the amount of change is 1 mg or less in 60 seconds, and the water content is calculated from the weighed values before and after heating.
  • the method for measuring the water content in the present specification is similarly applied to the measurement of the water content of a mixture other than the composition, for example, in the method for producing a composition described later.
  • the composition contains nicotine, but the mode containing nicotine is not particularly limited.
  • nicotine as a compound may be contained, and a nicotine salt or stabilized nicotine (for example, nicotine adsorbed on an ion exchange resin) may be contained.
  • tobacco leaves may be added as a nicotine source, or a nicotine-containing extract obtained by extracting a nicotine-containing substance such as tobacco leaves may be contained. good.
  • the mode in which nicotine is contained is not particularly limited, and the above compound, nicotine source, and extract may be contained in the gel particles, or may be contained in the composition separately from the gel particles.
  • the addition of a nicotine-containing compound is preferable from the viewpoint of accurate supply of nicotine and ease of handling.
  • the color of the composition or pouch product tends to be the color of the tobacco leaf, whereas when a colorless nicotine-containing compound is used, a white composition or pouch product is provided. It becomes possible to do. For users who prefer white pouch products, such an embodiment is an advantage.
  • One aspect may be applied alone, or two or more aspects may be applied in combination.
  • the content of nicotine in the composition is not particularly limited, but is usually 0.1% by weight or more and usually 6.7% by weight or less from the viewpoint of user preference.
  • the above content is the content as a nicotine ion.
  • the content of nicotine in the composition can be measured with a gas chromatography-mass spectrometer (GC-MS).
  • the composition may contain substances other than the above-mentioned anionic natural polymer carbohydrates, calcium ions, other gelling aids, water and nicotine (also referred to as "other substances"), and the other substances may contain. It may be contained in the gel particles, or may be contained in the composition separately from the gel particles. Examples of other substances include base materials, flavors, pH adjusters, sweeteners, moisturizers, bitterness suppressants, whitening agents, emulsifiers and the like. The content of other substances in the composition is not particularly limited, and the composition can be appropriately adjusted according to the product design.
  • the type of the base material is not particularly limited, and examples thereof include cellulose, microcrystalline cellulose, spherical cellulose, and porous cellulose, and cellulose is preferable from the viewpoint of the degree of freedom in adjusting the bulk density of the composition.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the content of the base material in the composition is not particularly limited, but is usually 24% by weight or more and 27% by weight or more from the viewpoint of quality improvement of suppressing elution of water during production or product storage.
  • the types of flavors are not particularly limited, for example, menthol, leaf tobacco extract, natural vegetable flavors (eg, cinnamon, sage, herbs, chamomile, kudzu, sweet tea, cloves, lavender, cardamon, chowji, nutmeg, bergamot, etc. Geranium, Honey Essence, Rose Oil, Lemon, Orange, Kay Skin, Caraway, Jasmine, Ginger, Coriander, Vanilla Extract, Spare Mint, Peppermint, Cassia, Coffee, Cellory, Cascarilla, Sandalwood, Cocoa, Iran Iran, Fennell, Anis , Licoris, St.
  • natural vegetable flavors eg, cinnamon, sage, herbs, chamomile, kudzu, sweet tea, cloves, lavender, cardamon, chowji, nutmeg, bergamot, etc.
  • Geranium Honey Essence, Rose Oil, Lemon, Orange, Kay Skin, Caraway, Jasmine, Ginger, Coriander, Vanilla Extract, Spare Mint, Peppermin
  • the content of the gel particles in the composition is not particularly limited, but from the viewpoint of enjoying the desired taste and aroma, it is usually 0.1% by weight or more, preferably 1% by weight or more, and 2% by weight. % Or more, and usually 20% by weight or less, preferably 15% by weight or less, and more preferably 10% by weight or less.
  • the type of pH adjuster is not particularly limited, and examples thereof include sodium carbonate, sodium hydrogencarbonate, potassium carbonate, potassium hydrogencarbonate, anhydrous sodium phosphate, sodium dihydrogen phosphate, sodium citrate, and the like.
  • Sodium carbonate, potassium carbonate, and sodium dihydrogen phosphate are preferable from the viewpoint of the influence on the taste.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the type of sweetener is not particularly limited, and examples thereof include sugar alcohols such as xylitol, maltitol, and erythritol, and sweeteners such as acesulfame potassium, sucralose, and aspartame.
  • Sugar alcohols are preferable from the viewpoint of adjusting the taste. ..
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the bitterness inhibitor is not particularly limited, and examples thereof include soybean lecithin.
  • Soybean lecithin is a phospholipid, and examples thereof include phosphatidylcholine, phosphatidylethanolamine, and phosphatidylic acid.
  • phosphatidylcholine phosphatidylcholine
  • phosphatidylethanolamine phosphatidylic acid.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the type of moisturizer is not particularly limited, and examples thereof include glycerin and propylene glycol, and glycerin is preferable from the viewpoint of product storage stability.
  • glycerin is preferable from the viewpoint of product storage stability.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the type of whitening agent is not particularly limited, and examples thereof include silicon dioxide, titanium dioxide, and calcium carbonate. Silicon dioxide is preferable from the viewpoint of the influence of taste on the product.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the type of emulsifier is not particularly limited, and examples thereof 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, and polyglycerin fatty acid ester and lecithin.
  • sucrose fatty acid ester include sucrose palmitic acid ester and sucrose stearic acid ester.
  • Examples of the organic acid glycerin fatty acid ester include succinate glycerin fatty acid ester and diacetyl tartrate glycerin fatty acid ester.
  • polyglycerin fatty acid ester examples include diglycerin fatty acid ester, triglycerin fatty acid ester, and decaglycerin fatty acid ester.
  • diglycerin fatty acid ester examples include diglycerin fatty acid ester, triglycerin fatty acid ester, and decaglycerin fatty acid ester.
  • One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
  • the content rate of each of the above components can also be calculated from the amount of raw materials charged.
  • the pH of the composition at a measurement temperature of 22 ° C. is not particularly limited, but is usually 6.0 or more, preferably 7.0 or more, and preferably 8.0 or more from the viewpoint of affecting the taste of the product. It is more preferable, and it is usually 10.0 or less, preferably 9.0 or less.
  • the pH can be adjusted by controlling the amount of the pH adjuster added.
  • the pH value in the present specification is a value measured at a measurement temperature of 22 ° C.
  • a pH analyzer for example, manufactured by HORIBA, Ltd .: LAQUA F-72 flat ISFET pH electrode
  • add 20 ml of water to 2 g of the composition and shake for 10 minutes.
  • equipment calibration for example, phthalic acid pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all by Wako Pure Chemical Industries, Ltd.) Perform a 3-point calibration using.
  • the fluidity of the composition is represented by the shear stress at a normal stress of 5 kPa at a measurement temperature of 22 ° C.
  • the pressure applied to the pouch product is usually 3 to 7 kPa, and therefore 5 kPa.
  • the shear stress is usually 5.99 kPa or less, preferably 5.93 kPa or less, and usually 5.02 kPa or more, 5.13 kPa or more, from the viewpoint of improving fluidity and / or adhesion.
  • shear stress can be increased / decreased by the combination of anionic natural polysaccharide (pectin) and Ca ion.
  • the shear stress of the composition at a normal stress of 5 kPa can be measured using a rheometer.
  • a rheometer For example, when a powder rheometer FT4 manufactured by Freeman Technology Co., Ltd. is used as a rheometer, measurement is performed under the following measurement conditions.
  • -Measurement mode standard program (25 mm_shear_9 kPa) ⁇ Measurement temperature: 22 ° C -Measured humidity: 60% RH -Measuring container: Cylindrical container with an inner diameter of 25 mm, volume 10 ml ⁇ Vertical load: 3-9kPa Each of the measurement raw materials is sieved (1.18 mm mesh opening), and the finely uniform particles are used as a measurement sample, and the measurement is performed according to the procedure of the rheometer.
  • the adhesiveness of the composition is represented by the shear stress at a normal stress of 0 kPa at a measurement temperature of 22 ° C.
  • the normal stress of 0 kPa assumes the pressure at which the pouch product is crushed in the thickness direction after the user puts the pouch product in the mouth and before saliva soaks in, that is, no pressure is applied other than this thickness direction. It is a numerical value.
  • the shear stress is usually 1.83 kPa or less, preferably 1.78 kPa or less, and usually 0.88 kPa or more, 1.12 kPa or more, from the viewpoint of improving fluidity and / or adhesion. It is preferably 1.26 kPa or more, and more preferably 1.26 kPa or more.
  • the shear rate can be increased / decreased by the combination of anionic natural polysaccharide (pectin) and Ca ion.
  • the shear stress of the composition at normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa is measured, and the vertical stress is plotted on the horizontal axis and the shear stress is plotted on the vertical axis to create a graph. do. Since the shear stress changes linearly with respect to the normal stress, the fitting of this graph is performed, and the shear stress at a normal stress of 0 kPa is calculated from the fitting result. The fitting conditions are shown below. A linear regression line is calculated from each value of the shear stress for each normal stress (3 kPa, 4 kPa, 5 kPa, 6 kPa, 7 kPa). Calculate the slope and the value of the Y-intercept. The calculated value of the Y-intercept is taken as the shear stress at a normal stress of 0 kPa.
  • Flow Function In the above evaluation of adhesiveness, the Mohr stress circle was fitted linearly with respect to the fitting used to calculate the shear stress at a normal stress of 0 kPa, and the maximum principal stress and uniaxial collapse strength were obtained to obtain the single-axis collapse strength. The ratio of the maximum principal stress to the maximum principal stress (maximum principal stress / single decay strength) can be calculated, and the Flow Function can be evaluated.
  • composition The size of the composition of the composition (also simply referred to as "composition") is not particularly limited, but for example, it is preferable that the composition of the dried composition satisfies the following classification conditions.
  • the dried composition is preferably classified by a sieve having the following sieve mesh. From the viewpoint of controlling the ease of handling during manufacturing and the variation in quality, as well as the good texture when used by the user, it usually passes through a sieve having a mesh of 15 mm ( ⁇ 15 mm), and a sieve of 10 mm.
  • a sieve having a mesh ⁇ 10 mm
  • those that pass through a sieve having a sieve of 5 mm ⁇ 5 mm
  • a sieve having a sieve of 3.2 mm is used. It is more preferable that the material passes through ( ⁇ 3.2 mm).
  • the maximum particle size of the gel particles when dried is X mm or less.
  • the above-mentioned dried composition is obtained by holding the composition at 70 ° C. to 80 ° C. for about 3 hours and drying it.
  • the maximum particle size of the composition can be appropriately increased / decreased depending on the blending of the anionic natural polysaccharide (pectin) and Ca ion and the amount of water contained. From the viewpoint of improving fluidity and / and adhesion, it is not necessary to set the lower limit of the particle size of the composition during drying, but from the viewpoint of preventing leakage from the pouch, the maximum particle size of the composition during drying is set. It is usually 0.3 ⁇ m or more.
  • the pouch is capable of packaging the above composition, is insoluble in water, and is permeable to liquids (water, saliva, etc.) and water-soluble components in the composition.
  • the material of the pouch include a cellulosic non-woven fabric, and a commercially available non-woven fabric may be used.
  • a pouch product can be produced by forming a sheet made of such a material into a bag shape, putting the above composition into the bag, and sealing the sheet by means such as heat sealing.
  • the basis weight of the above sheet is not particularly limited, and is usually 12 gsm or more and 54 gsm or less, and preferably 24 gsm or more and 30 gsm or less.
  • the thickness of the above sheet is not particularly limited, and is usually 100 ⁇ m or more and 300 ⁇ m or less, and preferably 175 ⁇ m or more and 215 ⁇ m or less.
  • a water-repellent material may be partially applied to at least one of the inner surface and the outer surface of the pouch.
  • a water-repellent fluororesin is suitable as the water-repellent material.
  • examples of this type of water-repellent fluororesin include Asahi Guard (registered trademark) manufactured by Asahi Glass Co., Ltd.
  • the water-repellent fluororesin is applied to packaging materials for foods and products containing oils and fats such as confectionery, dairy products, prepared foods, fast foods and pet foods, for example. Therefore, this type of water-repellent fluororesin is safe even when applied to a pouch placed in the oral cavity.
  • the water-repellent material is not limited to the fluorine-based resin, and may be any material having a water-repellent action such as a paraffin resin, a silicon-based resin, or an epoxy-based resin.
  • the pouch may contain any component, and examples thereof include raw materials for adjusting aroma and taste, flavors, additives, tobacco extracts, pigments and the like. Further, the mode in which these components are contained is not particularly limited, and examples thereof include a mode in which the pouch surface is coated or impregnated, and in the case of a fiber, the fiber is contained. Further, the appearance of the pouch is not particularly limited, and it may be translucent or transparent as well as non-transparent, in which case the composition packaged in the pouch can be seen through.
  • the pouch product is not particularly limited as long as it has the above composition and the above pouch for packaging the composition (the above pouch is encapsulated with the above composition).
  • the size and weight of the pouch product are not particularly limited, and the size of the pouch product before use may be 25 mm or more (for example, 28 mm, 35 mm, 38 mm) or 40 mm or less on the long side, or 28 mm or more and 38 mm or less.
  • the short side may be 10 mm or more and 20 mm or less, and may be 14 mm or more and 18 mm or less.
  • the weight of the pouch product before use may be 0.1 g or more and 2.0 g or less, or 0.3 g or more and 1.0 g or less.
  • the ratio of the weight of the composition to the total weight of the pouch product is not particularly limited, but is usually 80% by weight or more, preferably 85% by weight or more, more preferably 90% by weight or more, and more preferably 90% by weight or more. It is usually 99% by weight or less, preferably 97% by weight or less, and more preferably 95% by weight or less.
  • the measurement sample is held in the same environment as the measurement environment for 48 hours or more before the measurement.
  • the measured temperature, measured humidity, and measured pressure shall be normal temperature (22 ⁇ 2 ° C), normal humidity (60 ⁇ 5% RH), and normal pressure (atmospheric pressure). ..
  • Another embodiment of the present invention which is a method for producing a nicotine-supplied oral pouch product (also simply referred to as "a method for producing a nicotine-supplied oral pouch product” or “a method for producing”), is at least an anionic natural polymer carbohydrate, a calcium ion feeder. , And a composition manufacturing process for producing a composition containing gel particles containing water.
  • the composition contains nicotine and A method for producing a nicotine-supplied oral pouch product, wherein the content of water in the composition is 15% by weight or more.
  • composition manufacturing process is not particularly limited as long as the above composition can be produced.
  • An example of a method for producing the composition is shown below.
  • each raw material shown below each of the above-mentioned raw materials can be used.
  • an anionic natural polymer carbohydrate such as pectin
  • a nicotine source such as a stabilized nicotine compound
  • a base material such as cellulose
  • a white agent such as silicon dioxide
  • an aqueous solution containing a calcium source such as calcium lactate and an aqueous solution containing a pH adjuster such as anhydrous sodium phosphate are added (for example, added by spraying), and these are mixed to obtain a mixture (mixture before heating).
  • the calcium supply source may be supplied as an aqueous solution or a solid, but when supplied as a liquid such as an aqueous solution, calcium can be mixed with other raw materials in the form of calcium ions and is a solid. It is preferable to supply it as an aqueous solution from the viewpoint of higher contact efficiency with the anionic natural polymer calcium than to supply it with.
  • the calcium source may be added after making the mixture containing the anionic natural polymer carbohydrates or may be mixed first with the anionic natural polymer carbohydrates, producing fine and uniform gel particles. From the viewpoint of allowing the mixture to be added, it is preferable to add the mixture after preparing the mixture containing the anionic natural polymer carbohydrate. On the other hand, it is not preferable to use an anionic natural polymer carbohydrate such as pectin as an aqueous solution from the viewpoint of handling because the viscosity increases when it is made into an aqueous solution. In the addition of each aqueous solution after the step of preparing the mixture before the addition of the calcium source, water may be added together with each aqueous solution in order to obtain a desired water content.
  • the mixture it is preferable to allow the mixture to take in a sufficient amount of water before the following heating step (gel particle forming step), for example, the above-mentioned preheating mixture.
  • the water content of the mixture is preferably 10% by weight or more and 50% by weight or less, and more preferably 20% by weight or more and 40% by weight or less.
  • the pH of the pre-heating mixture is preferably adjusted, and the amount added is preferably adjusted so that the pre-heating mixture becomes acidic, for example, with a pH adjusting agent such as sodium dihydrogen phosphate.
  • the pH of the preheating mixture is preferably 3.0 or more and 6.0 or less, and more preferably 4.0 or more and 6.0 or less. By adjusting the pH to 6.0 or less in this step, it is possible to proceed to the heating process while maintaining the nicotine contained in the preheating mixture in a stable state.
  • Gel particles are prepared by heating the above preheating mixture to hydrate the anionic natural polymer carbohydrates and promote contact between the anionic natural polymer carbohydrates and calcium ions, and the mixture containing the gel particles (gel particle-containing mixture). ) (Heating step).
  • the heating method in the heating step is not particularly limited, and examples thereof include one or both of a method of raising the jacket temperature of the mixer holding the mixture (jacket heating) and a method of injecting steam into the inside of the mixture. ..
  • the temperature of the mixture during heating is not particularly limited, but is preferably 60 ° C. or higher and 90 ° C. or lower, and 70 ° C. or higher and 80 ° C. or lower, from the viewpoint of efficiently hydrating the anionic natural polymer carbohydrate. More preferred.
  • the heating time is not particularly limited, but is preferably 1 hour or more and 3 hours or less from the viewpoint of efficiently reacting the anionic natural polymer carbohydrate with Ca ions and appropriately adjusting the water content in the composition. More preferably, it is 1 hour or more and 2 hours or less.
  • a process of drying the above mixture may be performed (drying step).
  • a cooling process may be performed.
  • the cooling may be natural cooling or may be performed by using some cooling means (cooling step).
  • An aqueous solution containing a pH adjuster such as potassium carbonate is further added to the gel particle-containing mixture obtained in the above heating step (or drying step, cooling step). It is preferable to adjust the addition amount with a pH adjuster such as potassium carbonate so that the mixture after heating becomes alkaline.
  • the pH of the mixture before heating is 6.0 or more and 10.0 or less. It is preferable, and it is more preferable that it is 8.0 or more and 9.0 or less.
  • a sweetening agent such as acesulfame potassium, a fragrance such as menthol, a bitterness inhibitor such as soybean lecithin, and a moisturizer such as glycerin are added (step of adding an additive to a gel particle-containing mixture) to obtain a desired composition.
  • additives and the like When the above additives and the like are added, they may be solid or added in an aqueous solution dissolved in water. When added as an aqueous solution, it may be added by dissolving it in a predetermined amount of water in advance so as to have the final water content of the pouch product.
  • the composition obtained in the above composition manufacturing step is packaged with a packaging agent to obtain a pouch product (packaging step).
  • the packaging method is not particularly limited, and a known method can be applied.
  • a known method such as a method of putting the above composition into a bag-shaped non-woven fabric and then sealing it can be used.
  • water may be further added in order to obtain a composition having a desired water content (water addition step). For example, when the water content of the target composition is 50% by weight and the water content of the composition obtained in the above composition preparation step is 15% by weight, the remaining 35% by weight Add water.
  • the use (use mode) of the pouch product is not particularly limited, and examples thereof include oral tobacco such as chewing tobacco, snuff tobacco, and compressed tobacco, and nicotine-containing preparations called nicotine pouches. These are inserted between the lips and gums in the oral cavity to enjoy the taste and aroma.
  • Example 2 In the above composition 1, the composition 2 (moisture content 18.47 weight) of Example 2 was carried out in the same manner as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 1.71 g. %) was produced in an amount of 100 g.
  • Example 3 In the above composition 1, the same method as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 42.57 g, and the composition 3 of Example 3 (moisture content 32.06 weight). %) was produced in an amount of 200 g.
  • Example 4 In the above composition 1, the composition 4 (moisture content 46.98 weight) of Example 4 was carried out in the same manner as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 108.73 g. %) was produced in an amount of 200 g.
  • Example 5 In the above composition 1, the composition 5 (moisture content 52.49 weight) of Example 5 was carried out in the same manner as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 66.80 g. %) was produced in an amount of 100 g.
  • composition 1 Comparison was made in the same manner as in composition 1 except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to the mixture C was changed from 0 g to 3.46 g. 100 g of the composition 6 of Example 1 (moisture content 18.18% by weight, pH 7.8) was prepared.
  • composition 2 (Comparative Example 2) In the above composition 1, comparison was made in the same manner as in composition 1 except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to the mixture C was changed from 0 g to 43.00 g. 200 g of the composition 7 of Example 2 (moisture content 31.46% by weight) was prepared.
  • Example 3 Comparison was made in the same manner as in composition 1 except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to the mixture C was changed from 0 g to 109.27 g. 200 g of the composition 8 (moisture content 46.60% by weight) of Example 3 was prepared.
  • PH The pH of the composition at a measurement temperature of 22 ° C. was measured using a pH analyzer (for example, manufactured by HORIBA, Ltd .: LAQUA F-72 flat ISFET pH electrode).
  • a pH analyzer for example, manufactured by HORIBA, Ltd .: LAQUA F-72 flat ISFET pH electrode.
  • phthalic acid pH standard solution pH 4.01
  • neutral phosphate pH standard solution pH 6.86
  • borate pH standard solution pH 9.18
  • the shear stress of the composition at a normal stress of 5 kPa was measured using a powder rheometer FT4 manufactured by Freeman Technology Co., Ltd. as a rheometer under the following measurement conditions, and the shear stress at a normal stress of 5 kPa was adopted.
  • a linear regression line is calculated from each value of the shear stress for each normal stress (3 kPa, 4 kPa, 5 kPa, 6 kPa, 7 kPa). Calculate the slope and the value of the Y-intercept. The calculated value of the Y-intercept is taken as the shear stress at a normal stress of 0 kPa.
  • Table 1 summarizes the ratio of raw materials used in each of the above compositions and the evaluation results of each characteristic.
  • the raw materials shown in Table 1 do not show all the raw materials contained, but show some of the raw materials contained.
  • the numerical values of the raw materials shown in the table are not the content rate of each component in the composition but the amount charged.
  • the notation of " ⁇ X" in the maximum particle size of the composition in Table 1 means that the maximum particle size of the composition at the time of drying is X or less.
  • the notation of "-" in Table 1 indicates that no additive is added.
  • Table 2 shows the measurement results of the shear stress of the composition at the normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa described in the above-mentioned adhesiveness, and also shows Example 2 and Comparative Example 1 (moisture content of about 18). 13% by weight), Graphs in which the measurement results of Example 3 and Comparative Example 2 (moisture content of about 30% by weight) and Example 4 and Comparative Example 3 (moisture content of about 45% by weight) are plotted are shown in FIGS. ..
  • compositions of Examples 1 to 5 satisfying the requirements of the above embodiments have a shear stress at a normal stress of 5 kPa as compared with the compositions of Comparative Examples 1 to 3 not satisfying the requirements. It was also found that the shear stress at normal stress of 0 kPa was low, that is, the fluidity and adhesiveness were improved. Specifically, it was found that the combined use of pectin and an aqueous solution of calcium lactate improves fluidity and adhesiveness.
  • Comparative Example 4 In the above composition 1, 200 g of the composition 9 (moisture content 16.12% by weight, pH 7.8) of Comparative Example 4 was prepared by the same method as that of the composition 1 except that the calcium lactate aqueous solution was not added. bottom.
  • Comparative Example 5 Comparative Example 5 in the same manner as in Composition 1 except that the calcium lactate aqueous solution was not added and the amount of water added to the mixture C was changed from 0 g to 105.33 g in the above composition 1. 200 g of the composition 10 (moisture content 47.06% by weight) was prepared.
  • Comparative Example 6 In Comparative Example 6 in the same manner as in Composition 1 except that the calcium lactate aqueous solution was not added and the amount of water added to the mixture C was changed from 0 g to 86.09 g in the above composition 1.
  • the composition 11 moisture content 55.97% by weight of the above was prepared in an amount of 100 g.
  • Table 4 shows the measurement results of the shear stress of the composition at the normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa described in the above-mentioned adhesiveness, and Example 1 and Comparative Example 4 (moisture content of about 15).
  • Figures 4 to 6 plot the measurement results of Example 4 and Comparative Example 5 (water content of about 45% by weight), and Example 5 and Comparative Example 6 (water content of about 50% by weight). ..
  • the compositions of Examples 1 to 5 satisfying the requirements of the above embodiments have a shear stress at a normal stress of 5 kPa as compared with the compositions of Comparative Examples 4 to 6 not satisfying the requirements. It was also found that the shear stress at normal stress of 0 kPa was low, that is, the fluidity and adhesiveness were improved. Specifically, it was found that the fluidity and adhesiveness were improved by using an aqueous solution of calcium lactate. Further, considering Table 1 in Experiment 1 above, from the comparison of the compositions of Example 4, Comparative Example 2 and Comparative Example 5 in which the water content of the composition is about 45% by weight, the normal stress of 5 kPa is in this order.
  • Comparative Example 7 Pectin 7.7 g (H & F Classic CU902), Nicotine Polacrilex 2.2 g (Contraf nicotex Nicotine Polacrilex 20%), Microcrystalline Cellulose 32.8 g (Brenntag Nordic HICEL 90M MCC), Carbonate Sodium 6.3 g (SODIUM CARBONATE ANHYDROUS manufactured by UNIVAR) and 41.2 g (C * Maltidex CH 16385 manufactured by CALDIC NORDIC) were mixed until uniform, and the composition 12 (pH 8.6) of Comparative Example 7 was mixed. , Water content 7.0% by weight) 100 g was obtained. As can be seen from the above production method, Comparative Example 7 is not subjected to addition of an aqueous solution or water, or heat treatment. The water indicated by the above water content is derived from the water originally contained in each of the above raw materials.
  • composition D was prepared in the same manner as in Example 6 except that the amount of cellulose was changed from 885 g to 888 g and the amount of sodium dihydrogen phosphate was changed from 339 g to 342 g. Then, 84 g of a fragrance was added to the obtained mixture D, and 912 g of water was further added and mixed to obtain a composition 13 (moisture content: 30.3% by weight).
  • Table 5 shows a summary of the composition of the raw materials of each of the above examples.
  • the composition of Example 6 satisfying the requirements of the above-described embodiment has a shear stress at a normal stress of 5 kPa and a shear stress at a normal stress of 5 kPa as compared with the composition of Comparative Example 8 not satisfying the requirements. It was found that the shear stress at the time of normal stress of 0 kPa was low, that is, the fluidity and adhesiveness were improved. Specifically, it was found that the composition in which gellan gum and the calcium lactate aqueous solution were used in combination improved the fluidity and adhesiveness. Further, it was found that Examples 6 to 7 had lower shear stress at low normal stress as compared with Comparative Example 8. This is considered to be due to the reduction of the adhesive force between the particles at low normal stress.

Abstract

This nicotine supply oral pouch product comprises a composition containing gel particles, and a pouch for packaging the composition. The gel particles contain at least an anionic natural polymer carbohydrate, calcium ions, and water. The composition contains nicotine. The water content of the composition is 15% by weight or more.

Description

ニコチン供給オーラルパウチ製品およびその製造方法Nicotine Supply Oral Pouch Products and Their Manufacturing Methods
 本発明は、ニコチン供給オーラルパウチ製品、及びその製造方法に関する。 The present invention relates to a nicotine-supplied oral pouch product and a method for producing the same.
 口腔用たばこ製品等のニコチン供給オーラルパウチ製品は、不織布のような材料により形成されたパウチ(包装材)に、ニコチンを含む組成物が収納されてなる包装体であり、使用者はこれを口腔内に入れて使用する。
 ニコチン供給オーラルパウチ製品は、それを使用者の口腔内に投入することで、組成物中のニコチン等の成分が包装材の外部に染み出ることにより、使用者に対して香喫味成分がデリバリーされる。
A nicotine-supplied oral pouch product such as an oral tobacco product is a package in which a composition containing nicotine is stored in a pouch (packaging material) formed of a material such as a non-woven fabric. Put it inside and use it.
In nicotine-supplied oral pouch products, by putting it into the oral cavity of the user, components such as nicotine in the composition exude to the outside of the packaging material, and the flavor component is delivered to the user. NS.
 ニコチン供給オーラルパウチ製品において、使用時における口腔内での使用感は重要であり、口当たりのよさを改善する技術や、製品と唾液とのなじみを改善する技術等が知られている。例えば、封止領域を小さくし、製品内の余剰空気の量を小さくすることにより、使用時の風味の所望の放出を可能とし、口腔内での口当たりのよさを改善する技術の開発(特許文献1)、また、組成物に特定の物質を含有させることにより、製品と唾液とのなじみを改善し、組成物内の物質の口腔内での迅速な経粘膜伝達を促進する技術の開発が進められている(特許文献2)。 In the nicotine-supplied oral pouch product, the feeling of use in the oral cavity at the time of use is important, and the technology for improving the mouthfeel and the technology for improving the familiarity between the product and saliva are known. For example, by reducing the sealing area and the amount of excess air in the product, it is possible to release the desired flavor during use, and the development of a technique for improving the palatability in the oral cavity (Patent Documents). 1) In addition, the development of technology that improves the compatibility between the product and saliva by containing a specific substance in the composition and promotes the rapid transmucosal transmission of the substance in the composition in the oral cavity is progressing. (Patent Document 2).
特表2019-505174号公報Special Table 2019-505174 特表2012-522765号公報Special Table 2012-522765
 上述したように、組成物内の物質の放出の容易さや、製品と唾液とのなじみの容易さ以外にも、ニコチン供給オーラルパウチ製品の使用時における口腔内の使用感に与える要素は挙げられ、該使用感を改善する余地は残されている。
 本発明者らは、一般的なニコチン供給オーラルパウチ製品では、使用時におけるパウチ中の組成物の流動性、及び組成物を構成する材料間の付着性に着目した。パウチ製品中の組成物の流動性を高くすることにより、パウチ製品に圧力がかかる方向と垂直な方向に対するパウチ製品の変形が容易となるため、使用者は、パウチ製品を好みの形状に容易に変形させて口腔内で保持させることができる。また、組成物を構成する材料間の付着性を低くすることにより、パウチ製品に圧力がかかる方向に対するパウチ製品の変形が容易となるため、使用者は、厚みの大きい初期のパウチ製品を容易に薄く変形させることができる。
 上記の流動性の改善は、使用者がパウチ製品を口に含み唾液がしみこんでから使用を終了して口から出すまでの間における使用感の改善であり、また、上記の付着性の改善は、使用者がパウチ製品を口に含んでから唾液がしみこむまでの初期の段階における使用感の改善であり、いずれ特性の改善も使用者にとって利点である。上記の特許文献1及び2には、これらの特性について何ら開示されていない。
As mentioned above, in addition to the ease of release of substances in the composition and the ease of familiarization between the product and saliva, there are other factors that give the oral feeling when using the nicotine-supplied oral pouch product. There is still room for improving the usability.
In a general nicotine-supplied oral pouch product, the present inventors have focused on the fluidity of the composition in the pouch during use and the adhesion between the materials constituting the composition. By increasing the fluidity of the composition in the pouch product, the pouch product can be easily deformed in the direction perpendicular to the direction in which the pressure is applied to the pouch product, so that the user can easily shape the pouch product into a desired shape. It can be deformed and held in the oral cavity. In addition, by reducing the adhesion between the materials constituting the composition, the pouch product can be easily deformed in the direction in which pressure is applied to the pouch product, so that the user can easily make an initial pouch product having a large thickness. It can be deformed thinly.
The above-mentioned improvement in fluidity is an improvement in usability between the time when the user puts the pouch product in the mouth and the saliva soaks into the mouth and the time when the user finishes using the product and takes it out of the mouth. , It is an improvement of usability in the initial stage from the time when the user puts the pouch product in the mouth until the saliva soaks in, and the improvement of the characteristics is also an advantage for the user. The above-mentioned Patent Documents 1 and 2 do not disclose any of these characteristics.
 そこで、本発明は、流動性が改善された、又は、付着性が改善されたニコチン供給オーラルパウチ製品、及びその製造方法を提供することを課題とする。 Therefore, it is an object of the present invention to provide a nicotine-supplied oral pouch product having improved fluidity or improved adhesiveness, and a method for producing the same.
 本発明者らは、鋭意検討の結果、特定の物質を含むゲル粒子を含む組成物を用い、かつ、該組成物中の水の含有率を特定値以上とすることにより、上記課題を解決できることを見出し、本発明に到達した。 As a result of diligent studies, the present inventors can solve the above problems by using a composition containing gel particles containing a specific substance and setting the water content in the composition to a specific value or more. And arrived at the present invention.
[1]ゲル粒子を含む組成物と、該組成物を包装するパウチとを有するニコチン供給オーラルパウチ製品であって、
 該ゲル粒子が、少なくともアニオン天然ポリマー炭水化物、カルシウムイオン、及び水を含み、
 該組成物がニコチンを含み、
 該組成物中の水の含有率が15重量%以上である、
 ニコチン供給オーラルパウチ製品。
[2]前記アニオン天然ポリマー炭水化物が、カルボキシル基を有する、[1]に記載のニコチン供給オーラルパウチ製品。
[3]前記アニオン天然ポリマー炭水化物が、LMペクチンである、[2]に記載のニコチン供給オーラルパウチ製品。
[4]前記組成物において、前記アニオン天然ポリマー炭水化物が有する総カルボキシル基数と、前記カルシウムイオンの総個数との比が、100:1~2:1である、[2]又は[3]に記載のニコチン供給オーラルパウチ製品。
[5]前記組成物の構成物の乾燥時の最大粒度が、15mm以下である、[1]~[4]のいずれかに記載のニコチン供給オーラルパウチ製品。
[6]前記パウチが不織布である、[1]~[5]のいずれかに記載のニコチン供給オーラルパウチ製品。
[7]少なくともアニオン天然ポリマー炭水化物、カルシウムイオン供給剤、及び水を含むゲル粒子を含む組成物を製造する組成物製造工程を有し、
 該組成物がニコチンを含み、かつ、
 該組成物中の水の含有率が、15重量%以上である、ニコチン供給オーラルパウチ製品の製造方法。
[8]前記カルシウムイオン供給剤が液体である、[7]に記載のニコチン供給オーラルパウチ製品の製造方法。
[9]前記カルシウムイオン供給剤が、乳酸カルシウムを含む、[7]又は[8]に記載のニコチン供給オーラルパウチ製品の製造方法。
[1] A nicotine-supplied oral pouch product comprising a composition containing gel particles and a pouch for packaging the composition.
The gel particles contain at least anionic natural polymer carbohydrates, calcium ions, and water.
The composition comprises nicotine
The content of water in the composition is 15% by weight or more.
Nicotine-supplied oral pouch products.
[2] The nicotine-supplied oral pouch product according to [1], wherein the anionic natural polymer carbohydrate has a carboxyl group.
[3] The nicotine-supplied oral pouch product according to [2], wherein the anionic natural polymer carbohydrate is LM pectin.
[4] The method according to [2] or [3], wherein the ratio of the total number of carboxyl groups of the anionic natural polymer carbohydrate to the total number of calcium ions in the composition is 100: 1 to 2: 1. Nicotine Supply Oral Pouch Products.
[5] The nicotine-supplied oral pouch product according to any one of [1] to [4], wherein the maximum particle size of the composition of the composition when dried is 15 mm or less.
[6] The nicotine-supplied oral pouch product according to any one of [1] to [5], wherein the pouch is a non-woven fabric.
[7] It has a composition manufacturing process for producing a composition containing at least an anionic natural polymer carbohydrate, a calcium ion feeder, and gel particles containing water.
The composition contains nicotine and
A method for producing a nicotine-supplied oral pouch product, wherein the content of water in the composition is 15% by weight or more.
[8] The method for producing a nicotine-supplied oral pouch product according to [7], wherein the calcium ion feeder is a liquid.
[9] The method for producing a nicotine-supplied oral pouch product according to [7] or [8], wherein the calcium ion feeder contains calcium lactate.
 本発明により、流動性が改善された、又は、付着性が改善されたニコチン供給オーラルパウチ製品、及びその製造方法を提供することができる。 INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide a nicotine-supplied oral pouch product having improved fluidity or improved adhesiveness, and a method for producing the same.
実施例2及び比較例1の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 2 and Comparative Example 1. 実施例3及び比較例2の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 3 and Comparative Example 2. 実施例4及び比較例3の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 4 and Comparative Example 3. 実施例1及び比較例4の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 1 and Comparative Example 4. 実施例4及び比較例5の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 4 and Comparative Example 5. 実施例5及び比較例6の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 5 and Comparative Example 6. 実施例6及び比較例8の各組成物における垂直応力と剪断応力との関係を示すグラフである。It is a graph which shows the relationship between the normal stress and the shear stress in each composition of Example 6 and Comparative Example 8.
 以下に本発明の実施の形態を詳細に説明するが、これらの説明は本発明の実施形態の一例(代表例)であり、本発明はその要旨を超えない限りこれらの内容に限定されない。
 本明細書において、「~」を用いて表される数値範囲は、「~」の前後に記載された数値を下限値及び上限値として含む範囲を意味し、「A~B」は、A以上B以下であることを意味する。
Hereinafter, embodiments of the present invention will be described in detail, but these descriptions are examples (representative examples) of the embodiments of the present invention, and the present invention is not limited to these contents as long as the gist thereof is not exceeded.
In the present specification, the numerical range represented by using "-" means a range including the numerical values before and after "-" as the lower limit value and the upper limit value, and "A to B" means A or more. It means that it is B or less.
<ニコチン供給オーラルパウチ製品>
 本発明の実施形態であるニコチン供給オーラルパウチ製品は、ゲル粒子を含む組成物と、該組成物を包装するパウチとを有するニコチン供給オーラルパウチ製品であって、
 該ゲル粒子が、少なくともアニオン天然ポリマー炭水化物、カルシウムイオン、及び水を含み、
 該組成物がニコチンを含み、
 該組成物中の水の含有率が15重量%以上である、
 ニコチン供給オーラルパウチ製品である。
<Nicotine supply oral pouch products>
The nicotine-supplied oral pouch product according to the embodiment of the present invention is a nicotine-supplied oral pouch product having a composition containing gel particles and a pouch for packaging the composition.
The gel particles contain at least anionic natural polymer carbohydrates, calcium ions, and water.
The composition comprises nicotine
The content of water in the composition is 15% by weight or more.
It is a nicotine-supplied oral pouch product.
 上記のオーラルパウチ製品では、パウチ内の組成物にゲル粒子を含ませ、さらに、ゲル粒子として、少なくともアニオン天然ポリマー炭水化物をカルシウムイオンで架橋させ、水を含む分散媒で膨潤させた構造を有するものを用い、かつ、組成物中の水の含有率を15重量%以上とすることにより、該組成物の流動性又は/及び付着性を改善することができる。具体的には、水を含んで膨潤するアニオン天然ポリマー炭水化物の流動性又は/及び付着性を改善することができる。 In the above oral pouch product, the composition in the pouch contains gel particles, and the gel particles have a structure in which at least anionic natural polymer carbohydrates are crosslinked with calcium ions and swollen with a dispersion medium containing water. , And the content of water in the composition is 15% by weight or more, so that the fluidity and / or adhesiveness of the composition can be improved. Specifically, the fluidity and / and adhesion of anionic natural polymer carbohydrates that swell with water can be improved.
[組成物]
 組成物の組成は、少なくともアニオン天然ポリマー炭水化物、カルシウムイオン、及び水を含むゲル粒子、及びニコチンを含んでいれば、特段制限されない。本発明における組成物とは、パウチ内に含まれる任意の物質の総称である。また、パウチ外への組成物の漏れを防ぐ観点から、組成物は液体でないことが好ましく、例えば、ゲル状のゲル粒子のみからなる、又はゲル粒子と固体状の物質からなることが好ましい。また、後述の粒度の好適態様を満たすようにするため、乾燥後に粒子形状(複数個の粒子)となることが好ましい。
[Composition]
The composition of the composition is not particularly limited as long as it contains at least anionic natural polymer carbohydrates, calcium ions, and gel particles containing water, and nicotine. The composition in the present invention is a general term for any substance contained in a pouch. Further, from the viewpoint of preventing the composition from leaking to the outside of the pouch, the composition is preferably not a liquid, and for example, it is preferably composed of only gel-like gel particles or a gel-like particles and a solid substance. Further, in order to satisfy the preferred embodiment of the particle size described later, it is preferable that the particles have a particle shape (plurality of particles) after drying.
 オーラルパウチ製品は、ゲル粒子を含む組成物を有する。組成物に含まれるゲル粒子は、粒子状のゲルであれば特段制限されない。
 本明細書において「粒子状」とは、小さい粒状を表し、完全な球体上でなくともよく、具体的には、球体状、楕円体状、棒状、板状、又は外観上、これらの形状に近い形状などが含まれる。
 また、本明細書において、「ゲル状」とは、流動性を有するゾル状の分解生成物が固化して弾性を維持しつつ自発的な流動性を喪失した状態をいい、そのような状態の物質を「ゲル」と称し、ゲルからなる物質を「ゲル物質」と称する。
Oral pouch products have compositions that include gel particles. The gel particles contained in the composition are not particularly limited as long as they are particulate gels.
As used herein, the term "particulate" means small particles, which do not have to be on a perfect sphere, and specifically, on a sphere, an ellipsoid, a rod, a plate, or in appearance. Includes similar shapes.
Further, in the present specification, the “gel-like” refers to a state in which a sol-like decomposition product having fluidity is solidified and loses spontaneous fluidity while maintaining elasticity, and in such a state. A substance is called a "gel", and a substance consisting of a gel is called a "gel substance".
 組成物中のゲル粒子の含有率は、特段制限されないが、通常0.01重量%以上であり、0.05重量%以上であることが好ましく、0.1重量%以上であることがより好ましく、1.0重量%以上であることがさらに好ましく、また、通常50.0重量%以下であり、20.0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、5.0重量%以下であることがさらに好ましい。 The content of the gel particles in the composition is not particularly limited, but is usually 0.01% by weight or more, preferably 0.05% by weight or more, and more preferably 0.1% by weight or more. , 1.0% by weight or more, and usually 50.0% by weight or less, preferably 20.0% by weight or less, and more preferably 10.0% by weight or less. , 5.0% by weight or less, more preferably.
 ゲル粒子は、少なくともアニオン天然ポリマー炭水化物、カルシウムイオン、及び水を含んで入れば特段制限されない。
(ゲル化剤)
 アニオン天然ポリマー炭水化物は、ゲル化剤であり、その種類は特段制限されないが、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(キサンタンガム)、ジェラン(ジェランガム)、トラガントガム、アルギン酸が好ましく、さらには、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、アルギン酸であることが好ましい。これらの中でも、後述の理由から、LMペクチンが好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。
The gel particles are not particularly limited as long as they contain at least anionic natural polymer carbohydrates, calcium ions, and water.
(Gel agent)
The anionic natural polymer carbohydrate is a gelling agent, the type of which is not particularly limited, but a polysaccharide having a carboxyl group is preferable, for example, carrageenan, pectin, arabic gum, xanthan (xanthan gum), gellan (gellan gum), tragant gum, etc. Alginic acid is preferable, and carrageenan, pectin, gellan gum, and alginic acid are preferable from the viewpoint that they are easily gelled in the presence of calcium ions and a junction zone can be formed by a carboxyl group and a cation to form a crosslinked structure. .. Among these, LM pectin is preferable for the reason described later. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 「ペクチン」は、ガラクツロン酸及びガラクツロン酸メチルエステルを構成単位とし、それらがα1,4-結合した多糖類である。ガラクツロン酸の他にも、いくつかの多様な糖を含むことが知られている。一般的にペクチンは、エステル化度が50%未満のLMペクチンと、エステル化度が50%以上のHMペクチンに分類され、上述の通り、本実施形態ではLMペクチンが好ましい。
 ペクチンは、特に、カルシウムイオン等の2価の陽イオンの存在下でゲル化し、ペクチン中のガラクツロン酸の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ゲルを形成する。ジャンクションゾーンの多い、即ち、エステル化度の低いペクチンの方が、ゲル化性が強くなる。
 ペクチンのエステル化度は、20%以下であることが好ましく、12%以下があることがより好ましく、10%以下であることがさらに好ましく、また、エステル化度の下限を設定する必要はないが、通常6%以上となる。
"Pectin" is a polysaccharide having galacturonic acid and galacturonic acid methyl ester as constituent units and α1,4-bonded to them. In addition to galacturonic acid, it is known to contain several diverse sugars. Generally, pectin is classified into LM pectin having a degree of esterification of less than 50% and HM pectin having a degree of esterification of 50% or more. As described above, LM pectin is preferable in this embodiment.
In particular, pectin gels in the presence of divalent cations such as calcium ions, and the carboxyl group of galacturonic acid in pectin and cations form a junction zone to form a gel. Pectin having a large number of junction zones, that is, a pectin having a low degree of esterification, has a stronger gelling property.
The degree of esterification of pectin is preferably 20% or less, more preferably 12% or less, further preferably 10% or less, and it is not necessary to set a lower limit of the degree of esterification. , Usually 6% or more.
 「ジェランガム」は、真正細菌の1種のシュードモナス・エロデア(Pseudomonas elodea)によって合成される水溶性の多糖類として知られている。水溶液に陽イオンが加わると、電気的に中和されてゲランガムの水溶性が低下してゲル化する。ジェランガムは、2つのD-グルコース残基、1つのL-ラムノース残基及び1つのD-グルクロン酸の4糖からなる繰り返し単位が、直鎖状に連結した高分子化合物である。4糖の繰り返し構造は、以下の通りである。
 [D-Glc(β1→4)D-GlcA(β1→4)D-Glc(β1→4)L-Rha(α1→3)]n
"Gelangum" is known as a water-soluble polysaccharide synthesized by one of the eubacteria, Pseudomonas elodea. When cations are added to the aqueous solution, they are electrically neutralized and the water solubility of gellan gum decreases, resulting in gelation. Gellan gum is a polymeric compound in which repeating units consisting of two D-glucose residues, one L-rhamnose residue and one D-glucuronic acid tetrasaccharide are linearly linked. The repeating structure of tetrasaccharides is as follows.
[D-Glc (β1 → 4) D-GlcA (β1 → 4) D-Glc (β1 → 4) L-Rha (α1 → 3)] n
 「カラギーナン」は、直鎖含硫黄多糖類の一種で、D-ガラクトース(又は3,6-アンヒドロ-D-ガラクトース)と硫酸とから構成される陰イオン性高分子化合物である。 "Carrageenan" is a kind of linear sulfur-containing polysaccharide and is an anionic polymer compound composed of D-galactose (or 3,6-anhydro-D-galactose) and sulfuric acid.
 「アルギン酸」は、主に褐藻に含まれる多糖類の一種である。α-L-グルロン酸、β-D-マンヌロン酸がピラノース型で1,4-グリコシド結合で結合した構造を有する(CAS 9005-38-3)。陽イオンを添加するとゲル化する性質を有する。 "Alginic acid" is a type of polysaccharide mainly contained in brown algae. It has a structure in which α-L-gluuronic acid and β-D-mannuronic acid are pyranose-type and bound by a 1,4-glycosidic bond (CAS 9005-38-3). It has the property of gelling when cations are added.
 「アラビアガム」は、「アラビアゴム」又は「アラビア樹脂」とも呼称され、マメ科ネムノキ亜科アカシア属アラビアゴムノキ(Acacia senegal)、またはその同属近縁植物の樹皮の傷口からの分泌物を乾燥させたものである。主成分は多糖類(ポリウロン酸)であり、アラビノガラクタン(75-94%)、アラビノガラクタン-プロテイン(5-20%)、糖タンパク質(1-5%)の混合物である。多糖類の構造は主鎖にガラクトース、側鎖にガラクトース、アラビノース、ラムノース、グルクロン酸を有する。細胞壁を構成するヘミセルロースとはカルボキシル基が遊離している点が異なり、通常カルシウム塩となっている。 "Gum arabic" is also called "gum arabic" or "resin arabic" and dries the secretions from the wounds of the bark of the legumes, Albizia subfamily, Acacia, or related plants of the same genus. It is a thing. The main component is a polysaccharide (polyuronic acid), which is a mixture of arabinogalactan (75-94%), arabinogalactan-protein (5-20%), and glycoprotein (1-5%). The structure of the polysaccharide has galactose in the main chain and galactose, arabinose, rhamnose, and glucuronic acid in the side chain. It is usually a calcium salt, unlike hemicellulose, which constitutes the cell wall, in that the carboxyl group is free.
 「キサンタン」は、多糖類の1種で、一般に、トウモロコシ糖のでんぷんを細菌により発酵させて製造される。グルコース2分子、マンノース2分子、グルクロン酸分子を単位とする繰り返し構造を有する(CAS 11138-66-2)。 "Xanthan" is a type of polysaccharide and is generally produced by fermenting corn sugar starch with bacteria. It has a repeating structure with two glucose molecules, two mannose molecules, and a glucuronic acid molecule as units (CAS 11138-66-2).
 「トラガントガム」は、マメ科植物のトラガントの分泌液を乾燥させて得られた増粘多糖類でありアラビノース、キシロース、フコース、ガラクトース、ガラクツロン酸などから成る複雑な多糖類混合物である。主成分は酸性および中性の2種の多糖類であるが、デンプン、セルロース、無機質などを含む。 "Tragant gum" is a thickening polysaccharide obtained by drying the secretion of Tragant, a legume, and is a complex polysaccharide mixture consisting of arabinose, xylose, fucose, galactose, galacturonic acid, and the like. The main components are two types of polysaccharides, acidic and neutral, but include starch, cellulose, minerals and the like.
 GPC(Gel Permeation Chromatography)で測定し、標準ポリスチレンの検量線で換算したアニオン天然ポリマー炭水化物の重量平均分子量(Mw)は、例えば、100,000g/mol以上、700,000g/mol以下であってよく、140,000g/mol以上、300,000g/mol以下であってよく、これらの範囲に制限されず、ゲル化が達成される最低限の分子量を担保していればよい。該重量平均分子量は、2価のカチオンの添加により増加させることができ、また、アルカリの添加により減少させることができる。 The weight average molecular weight (Mw) of the anionic natural polymer carbohydrate measured by GPC (Gel Permeation Chromatography) and converted by the calibration curve of standard polystyrene may be, for example, 100,000 g / mol or more and 700,000 g / mol or less. , 140,000 g / mol or more and 300,000 g / mol or less, and is not limited to these ranges, as long as the minimum molecular weight at which gelation is achieved is guaranteed. The weight average molecular weight can be increased by the addition of a divalent cation and can be decreased by the addition of an alkali.
 組成物中のアニオン天然ポリマー炭水化物の含有率は、特段制限されないが、通常0.01重量%以上であり、0.1重量%以上であることが好ましく、1.0重量%以上であることがより好ましく、2.0重量%以上であることがさらに好ましく、また、通常50.0重量%以下であり、20重量%以下であることが好ましく、10重量%以下であることがより好ましく、5重量%以下であることがさらに好ましい。
 組成物中のアニオン天然ポリマー炭水化物の含有率は、液体クロマトグラフィーや液体クロマトグラフィー質量分析計などによる種々の分画分離方法、検出方法で測定することができる。
The content of the anionic natural polymer carbohydrate in the composition is not particularly limited, but is usually 0.01% by weight or more, preferably 0.1% by weight or more, and preferably 1.0% by weight or more. More preferably, it is more preferably 2.0% by weight or more, and usually it is 50.0% by weight or less, preferably 20% by weight or less, and more preferably 10% by weight or less. It is more preferably 0% by weight or less.
The content of anionic natural polymer carbohydrates in the composition can be measured by various fraction separation methods and detection methods such as liquid chromatography and liquid chromatography mass spectrometer.
(ゲル化補助成分)
 カルシウムイオンは、ゲル化補助成分であり、その供給源(ゲル化補助剤)は、特段制限されないが、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、乳酸塩等が挙げられるが、これらのうち、パウチ製品への味の影響が少ない、溶解性が高い、溶解後のpHの観点から、乳酸カルシウム、炭酸カルシウム、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種類以上を任意の種類及び比率で併用してもよい。
(Auxiliary gelation component)
Calcium ion is a gelling auxiliary component, and its source (gelling auxiliary agent) is not particularly limited, but for example, calcium halide (chloride, etc.), citric acid, carbonate, sulfate, phosphorus. Examples thereof include acid salts and lactates, and among these, calcium lactate, calcium carbonate, and calcium phosphate are preferable from the viewpoint of less influence of taste on pouch products, high solubility, and pH after dissolution, and in particular, Calcium lactate is preferred. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 組成物中のカルシウムイオンの含有率は、特段制限されないが、良好な流動性及び付着性を確保する観点から、組成物の重量に対するモル比率で、通常0.00023mol/kg以上であり、0.0023mol/kg以上であることが好ましく、0.023mol/kg以上であることがより好ましく、0.046mol/kg以上であることがさらに好ましく、また、通常1.15mol/kg以下であり、0.46mol/kg以下であることが好ましく、0.23mol/kg以下であることがより好ましく、0.11mol/kg以下であることがさらに好ましい。
 組成物中のカルシウムイオンの含有率は、通常、原子吸光分析法で測定することができる。
The content of calcium ions in the composition is not particularly limited, but from the viewpoint of ensuring good fluidity and adhesiveness, the molar ratio to the weight of the composition is usually 0.00023 mol / kg or more, and 0. It is preferably 0023mol / kg or more, more preferably 0.023 mol / kg or more, further preferably 0.046 mol / kg or more, and usually 1.15 mol / kg or less, 0. It is preferably 46 mol / kg or less, more preferably 0.23 mol / kg or less, and even more preferably 0.11 mol / kg or less.
The content of calcium ions in the composition can usually be measured by atomic absorption spectrometry.
 アニオン天然ポリマー炭水化物として、カルボキシル基を有する化合物を用いる場合、上述のゲル化剤を構成するアニオン天然ポリマー炭水化物は、2価の陽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ゲルを形成する。ゲルにジャンクションゾーンが存在すると、ゲルを含む組成物は、網目構造となる。カルボキシル基とゲル化促進成分である2価の陽イオンを含む化合物とを効率良くゲル化させ、両者が2:1の個数比で存在することが望ましい。これは、アニオン天然ポリマー炭水化物中のカルボキシル基を含むモノマーと陽イオンのモル比が2:1である場合に対応する。したがって、アニオン天然ポリマー炭水化物が有する総カルボキシル基数と、カルシウムイオンの総個数との比は、好ましくは、100:1~2:1、50:1~2:1、10:1~2:1の範囲である。 When a compound having a carboxyl group is used as the anionic natural polymer carbohydrate, the anionic natural polymer carbohydrate constituting the above-mentioned gelling agent tends to gel in the presence of divalent cations, and the junction zone is formed by the carboxyl group and the cations. To form a gel. If a junction zone is present in the gel, the composition containing the gel will have a network structure. It is desirable that a compound containing a carboxyl group and a divalent cation which is a gelation promoting component is efficiently gelled, and both are present in a number ratio of 2: 1. This corresponds to the case where the molar ratio of the monomer containing a carboxyl group to the cation in the anionic natural polymer carbohydrate is 2: 1. Therefore, the ratio of the total number of carboxyl groups of the anionic natural polymer carbohydrate to the total number of calcium ions is preferably 100: 1 to 2: 1, 50: 1 to 2: 1, 10: 1 to 2: 1. The range.
(その他のゲル化補助成分)
 組成物は、カルシウムイオン以外のゲル化補助成分を含有してもよく、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、カチオン性高分子のイオン等が挙げられ、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、カチオン性高分子等が挙げられる。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。
(Other gelling auxiliary ingredients)
The composition may contain a gelling auxiliary component other than calcium ions, for example, magnesium, silver, zinc, copper, gold, aluminum, etc., to which a gelling agent can be bonded by an ionic bond like calcium ions. Metal ions, cationic polymer ions, etc., and examples of these sources (other gelling aids) include halides (chlorides, etc.), citric acid, and carbonic acid of these metal ions. Examples thereof include salts, sulfates, phosphates and cationic polymers. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
(水)
 組成物に含まれる水の種類は、特段制限されない。
 組成物中の水の含有率(含水率)は、15重量%以上である。含水率が15重量%未満の場合、ざらつきのある食感となってしまい、また、組成物の製造が困難となる。さらに、組成物の良好な流動性及び付着性の確保、及び組成物の製造容易性の観点から、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、また、通常55重量%以下であり、50重量%以下であることが好ましい。該含水率は、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。
(water)
The type of water contained in the composition is not particularly limited.
The water content (moisture content) in the composition is 15% by weight or more. If the water content is less than 15% by weight, the texture becomes rough and the composition becomes difficult to produce. Further, from the viewpoint of ensuring good fluidity and adhesiveness of the composition and easiness of producing the composition, it is preferably 30% by weight or more, more preferably 45% by weight or more, and usually. It is 55% by weight or less, and preferably 50% by weight or less. The water content can be adjusted by adjusting the amount of water to be added, or by providing a heat treatment or a drying treatment at the production stage.
 上記の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。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。
 なお、本明細書における含水率の測定方法は、組成物以外の対象、例えば、後述する組成物の製造方法における混合物の含水率の測定においても同様に適用する。
The water content (moisture content) of the above composition is measured using a heat-drying moisture meter (for example, manufactured by METTER TOLEDO: HB 43-S). At the time of measurement, the sample is put into a predetermined container and heated to an ultimate temperature of 100 ° C. The measurement is completed when the amount of change is 1 mg or less in 60 seconds, and the water content is calculated from the weighed values before and after heating.
The method for measuring the water content in the present specification is similarly applied to the measurement of the water content of a mixture other than the composition, for example, in the method for producing a composition described later.
(ニコチン)
 組成物は、ニコチンを含むが、ニコチンを含む態様は特段制限されず、例えば、化合物としてのニコチンを含有させてもよく、ニコチン塩や安定化させたニコチン(例えばイオン交換樹脂に吸着させたニコチン)等のニコチン含有化合物を含有させてもよく、また、ニコチン供給源としてたばこ葉を加えてもよく、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を含有させてもよい。また、ニコチンを含有させる態様も特段制限されず、上記の化合物やニコチン供給源、抽出液を、ゲル粒子に含有させてもよく、ゲル粒子とは別に組成物中に含有させてもよい。これらの態様の中でも、的確なニコチンの供給や、取扱い易さの観点から、ニコチン含有化合物の添加が好ましい。また、通常、たばこ葉を添加した場合、組成物やパウチ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、白色の組成物やパウチ製品を提供することが可能となる。白色のパウチ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。
 上記の態様は、1つの態様を単独で適用してもよく、また、2つ以上の態様を併用して適用してもよい。
(nicotine)
The composition contains nicotine, but the mode containing nicotine is not particularly limited. For example, nicotine as a compound may be contained, and a nicotine salt or stabilized nicotine (for example, nicotine adsorbed on an ion exchange resin) may be contained. ) Or other nicotine-containing compounds may be contained, tobacco leaves may be added as a nicotine source, or a nicotine-containing extract obtained by extracting a nicotine-containing substance such as tobacco leaves may be contained. good. Further, the mode in which nicotine is contained is not particularly limited, and the above compound, nicotine source, and extract may be contained in the gel particles, or may be contained in the composition separately from the gel particles. Among these aspects, the addition of a nicotine-containing compound is preferable from the viewpoint of accurate supply of nicotine and ease of handling. In addition, when tobacco leaves are added, the color of the composition or pouch product tends to be the color of the tobacco leaf, whereas when a colorless nicotine-containing compound is used, a white composition or pouch product is provided. It becomes possible to do. For users who prefer white pouch products, such an embodiment is an advantage.
One aspect may be applied alone, or two or more aspects may be applied in combination.
 組成物中のニコチンの含有率は、特段制限されないが、ユーザーの嗜好性の観点から、通常0.1重量%以上であり、また、通常6.7重量%以下である。なお、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。
 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)で測定することができる。
The content of nicotine in the composition is not particularly limited, but is usually 0.1% by weight or more and usually 6.7% by weight or less from the viewpoint of user preference. When nicotine is present as an ion, the above content is the content as a nicotine ion.
The content of nicotine in the composition can be measured with a gas chromatography-mass spectrometer (GC-MS).
(その他の物質)
 組成物は、上記のアニオン天然ポリマー炭水化物、カルシウムイオン、その他のゲル化補助剤、水、ニコチン以外の物質(「その他の物質」とも称する)を含有していてもよく、該その他の物質は、ゲル粒子に含ませてもよく、また、ゲル粒子とは別に組成物に含ませてもよい。その他の物質としては、例えば、基材、香料、pH調整剤、甘味料、保湿剤、苦味抑制剤、白色剤、又は乳化剤等が挙げられる。
 組成物中のその他の物質の含有率は、特段制限されず、製品設計に応じて適宜配合を調整することができる。
(Other substances)
The composition may contain substances other than the above-mentioned anionic natural polymer carbohydrates, calcium ions, other gelling aids, water and nicotine (also referred to as "other substances"), and the other substances may contain. It may be contained in the gel particles, or may be contained in the composition separately from the gel particles. Examples of other substances include base materials, flavors, pH adjusters, sweeteners, moisturizers, bitterness suppressants, whitening agents, emulsifiers and the like.
The content of other substances in the composition is not particularly limited, and the composition can be appropriately adjusted according to the product design.
 基材の種類は、特段制限されず、例えば、セルロース、微結晶セルロース、球状セルロース、多孔質セルロース等が挙げられ、組成物のかさ密度調整の自由度の観点から、セルロースが好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。
 組成物中の基材の含有率は、特段制限されないが、製造中又は製品保管中における水分の溶出の抑制という品質向上の観点から、通常24重量%以上であり、27量%以上であることが好ましく、30重量%以上であることがより好ましく、また、特段上限を制限する必要はないが、その他の原料を配合できる限界の観点から、通常65重量%以下であり、55重量%以下であることが好ましく、50重量%以下であることがより好ましい。
The type of the base material is not particularly limited, and examples thereof include cellulose, microcrystalline cellulose, spherical cellulose, and porous cellulose, and cellulose is preferable from the viewpoint of the degree of freedom in adjusting the bulk density of the composition. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
The content of the base material in the composition is not particularly limited, but is usually 24% by weight or more and 27% by weight or more from the viewpoint of quality improvement of suppressing elution of water during production or product storage. Is preferable, and it is more preferably 30% by weight or more, and it is not necessary to limit the upper limit in particular, but from the viewpoint of the limit in which other raw materials can be blended, it is usually 65% by weight or less, and 55% by weight or less. It is preferably present, and more preferably 50% by weight or less.
 香料の種類は、特段制限されず、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、β-ダマセノン等のダマセノン、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)、炭化水素類(例えば、リモネン、ピネン等)が挙げられる。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The types of flavors are not particularly limited, for example, menthol, leaf tobacco extract, natural vegetable flavors (eg, cinnamon, sage, herbs, chamomile, kudzu, sweet tea, cloves, lavender, cardamon, chowji, nutmeg, bergamot, etc. Geranium, Honey Essence, Rose Oil, Lemon, Orange, Kay Skin, Caraway, Jasmine, Ginger, Coriander, Vanilla Extract, Spare Mint, Peppermint, Cassia, Coffee, Cellory, Cascarilla, Sandalwood, Cocoa, Iran Iran, Fennell, Anis , Licoris, St. John's bread, peach extract, peach extract, etc.), sugars (eg glucose, fructose, isomerized sugar, caramel, honey, sugar honey, etc.), cocoa (powder, extract, etc.), esters (eg, acetic acid) Isoamyl, linalyl acetate, isoamyl propionate, linaryl butyrate, etc.), ketones (eg, menton, ionone, damasenone such as β-damasenone, ethylmaltor, etc.), alcohols (eg, geraniol, linalol, anetol, eugenol, etc.), Urdes (eg, vanillin, benzaldehyde, anisaldehyde, etc.), lactones (eg, γ-undecalactone, γ-nonalactone, etc.), animal flavors (eg, musk, amberglis, civet, castorium, etc.), hydrocarbons Classes (eg, limonene, pinen, etc.) can be mentioned. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 組成物中のゲル粒子の含有率は、特段制限されないが、所望の味香りを楽しむことができる観点から、通常0.1重量%以上であり、1重量%以上であることが好ましく、2重量%以上であることがより好ましく、また、通常20重量%以下であり、15重量%以下であることが好ましく、10重量%以下であることがより好ましい。 The content of the gel particles in the composition is not particularly limited, but from the viewpoint of enjoying the desired taste and aroma, it is usually 0.1% by weight or more, preferably 1% by weight or more, and 2% by weight. % Or more, and usually 20% by weight or less, preferably 15% by weight or less, and more preferably 10% by weight or less.
 pH調整剤の種類は、特段制限されず、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、無水リン酸ナトリウム、リン酸二水素ナトリウム、クエン酸ナトリウム等が挙げられ、製品の呈味への影響の観点から、炭酸ナトリウム、炭酸カリウム、リン酸二水素ナトリウムが好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The type of pH adjuster is not particularly limited, and examples thereof include sodium carbonate, sodium hydrogencarbonate, potassium carbonate, potassium hydrogencarbonate, anhydrous sodium phosphate, sodium dihydrogen phosphate, sodium citrate, and the like. Sodium carbonate, potassium carbonate, and sodium dihydrogen phosphate are preferable from the viewpoint of the influence on the taste. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 甘味料の種類は、特段制限されず、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、アスパルテーム等の甘味料などが挙げられ、味の調節の観点から糖アルコールが好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The type of sweetener is not particularly limited, and examples thereof include sugar alcohols such as xylitol, maltitol, and erythritol, and sweeteners such as acesulfame potassium, sucralose, and aspartame. Sugar alcohols are preferable from the viewpoint of adjusting the taste. .. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 苦味抑制剤は、特段制限されず、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、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、ホスファチジン酸などが挙げられる。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The bitterness inhibitor is not particularly limited, and examples thereof include soybean lecithin. Soybean lecithin is a phospholipid, and examples thereof include phosphatidylcholine, phosphatidylethanolamine, and phosphatidylic acid. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 保湿剤の種類は、特段制限されず、例えば、グリセリン、プロピレングリコール等が挙げられ、製品保存性の観点から、グリセリンが好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The type of moisturizer is not particularly limited, and examples thereof include glycerin and propylene glycol, and glycerin is preferable from the viewpoint of product storage stability. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 白色剤の種類は、特段制限されず、例えば、二酸化ケイ素、二酸化チタン、炭酸カルシウム等が挙げられ、製品への味の影響の観点から、二酸化ケイ素が好ましい。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The type of whitening agent is not particularly limited, and examples thereof include silicon dioxide, titanium dioxide, and calcium carbonate. Silicon dioxide is preferable from the viewpoint of the influence of taste on the product. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 乳化剤の種類は、特段制限されず、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、および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あげることできる。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、ジグリセリン脂肪酸エステル、トリグリセリン脂肪酸エステル、デカグリセリン脂肪酸エステルを挙げることができる。これらの物質は、1種類を単独で用いてもよく、また、2種類以上を任意の種類及び比率で併用してもよい。 The type of emulsifier is not particularly limited, and examples thereof 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, and polyglycerin fatty acid ester and lecithin. Examples of the sucrose fatty acid ester include sucrose palmitic acid ester and sucrose stearic acid ester. Examples of the organic acid glycerin fatty acid ester include succinate glycerin fatty acid ester and diacetyl tartrate glycerin fatty acid ester. Examples of the polyglycerin fatty acid ester include diglycerin fatty acid ester, triglycerin fatty acid ester, and decaglycerin fatty acid ester. One of these substances may be used alone, or two or more of these substances may be used in combination in any kind and ratio.
 上記の各成分の含有率(水の含有率を除く)は、原料の仕込み量から算出することもできる。 The content rate of each of the above components (excluding the water content rate) can also be calculated from the amount of raw materials charged.
(組成物のpH)
 測定温度22℃における組成物のpHは、特段制限されないが、製品の味への影響の観点から、通常6.0以上であり、7.0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、9.0以下であることが好ましい。該pHは、pH調整剤の添加量を制御することで調整することができる。なお、上記のpHの値だけでなく、本明細におけるpHの値は、測定温度22℃で測定した値である。
(PH of composition)
The pH of the composition at a measurement temperature of 22 ° C. is not particularly limited, but is usually 6.0 or more, preferably 7.0 or more, and preferably 8.0 or more from the viewpoint of affecting the taste of the product. It is more preferable, and it is usually 10.0 or less, preferably 9.0 or less. The pH can be adjusted by controlling the amount of the pH adjuster added. In addition to the above pH value, the pH value in the present specification is a value measured at a measurement temperature of 22 ° C.
 上記の測定温度22℃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、その上清液を測定する。
 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。
For the pH of the composition at the above measurement temperature of 22 ° C., use a pH analyzer (for example, manufactured by HORIBA, Ltd .: LAQUA F-72 flat ISFET pH electrode), add 20 ml of water to 2 g of the composition, and shake for 10 minutes. , Measure the supernatant.
For equipment calibration, for example, phthalic acid pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all by Wako Pure Chemical Industries, Ltd.) Perform a 3-point calibration using.
(組成物の流動性)
 上述したように、本明細書では、組成物の流動性を、測定温度22℃における垂直応力5kPaでの剪断応力で表す。使用者がパウチ製品を口に入れ、口内壁と歯茎との間や、口内壁と舌下との間に入れた場合における、パウチ製品にかかる圧力は通常垂直応力3~7kPaとなるため、5kPaの垂直応力を採用する。該剪断応力は、流動性又は/及び付着性の改善の観点から、通常5.99kPa以下であり、5.93kPa以下であることが好ましく、また、通常5.02kPa以上であり、5.13kPa以上であることが好ましく、5.42kPa以上であることがより好ましい。該剪断応力は、アニオン天然多糖類(ペクチン)およびCaイオンの配合で増加/減少させることができる。
(Fluidity of composition)
As described above, in the present specification, the fluidity of the composition is represented by the shear stress at a normal stress of 5 kPa at a measurement temperature of 22 ° C. When the user puts the pouch product in the mouth and puts it between the inner wall of the mouth and the gums or between the inner wall of the mouth and the sublingual area, the pressure applied to the pouch product is usually 3 to 7 kPa, and therefore 5 kPa. Adopt the normal stress of. The shear stress is usually 5.99 kPa or less, preferably 5.93 kPa or less, and usually 5.02 kPa or more, 5.13 kPa or more, from the viewpoint of improving fluidity and / or adhesion. It is preferable that it is 5.42 kPa or more, and it is more preferable that it is 5.42 kPa or more. The shear stress can be increased / decreased by the combination of anionic natural polysaccharide (pectin) and Ca ion.
 上記の垂直応力5kPaでの組成物の剪断応力は、レオメーターを用いて測定することができる。例えば、レオメーターとしてフリーマンテクノロジー社製のパウダーレオメーターFT4を用いた場合、下記の測定条件で測定する。
・測定モード:stantard program (25mm_shear_9kPa)
・測定温度:22℃
・測定湿度:60%RH
・測定容器:内径25mmの円筒容器、容積10ml
・垂直荷重:3~9kPa
 測定原料をそれぞれ篩(1.18mm目開き)にかけ、粒子を細かく均一にしたものを測定サンプルとし、上記レオメーターの手順に沿って測定を行う。
The shear stress of the composition at a normal stress of 5 kPa can be measured using a rheometer. For example, when a powder rheometer FT4 manufactured by Freeman Technology Co., Ltd. is used as a rheometer, measurement is performed under the following measurement conditions.
-Measurement mode: standard program (25 mm_shear_9 kPa)
・ Measurement temperature: 22 ° C
-Measured humidity: 60% RH
-Measuring container: Cylindrical container with an inner diameter of 25 mm, volume 10 ml
・ Vertical load: 3-9kPa
Each of the measurement raw materials is sieved (1.18 mm mesh opening), and the finely uniform particles are used as a measurement sample, and the measurement is performed according to the procedure of the rheometer.
(組成物の付着性)
 上述したように、本明細書では、組成物の付着性を、測定温度22℃における垂直応力0kPaでの剪断応力で表す。垂直応力0kPaは、使用者がパウチ製品を口に入れてから唾液がしみこむ前において、パウチ製品を厚さ方向に潰す際の圧力、つまり、この厚さ方向以外に圧力がかかっていない状態を想定した数値である。該剪断応力は、流動性又は/及び付着性の改善の観点から、通常1.83kPa以下であり、1.78kPa以下であることが好ましく、また、通常0.88kPa以上であり、1.12kPa以上であることが好ましく、1.26kPa以上であることがより好ましい。該剪断率は、アニオン天然多糖類(ペクチン)およびCaイオンの配合で増加/減少させることができる。
(Adhesion of composition)
As described above, in the present specification, the adhesiveness of the composition is represented by the shear stress at a normal stress of 0 kPa at a measurement temperature of 22 ° C. The normal stress of 0 kPa assumes the pressure at which the pouch product is crushed in the thickness direction after the user puts the pouch product in the mouth and before saliva soaks in, that is, no pressure is applied other than this thickness direction. It is a numerical value. The shear stress is usually 1.83 kPa or less, preferably 1.78 kPa or less, and usually 0.88 kPa or more, 1.12 kPa or more, from the viewpoint of improving fluidity and / or adhesion. It is preferably 1.26 kPa or more, and more preferably 1.26 kPa or more. The shear rate can be increased / decreased by the combination of anionic natural polysaccharide (pectin) and Ca ion.
 上記の流動性の測定と同様に、垂直応力3kPa、4kPa、5kPa、6kPa、7kPaでの組成物の剪断応力を測定し、垂直応力を横軸に、剪断応力を縦軸にプロットしグラフを作成する。剪断応力は垂直応力に対して線型的に変化するため、このグラフのフィッティングを行い、そのフィッティングの結果から垂直応力0kPaにおける剪断応力を算出する。フィッティングの条件を以下に示す。
 各垂直応力(3kPa、4kPa、5kPa、6kPa、7kPa)に対する剪断応力の各値から、計算により1次線形の回帰直線が導かれる。その傾きおよびY切片の値を算出する。算出されたY切片の値を垂直応力0kPaにおける剪断応力とする。
Similar to the above fluidity measurement, the shear stress of the composition at normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa is measured, and the vertical stress is plotted on the horizontal axis and the shear stress is plotted on the vertical axis to create a graph. do. Since the shear stress changes linearly with respect to the normal stress, the fitting of this graph is performed, and the shear stress at a normal stress of 0 kPa is calculated from the fitting result. The fitting conditions are shown below.
A linear regression line is calculated from each value of the shear stress for each normal stress (3 kPa, 4 kPa, 5 kPa, 6 kPa, 7 kPa). Calculate the slope and the value of the Y-intercept. The calculated value of the Y-intercept is taken as the shear stress at a normal stress of 0 kPa.
(Flow Function)
 上記の付着性の評価において垂直応力0kPaにおける剪断応力を算出するために用いたフィッティングに係る1次線形にMohrの応力円のフィッティングを行い、最大主応力及び単軸崩壊強度を求め、単独崩壊強度に対する最大主応力の比率(最大主応力/単独崩壊強度)を算出し、Flow Functionを評価することができる。
 Flow Function(FF)は、その値が大きいほど流動性が高いことを示し、1.90以上であることが好ましく、1.95以上であることがより好ましく、2.0以上であることがさらに好ましく、また、通常7.0以下である。
(Flow Function)
In the above evaluation of adhesiveness, the Mohr stress circle was fitted linearly with respect to the fitting used to calculate the shear stress at a normal stress of 0 kPa, and the maximum principal stress and uniaxial collapse strength were obtained to obtain the single-axis collapse strength. The ratio of the maximum principal stress to the maximum principal stress (maximum principal stress / single decay strength) can be calculated, and the Flow Function can be evaluated.
The larger the value of Flow Function (FF), the higher the fluidity, and it is preferably 1.90 or more, more preferably 1.95 or more, and further preferably 2.0 or more. It is preferable, and is usually 7.0 or less.
(乾燥時の組成物の構成物の粒度)
 組成物の構成物(単に「組成物」とも称する)のサイズは、特段制限されないが、例えば、乾燥させた組成物の構成物が下記の分級の条件を充たすものであることが好ましい。
 乾燥した組成物は、以下の篩目を有する篩により分級されたものであることが好ましい。ユーザーの使用時の口触りの良さをはじめ、製造時の扱いやすさ、品質のばらつきを制御する観点から、通常15mmの篩目を有する篩を通過するもの(≦15mm)であり、10mmの篩目を有する篩を通過するもの(≦10mm)であることが好ましく、5mmの篩目を有する篩を通過するもの(≦5mm)であることがより好ましく、3.2mmの篩目を有する篩を通過するもの(≦3.2mm)であることがさらに好ましい。例えば、乾燥したゲル粒子の全てがXmmの篩目の篩を通過した場合、ゲル粒子の乾燥時の最大粒度がXmm以下であることを表す。
 上記の乾燥した組成物は、組成物を70℃~80℃、3時間程度保持して乾燥することにより得られる。
 組成物の最大粒度は、アニオン天然多糖類(ペクチン)およびCaイオンの配合や含有させる水分量により適宜増加/減少させることができる。
 流動性又は/及び付着性の改善の観点からは、乾燥時の組成物の粒度の下限を設定する必要はないが、パウチからの漏れを防ぐ観点から、乾燥時の組成物の最大粒度は、通常0.3μm以上である。
(Particle size of composition when dried)
The size of the composition of the composition (also simply referred to as "composition") is not particularly limited, but for example, it is preferable that the composition of the dried composition satisfies the following classification conditions.
The dried composition is preferably classified by a sieve having the following sieve mesh. From the viewpoint of controlling the ease of handling during manufacturing and the variation in quality, as well as the good texture when used by the user, it usually passes through a sieve having a mesh of 15 mm (≤15 mm), and a sieve of 10 mm. Those that pass through a sieve having a mesh (≦ 10 mm) are preferable, and those that pass through a sieve having a sieve of 5 mm (≦ 5 mm) are more preferable, and a sieve having a sieve of 3.2 mm is used. It is more preferable that the material passes through (≦ 3.2 mm). For example, when all of the dried gel particles have passed through a sieve of X mm, it means that the maximum particle size of the gel particles when dried is X mm or less.
The above-mentioned dried composition is obtained by holding the composition at 70 ° C. to 80 ° C. for about 3 hours and drying it.
The maximum particle size of the composition can be appropriately increased / decreased depending on the blending of the anionic natural polysaccharide (pectin) and Ca ion and the amount of water contained.
From the viewpoint of improving fluidity and / and adhesion, it is not necessary to set the lower limit of the particle size of the composition during drying, but from the viewpoint of preventing leakage from the pouch, the maximum particle size of the composition during drying is set. It is usually 0.3 μm or more.
[パウチ]
 パウチ(包装材)は、上記の組成物を包装することができ、水に溶解しないものであり、かつ、液体(水や唾液等)や組成物中の水溶性成分の透過性を有すれば、特段制限されず、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、その中に上記の組成物を投入し、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。
 上記のシートの坪量は、特段制限されず、通常12gsm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。
[Pouch]
The pouch (packaging material) is capable of packaging the above composition, is insoluble in water, and is permeable to liquids (water, saliva, etc.) and water-soluble components in the composition. , There is no particular limitation, and known ones can be used. Examples of the material of the pouch include a cellulosic non-woven fabric, and a commercially available non-woven fabric may be used. A pouch product can be produced by forming a sheet made of such a material into a bag shape, putting the above composition into the bag, and sealing the sheet by means such as heat sealing.
The basis weight of the above sheet is not particularly limited, and is usually 12 gsm or more and 54 gsm or less, and preferably 24 gsm or more and 30 gsm or less.
The thickness of the above sheet is not particularly limited, and is usually 100 μm or more and 300 μm or less, and preferably 175 μm or more and 215 μm or less.
 パウチの内面及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ものである。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。なお、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、シリコン系樹脂又はエポキシ系樹脂等の撥水作用を有するものであればよい。 A water-repellent material may be partially applied to at least one of the inner surface and the outer surface of the pouch. A water-repellent fluororesin is suitable as the water-repellent material. Specifically, examples of this type of water-repellent fluororesin include Asahi Guard (registered trademark) manufactured by Asahi Glass Co., Ltd. The water-repellent fluororesin is applied to packaging materials for foods and products containing oils and fats such as confectionery, dairy products, prepared foods, fast foods and pet foods, for example. Therefore, this type of water-repellent fluororesin is safe even when applied to a pouch placed in the oral cavity. The water-repellent material is not limited to the fluorine-based resin, and may be any material having a water-repellent action such as a paraffin resin, a silicon-based resin, or an epoxy-based resin.
 パウチは、任意の成分を含んでいてよく、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、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特段制限されず、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。
 さらに、パウチの外観も特段制限されず、非透明なものだけでなく、半透明や透明なものであってもよく、この場合には、パウチに包装される組成物が透けて見える。
The pouch may contain any component, and examples thereof include raw materials for adjusting aroma and taste, flavors, additives, tobacco extracts, pigments and the like. Further, the mode in which these components are contained is not particularly limited, and examples thereof include a mode in which the pouch surface is coated or impregnated, and in the case of a fiber, the fiber is contained.
Further, the appearance of the pouch is not particularly limited, and it may be translucent or transparent as well as non-transparent, in which case the composition packaged in the pouch can be seen through.
[パウチ製品]
 パウチ製品は、上記の組成物と、該組成物を包装する上記のパウチとを有するもの(上記のパウチに上記の組成物を封入したもの)であれば、特段制限されない。
 パウチ製品のサイズや重量は、特段制限されず、使用前のパウチ製品のサイズは、長辺が25mm以上(例えば、28mm、35mm、38mm)、40mm以下としてもよく、28mm以上、38mm以下としてもよく、短辺が10mm以上、20mm以下であってもよく、14mm以上、18mm以下であってもよい。また、使用前のパウチ製品の重量は、0.1g以上、2.0g以下としてもよく、0.3g以上、1.0g以下としてもよい。
 パウチ製品の全重量に対する組成物の重量の割合は、特段制限されないが、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。
[Pouch products]
The pouch product is not particularly limited as long as it has the above composition and the above pouch for packaging the composition (the above pouch is encapsulated with the above composition).
The size and weight of the pouch product are not particularly limited, and the size of the pouch product before use may be 25 mm or more (for example, 28 mm, 35 mm, 38 mm) or 40 mm or less on the long side, or 28 mm or more and 38 mm or less. The short side may be 10 mm or more and 20 mm or less, and may be 14 mm or more and 18 mm or less. The weight of the pouch product before use may be 0.1 g or more and 2.0 g or less, or 0.3 g or more and 1.0 g or less.
The ratio of the weight of the composition to the total weight of the pouch product is not particularly limited, but is usually 80% by weight or more, preferably 85% by weight or more, more preferably 90% by weight or more, and more preferably 90% by weight or more. It is usually 99% by weight or less, preferably 97% by weight or less, and more preferably 95% by weight or less.
 本明細書における各特性の測定では、測定前に、測定する環境と同様の環境に測定サンプルを48時間以上保持する。また、測定温度、測定湿度、及び測定圧力については、特段特定されていない場合には、常温(22±2℃)、常湿(60±5%RH)、及び常圧(大気圧)とする。 In the measurement of each characteristic in the present specification, the measurement sample is held in the same environment as the measurement environment for 48 hours or more before the measurement. Unless otherwise specified, the measured temperature, measured humidity, and measured pressure shall be normal temperature (22 ± 2 ° C), normal humidity (60 ± 5% RH), and normal pressure (atmospheric pressure). ..
<ニコチン供給オーラルパウチ製品の製造方法>
 本発明の別の実施形態であるニコチン供給オーラルパウチ製品の製造方法(単に「ニコチン供給オーラルパウチ製品の製造方法」、又は「製造方法」とも称する)は、少なくともアニオン天然ポリマー炭水化物、カルシウムイオン供給剤、及び水を含むゲル粒子を含む組成物を製造する組成物製造工程を有し、
 該組成物がニコチンを含み、かつ、
 該組成物中の水の含有率が、15重量%以上である、ニコチン供給オーラルパウチ製品の製造方法である。
<Manufacturing method of nicotine-supplied oral pouch products>
Another embodiment of the present invention, which is a method for producing a nicotine-supplied oral pouch product (also simply referred to as "a method for producing a nicotine-supplied oral pouch product" or "a method for producing"), is at least an anionic natural polymer carbohydrate, a calcium ion feeder. , And a composition manufacturing process for producing a composition containing gel particles containing water.
The composition contains nicotine and
A method for producing a nicotine-supplied oral pouch product, wherein the content of water in the composition is 15% by weight or more.
[組成物製造工程]
 上記の組成物製造工程は、上記の組成物を製造できれば特段制限されない。該組成物の製造方法の一例を以下に示す。以下で示す各原料は、上述した各原料を用いることができる。
 まず、ペクチン等のアニオン天然ポリマー炭水化物、安定化ニコチン化合物等のニコチン供給源、セルロース等の基材、二酸化ケイ素等の白色剤を混合して混合物(カルシウム供給源添加前混合物)を得る(カルシウム供給源添加前混合物作製工程)。その後、乳酸カルシウム等のカルシウム供給源を含む水溶液、及び無水リン酸ナトリウム等のpH調整剤を含む水溶液を添加(例えば、噴霧による添加)し、これらを混合して混合物(加熱前混合物)を得る(加熱前混合物作製工程)。
 カルシウム供給源は、水溶液として供給しても、固体として供給してもよいが、水溶液等の液体として供給した場合には、カルシウムをカルシウムイオンの状態で他の原料と混合することができ、固体で供給するよりもアニオン天然ポリマー炭水化物との接触効率が高くなる観点から、水溶液として供給することが好ましい。また、カルシウム供給源は、上述のように、アニオン天然ポリマー炭水化物を含む混合物を作製した後に添加しても、最初にアニオン天然ポリマー炭水化物とともに混合してもよいが、微細で均一なゲル粒子を生成させる観点から、アニオン天然ポリマー炭水化物を含む混合物を作製した後に添加する態様が好ましい。一方で、水溶液にした際に粘度が上昇するので取り扱いの観点から、ペクチン等のアニオン天然ポリマー炭水化物を水溶液として用いることは好ましくない。
 カルシウム供給源添加前混合物作製工程後の各水溶液の添加において、所望の水分量を得るため、各水溶液とともに水を添加してもよい。
 また、アニオン天然ポリマー炭水化物を事前に十分に溶解させる観点から、以下の加熱工程(ゲル粒子の形成工程)前に混合物に十分な量の水を取り込ませることが好ましく、例えば、上記の加熱前混合物作製工程完了後の時点で、混合物の含水率が10重量%以上、50重量%以下であることが好ましく、20重量%以上、40重量%以下であることがより好ましい。
 加熱前混合物は、pH調整がされていることが好ましく、例えば、リン酸二水素ナトリウム等のpH調整剤により、加熱前混合物が酸性になるように添加量を調整することが好ましい。具体的には、加熱前混合物のpHを、3.0以上、6.0以下であることが好ましく、4.0以上、6.0以下であることがより好ましい。
 本工程において、pHを6.0以下に調整することにより、加熱前混合物中に含まれるニコチンを安定な状態で保持しつつ加熱の行程に進めることができる。
[Composition manufacturing process]
The above composition manufacturing process is not particularly limited as long as the above composition can be produced. An example of a method for producing the composition is shown below. As each raw material shown below, each of the above-mentioned raw materials can be used.
First, an anionic natural polymer carbohydrate such as pectin, a nicotine source such as a stabilized nicotine compound, a base material such as cellulose, and a white agent such as silicon dioxide are mixed to obtain a mixture (mixture before addition of a calcium source) (calcium supply). Mixture preparation step before source addition). Then, an aqueous solution containing a calcium source such as calcium lactate and an aqueous solution containing a pH adjuster such as anhydrous sodium phosphate are added (for example, added by spraying), and these are mixed to obtain a mixture (mixture before heating). (Mixture preparation step before heating).
The calcium supply source may be supplied as an aqueous solution or a solid, but when supplied as a liquid such as an aqueous solution, calcium can be mixed with other raw materials in the form of calcium ions and is a solid. It is preferable to supply it as an aqueous solution from the viewpoint of higher contact efficiency with the anionic natural polymer calcium than to supply it with. Also, as described above, the calcium source may be added after making the mixture containing the anionic natural polymer carbohydrates or may be mixed first with the anionic natural polymer carbohydrates, producing fine and uniform gel particles. From the viewpoint of allowing the mixture to be added, it is preferable to add the mixture after preparing the mixture containing the anionic natural polymer carbohydrate. On the other hand, it is not preferable to use an anionic natural polymer carbohydrate such as pectin as an aqueous solution from the viewpoint of handling because the viscosity increases when it is made into an aqueous solution.
In the addition of each aqueous solution after the step of preparing the mixture before the addition of the calcium source, water may be added together with each aqueous solution in order to obtain a desired water content.
Further, from the viewpoint of sufficiently dissolving the anionic natural polymer carbohydrate in advance, it is preferable to allow the mixture to take in a sufficient amount of water before the following heating step (gel particle forming step), for example, the above-mentioned preheating mixture. At the time after the completion of the production step, the water content of the mixture is preferably 10% by weight or more and 50% by weight or less, and more preferably 20% by weight or more and 40% by weight or less.
The pH of the pre-heating mixture is preferably adjusted, and the amount added is preferably adjusted so that the pre-heating mixture becomes acidic, for example, with a pH adjusting agent such as sodium dihydrogen phosphate. Specifically, the pH of the preheating mixture is preferably 3.0 or more and 6.0 or less, and more preferably 4.0 or more and 6.0 or less.
By adjusting the pH to 6.0 or less in this step, it is possible to proceed to the heating process while maintaining the nicotine contained in the preheating mixture in a stable state.
 上記の加熱前混合物を加熱し、アニオン天然ポリマー炭水化物を水和させ、アニオン天然ポリマー炭水化物とカルシウムイオンとの接触を促進することにより、ゲル粒子を作製し、ゲル粒子を含む混合物(ゲル粒子含有混合物)を得る(加熱工程)。
 加熱工程における加熱の方法は、特段制限されず、例えば、上記混合物を保持するミキサーのジャケット温度を上げる方法(ジャケット加熱)、および上記混合物の内部へ蒸気を注入する方法の一方または両方が挙げられる。加熱時の混合物の温度は、特段制限されないが、アニオン天然ポリマー炭水化物を効率よく水和させる観点から、60℃以上、90℃以下であることが好ましく、70℃以上、80℃以下であることがより好ましい。また、加熱時間は、特段制限されないが、アニオン天然ポリマー炭水化物とCaイオンを効率よく反応させる観点、および組成物中の水分を適宜調節する観点から、1時間以上、3時間以下であることが好ましく、1時間以上、2時間以下であることがより好ましい。
Gel particles are prepared by heating the above preheating mixture to hydrate the anionic natural polymer carbohydrates and promote contact between the anionic natural polymer carbohydrates and calcium ions, and the mixture containing the gel particles (gel particle-containing mixture). ) (Heating step).
The heating method in the heating step is not particularly limited, and examples thereof include one or both of a method of raising the jacket temperature of the mixer holding the mixture (jacket heating) and a method of injecting steam into the inside of the mixture. .. The temperature of the mixture during heating is not particularly limited, but is preferably 60 ° C. or higher and 90 ° C. or lower, and 70 ° C. or higher and 80 ° C. or lower, from the viewpoint of efficiently hydrating the anionic natural polymer carbohydrate. More preferred. The heating time is not particularly limited, but is preferably 1 hour or more and 3 hours or less from the viewpoint of efficiently reacting the anionic natural polymer carbohydrate with Ca ions and appropriately adjusting the water content in the composition. More preferably, it is 1 hour or more and 2 hours or less.
 上記の加熱工程の後、上記の混合物を乾燥する処理を行ってもよい(乾燥工程)。その後、冷却する処理を行ってもよい。冷却は自然冷却でもよいし、何らかの冷却手段を用いて行ってもよい(冷却工程)。乾燥を行うことで、例えば上記の混合物の含水量を5~45重量%に調整することができる。これにより、目的物としての組成物における含水量の調整が容易になる。 After the above heating step, a process of drying the above mixture may be performed (drying step). After that, a cooling process may be performed. The cooling may be natural cooling or may be performed by using some cooling means (cooling step). By performing drying, for example, the water content of the above mixture can be adjusted to 5 to 45% by weight. This facilitates the adjustment of the water content in the composition as the target product.
 上記の加熱工程(又は乾燥工程、冷却工程)で得られたゲル粒子含有混合物に、さらに、炭酸カリウム等のpH調整剤を含む水溶液を添加する。
 炭酸カリウム等のpH調整剤により、加熱後混合物がアルカリ性になるように添加量を調整することが好ましく、具体的には、加熱前混合物のpHを、6.0以上、10.0以下であることが好ましく、8.0以上、9.0以下であることがより好ましい。
 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し(ゲル粒子含有混合物への添加剤添加工程)、所望の組成物を得る。
 なお上記の添加物等を添加する際には、固体でもよいし水に溶解した水溶液での添加でもよい。水溶液で添加する場合は、パウチ製品の最終水分含量になるように予め所定量の水に溶解して添加してもよい。
An aqueous solution containing a pH adjuster such as potassium carbonate is further added to the gel particle-containing mixture obtained in the above heating step (or drying step, cooling step).
It is preferable to adjust the addition amount with a pH adjuster such as potassium carbonate so that the mixture after heating becomes alkaline. Specifically, the pH of the mixture before heating is 6.0 or more and 10.0 or less. It is preferable, and it is more preferable that it is 8.0 or more and 9.0 or less.
A sweetening agent such as acesulfame potassium, a fragrance such as menthol, a bitterness inhibitor such as soybean lecithin, and a moisturizer such as glycerin are added (step of adding an additive to a gel particle-containing mixture) to obtain a desired composition.
When the above additives and the like are added, they may be solid or added in an aqueous solution dissolved in water. When added as an aqueous solution, it may be added by dissolving it in a predetermined amount of water in advance so as to have the final water content of the pouch product.
[包装工程]
 上記の組成物作製工程で得られた組成物を包装剤で包装しパウチ製品を得る(包装工程)。包装する方法は特段制限されず、公知の方法を適用することができ、例えば、袋形状の不織布に上記の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、包装剤に組成物を投入した後、包装剤をシールした後において、所望の水分含有率を有する組成物を得るため、さらに水を加えてもよい(水添加工程)。例えば、目的の組成物の水の含有率が50重量%であり、上記の組成物作製工程で得られた組成物の水の含有率が15重量%である場合、残りの35重量%分の水を添加する。
[Packaging process]
The composition obtained in the above composition manufacturing step is packaged with a packaging agent to obtain a pouch product (packaging step). The packaging method is not particularly limited, and a known method can be applied. For example, a known method such as a method of putting the above composition into a bag-shaped non-woven fabric and then sealing it can be used.
In the packaging step, after the composition is added to the packaging agent and the packaging agent is sealed, water may be further added in order to obtain a composition having a desired water content (water addition step). For example, when the water content of the target composition is 50% by weight and the water content of the composition obtained in the above composition preparation step is 15% by weight, the remaining 35% by weight Add water.
<パウチ製品の用途>
 パウチ製品の用途(使用態様)は、特段制限されないが、例えば、かみたばこやかぎたばこ、圧縮たばこ等の口腔用たばこ、またはニコチンパウチといわれる、ニコチン含有製剤等が挙げられる。これらは、口腔内で唇と歯茎の間に挿入し、味や香りを愉しむものである。
<Use of pouch products>
The use (use mode) of the pouch product is not particularly limited, and examples thereof include oral tobacco such as chewing tobacco, snuff tobacco, and compressed tobacco, and nicotine-containing preparations called nicotine pouches. These are inserted between the lips and gums in the oral cavity to enjoy the taste and aroma.
 以下、実施例を示して本発明について更に具体的に説明する。ただし、本発明は以下の実施例に限定して解釈されるものではない。 Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not construed as being limited to the following examples.
<実験1>
[組成物の作製]
(実施例1)
 ペクチン 75.0g(H&F社製のClassic CU902)、ニコチンポラクリレックス 680.0g(Contraf nicotex社製のNicotine Polacrilex 20%)、セルロース 2175g(J.RETTENMAIER & SOHNE社製の VITACEL L600-30)、二酸化ケイ素(シリカ) 75.0g(富士シリシア株式会社製のSYLOPAGE 720)を混合した後、該混合物に乳酸カルシウム水溶液 35.3g(太平化学産業株式会社製の乳酸カルシウム(顆粒))、及び無水リン酸ナトリウム水溶液 302.1g(Univar B.V. 社製の Monosodium phosphate anhydrous, FG (MSP A FG))、を添加し、これらを均一になるまで混合してpH6.2の混合物A(含水率23.5重量%)を得た。
 得られた混合物Aを、ジャケット加熱(缶壁温度100℃)を原料の品温が70℃~80℃となるように1時間行った(加熱後の含水量は6.2重量%、pHは6.0(上記で説明したたばこ充填物の場合と同じ測定法により測定))。その後、周囲温度が20℃となる条件下で1時間冷却し、混合物B(冷却後のpHは6.2)を得た。
 冷却して得られた混合物Bに、炭酸カリウム水溶液 256.1g(Univar B.V. 製のPOTASSIUM CARBONATE)を添加し、混合物Cを得た。
 最後に、含水率を調整するために、水 0gを混合物Cに添加し(つまり、水の追加添加なし)、実施例1の組成物1(含水率15.10重量%、pH7.8) 200gを得た。
<Experiment 1>
[Preparation of composition]
(Example 1)
Pectin 75.0 g (H & F Classic CU902), Nicotin Polacrilex 680.0 g (Contraf nicotex Nicotine Polacrilex 20%), Cellulose 2175 g (J.RETTENMAIER & SOHNE VITACEL L600-30), Dioxide After mixing 75.0 g of silicon (silica) (SYLOPAGE 720 manufactured by Fuji Silysia Chemical Ltd.), 35.3 g of an aqueous calcium lactate solution (calcium lactate (granule) manufactured by Taihei Kagaku Sangyo Co., Ltd.) and anhydrous phosphate are added to the mixture. 302.1 g of an aqueous sodium solution (Monosodium phosphate formula, FG (MSP A FG) manufactured by Univar BV) was added, and these were mixed until uniform, and the mixture A (moisture content 23.5% by weight) having a pH of 6.2 was added. ) Was obtained.
The obtained mixture A was jacket-heated (can wall temperature 100 ° C.) for 1 hour so that the product temperature of the raw material was 70 ° C. to 80 ° C. (water content after heating was 6.2% by weight, pH was 6.0 (measured by the same measurement method as for the tobacco filling described above). Then, the mixture was cooled for 1 hour under the condition that the ambient temperature was 20 ° C. to obtain a mixture B (pH after cooling was 6.2).
256.1 g of an aqueous potassium carbonate solution (POTASSIUM CARBONATE manufactured by Univar BV) was added to the mixture B obtained by cooling to obtain a mixture C.
Finally, in order to adjust the water content, 0 g of water was added to the mixture C (that is, no additional water was added), and 200 g of the composition 1 of Example 1 (water content 15.10% by weight, pH 7.8). Got
(実施例2)
 上記の組成物1において、混合物Cへの水の添加量を0gから1.71gに変更したこと以外は組成物1と同様の方法で、実施例2の組成物2(含水率18.47重量%)を100g作製した。
(Example 2)
In the above composition 1, the composition 2 (moisture content 18.47 weight) of Example 2 was carried out in the same manner as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 1.71 g. %) Was produced in an amount of 100 g.
(実施例3)
 上記の組成物1において、混合物Cへの水の添加量を0gから42.57gに変更したこと以外は組成物1と同様の方法で、実施例3の組成物3(含水率32.06重量%)を200g作製した。
(Example 3)
In the above composition 1, the same method as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 42.57 g, and the composition 3 of Example 3 (moisture content 32.06 weight). %) Was produced in an amount of 200 g.
(実施例4)
 上記の組成物1において、混合物Cへの水の添加量を0gから108.73gに変更したこと以外は組成物1と同様の方法で、実施例4の組成物4(含水率46.98重量%)を200g作製した。
(Example 4)
In the above composition 1, the composition 4 (moisture content 46.98 weight) of Example 4 was carried out in the same manner as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 108.73 g. %) Was produced in an amount of 200 g.
(実施例5)
 上記の組成物1において、混合物Cへの水の添加量を0gから66.80gに変更したこと以外は組成物1と同様の方法で、実施例5の組成物5(含水率52.49重量%)を100g作製した。
(Example 5)
In the above composition 1, the composition 5 (moisture content 52.49 weight) of Example 5 was carried out in the same manner as in composition 1 except that the amount of water added to the mixture C was changed from 0 g to 66.80 g. %) Was produced in an amount of 100 g.
(比較例1)
 上記の組成物1において、ペクチン及び乳酸カルシウム水溶液を添加しなかったこと、及び混合物Cへの水の添加量を0gから3.46gに変更したこと以外は組成物1と同様の方法で、比較例1の組成物6(含水率18.18重量%、pH7.8)を100g作製した。
(Comparative Example 1)
In the above composition 1, comparison was made in the same manner as in composition 1 except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to the mixture C was changed from 0 g to 3.46 g. 100 g of the composition 6 of Example 1 (moisture content 18.18% by weight, pH 7.8) was prepared.
(比較例2)
 上記の組成物1において、ペクチン及び乳酸カルシウム水溶液を添加しなかったこと、及び混合物Cへの水の添加量を0gから43.00gに変更したこと以外は組成物1と同様の方法で、比較例2の組成物7(含水率31.46重量%)を200g作製した。
(Comparative Example 2)
In the above composition 1, comparison was made in the same manner as in composition 1 except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to the mixture C was changed from 0 g to 43.00 g. 200 g of the composition 7 of Example 2 (moisture content 31.46% by weight) was prepared.
(比較例3)
 上記の組成物1において、ペクチン及び乳酸カルシウム水溶液を添加しなかったこと、及び混合物Cへの水の添加量を0gから109.27gに変更したこと以外は組成物1と同様の方法で、比較例3の組成物8(含水率46.60重量%)を200g作製した。
(Comparative Example 3)
In the above composition 1, comparison was made in the same manner as in composition 1 except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to the mixture C was changed from 0 g to 109.27 g. 200 g of the composition 8 (moisture content 46.60% by weight) of Example 3 was prepared.
[特性評価]
(含水率)
 各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)を用いて測定した。
・測定モード:FAST
・到達温度(安定時):100℃
・測定終了条件:AUTO60(60秒で1mg以下の変化量)
・結果表示:Moisture%
[Characteristic evaluation]
(Moisture content)
The water content (moisture content) of each composition was measured using a heat-drying moisture meter (for example, manufactured by METTER TOLEDO: HB 43-S).
・ Measurement mode: FAST
-Achieved temperature (when stable): 100 ° C
-Measurement end condition: AUTO60 (change amount of 1 mg or less in 60 seconds)
・ Result display: Moisture%
(pH)
 測定温度22℃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)を用いて測定した。
 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)
The pH of the composition at a measurement temperature of 22 ° C. was measured using a pH analyzer (for example, manufactured by HORIBA, Ltd .: LAQUA F-72 flat ISFET pH electrode).
For equipment calibration, for example, phthalic acid pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18) (all by Wako Pure Chemical Industries, Ltd.) It was performed by 3-point calibration using.
(流動性)
 垂直応力5kPaでの組成物の剪断応力は、レオメーターとしてフリーマンテクノロジー社製のパウダーレオメーターFT4を用い、下記の測定条件で測定し、垂直応力5kPaにおける剪断応力を採用した。
・測定モード:stantard program (25mm_shear_9kPa)
・測定温度:22℃
・測定湿度:60%RH
・測定容器:内径25mmの円筒容器、容積10ml
・垂直応力:3~9kPa
 測定原料をそれぞれ篩(1.18mm目開き)にかけ、粒子を細かく均一にしたものを測定サンプルとし、上記レオメーターの手順に沿って測定を行った。
(Liquidity)
The shear stress of the composition at a normal stress of 5 kPa was measured using a powder rheometer FT4 manufactured by Freeman Technology Co., Ltd. as a rheometer under the following measurement conditions, and the shear stress at a normal stress of 5 kPa was adopted.
-Measurement mode: standard program (25 mm_shear_9 kPa)
・ Measurement temperature: 22 ° C
-Measured humidity: 60% RH
-Measuring container: Cylindrical container with an inner diameter of 25 mm, volume 10 ml
・ Normal stress: 3-9 kPa
Each of the measurement raw materials was sieved (1.18 mm mesh opening), and the particles were finely and uniformly used as a measurement sample, and the measurement was performed according to the procedure of the rheometer.
(付着性)
 上記の流動性の測定と同様に、垂直応力3kPa、4kPa、5kPa、6kPa、7kPaでの組成物の剪断応力を測定し、垂直応力を横軸に、剪断応力を縦軸にプロットしグラフを作成した。剪断応力は垂直応力に対して線型的に変化するため、このグラフのフィッティングを行い、そのフィッティングの結果から垂直応力0kPaにおける剪断応力を算出した。フィッティングの条件を以下に示す。
 各垂直応力(3kPa、4kPa、5kPa、6kPa、7kPa)に対する剪断応力の各値から、計算により1次線形の回帰直線が導かれる。その傾きおよびY切片の値を算出する。算出されたY切片の値を垂直応力0kPaにおける剪断応力とする。
(Adhesiveness)
Similar to the above fluidity measurement, the shear stress of the composition at normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa is measured, and the vertical stress is plotted on the horizontal axis and the shear stress is plotted on the vertical axis to create a graph. bottom. Since the shear stress changes linearly with respect to the normal stress, fitting of this graph was performed, and the shear stress at a normal stress of 0 kPa was calculated from the fitting result. The fitting conditions are shown below.
A linear regression line is calculated from each value of the shear stress for each normal stress (3 kPa, 4 kPa, 5 kPa, 6 kPa, 7 kPa). Calculate the slope and the value of the Y-intercept. The calculated value of the Y-intercept is taken as the shear stress at a normal stress of 0 kPa.
 上記の各組成物の原料の使用比率、及び各特性の評価結果を下記の表1にまとめる。なお、表1に記載の原料は、含有される全ての原料を示してはおらず、含有される原料の一部を示している。また、表に記載の原料の数値は、組成物中の各成分の含有率ではなく、仕込み量である。また、表1中の組成物中の最大粒度における「≦X」の表記は、乾燥時の組成物の最大粒度がX以下であることを意味する。
 また、表1中の「-」の表記は、無添加であることを示す。
 また、上記の付着性に記載の垂直応力3kPa、4kPa、5kPa、6kPa、7kPaでの組成物の剪断応力の測定結果を表2に示し、かつ、実施例2と比較例1(含水率約18重量%)、実施例3と比較例2(含水率約30重量%)、実施例4と比較例3(含水率約45重量%)のそれぞれ測定結果をプロットしたグラフを図1~3に示す。
Table 1 below summarizes the ratio of raw materials used in each of the above compositions and the evaluation results of each characteristic. The raw materials shown in Table 1 do not show all the raw materials contained, but show some of the raw materials contained. In addition, the numerical values of the raw materials shown in the table are not the content rate of each component in the composition but the amount charged. Further, the notation of "≦ X" in the maximum particle size of the composition in Table 1 means that the maximum particle size of the composition at the time of drying is X or less.
In addition, the notation of "-" in Table 1 indicates that no additive is added.
Table 2 shows the measurement results of the shear stress of the composition at the normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa described in the above-mentioned adhesiveness, and also shows Example 2 and Comparative Example 1 (moisture content of about 18). 13% by weight), Graphs in which the measurement results of Example 3 and Comparative Example 2 (moisture content of about 30% by weight) and Example 4 and Comparative Example 3 (moisture content of about 45% by weight) are plotted are shown in FIGS. ..
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
 上記の表1より、上記の実施形態の要件を充たす実施例1~5の組成物は、該要件を充たしていない比較例1~3の組成物よりも、5kPaの垂直応力時の剪断応力、及び0kPaの垂直応力時の剪断応力が低い、つまり、流動性及び付着性が向上していることが分かった。具体的には、ペクチンと乳酸カルシウム水溶液を併用することにより、流動性及び付着性が改善することが分かった。 From Table 1 above, the compositions of Examples 1 to 5 satisfying the requirements of the above embodiments have a shear stress at a normal stress of 5 kPa as compared with the compositions of Comparative Examples 1 to 3 not satisfying the requirements. It was also found that the shear stress at normal stress of 0 kPa was low, that is, the fluidity and adhesiveness were improved. Specifically, it was found that the combined use of pectin and an aqueous solution of calcium lactate improves fluidity and adhesiveness.
<実験2>
[組成物の作製]
(実施例1~5)
 実施例の組成物としては、上記の実施例1~5における組成物1~5を用いた。
<Experiment 2>
[Preparation of composition]
(Examples 1 to 5)
As the composition of the example, the compositions 1 to 5 in the above-mentioned Examples 1 to 5 were used.
(比較例4)
 上記の組成物1において、乳酸カルシウム水溶液を添加しなかったこと以外は組成物1と同様の方法で、比較例4の組成物9(含水率16.12重量%、pH7.8)を200g作製した。
(Comparative Example 4)
In the above composition 1, 200 g of the composition 9 (moisture content 16.12% by weight, pH 7.8) of Comparative Example 4 was prepared by the same method as that of the composition 1 except that the calcium lactate aqueous solution was not added. bottom.
(比較例5)
 上記の組成物1において、乳酸カルシウム水溶液を添加しなかったこと、及び混合物Cへの水の添加量を0gから105.33gに変更したこと以外は組成物1と同様の方法で、比較例5の組成物10(含水率47.06重量%)を200g作製した。
(Comparative Example 5)
Comparative Example 5 in the same manner as in Composition 1 except that the calcium lactate aqueous solution was not added and the amount of water added to the mixture C was changed from 0 g to 105.33 g in the above composition 1. 200 g of the composition 10 (moisture content 47.06% by weight) was prepared.
(比較例6)
 上記の組成物1において、乳酸カルシウム水溶液を添加しなかったこと、及び混合物Cへの水の添加量を0gから86.09gに変更したこと以外は組成物1と同様の方法で、比較例6の組成物11(含水率55.97重量%)を100g作製した。
(Comparative Example 6)
In Comparative Example 6 in the same manner as in Composition 1 except that the calcium lactate aqueous solution was not added and the amount of water added to the mixture C was changed from 0 g to 86.09 g in the above composition 1. The composition 11 (moisture content 55.97% by weight) of the above was prepared in an amount of 100 g.
[特性評価]
 上記の各組成物に対して、上記の実験1と同様の特性評価を行った。この特性の評価結果を下記表3に示す。なお、表3に記載の原料は、含有される全ての原料を示してはおらず、含有される原料の一部を示している。また、表に記載の原料の数値は、組成物中の各成分の含有率ではなく、仕込み量である。また、表3中の組成物中の最大粒度における「≦X」の表記は、乾燥時の組成物の最大粒度がX以下であることを意味する。
 また、上記の付着性に記載の垂直応力3kPa、4kPa、5kPa、6kPa、7kPaでの組成物の剪断応力の測定結果を表4に示し、かつ、実施例1と比較例4(含水率約15重量%)、実施例4と比較例5(含水率約45重量%)、実施例5と比較例6(含水率約50重量%)のそれぞれ測定結果をプロットしたグラフを図4~6に示す。
[Characteristic evaluation]
The characteristics of each of the above compositions were evaluated in the same manner as in Experiment 1 above. The evaluation results of this characteristic are shown in Table 3 below. The raw materials shown in Table 3 do not show all the raw materials contained, but show some of the raw materials contained. In addition, the numerical values of the raw materials shown in the table are not the content rate of each component in the composition but the amount charged. Further, the notation of “≦ X” in the maximum particle size of the composition in Table 3 means that the maximum particle size of the composition at the time of drying is X or less.
Table 4 shows the measurement results of the shear stress of the composition at the normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa described in the above-mentioned adhesiveness, and Example 1 and Comparative Example 4 (moisture content of about 15). Figures 4 to 6 plot the measurement results of Example 4 and Comparative Example 5 (water content of about 45% by weight), and Example 5 and Comparative Example 6 (water content of about 50% by weight). ..
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
 上記の表3より、上記の実施形態の要件を充たす実施例1~5の組成物は、該要件を充たしていない比較例4~6の組成物よりも、5kPaの垂直応力時の剪断応力、及び0kPaの垂直応力時の剪断応力が低い、つまり、流動性及び付着性が向上していることが分かった。具体的には、乳酸カルシウム水溶液を使用することにより、流動性及び付着性が改善することが分かった。
 さらに、上記の実験1における表1も考慮すると、組成物の含水率が約45重量%である実施例4、比較例2、比較例5の組成物の比較から、この順番で5kPaの垂直応力時の剪断応力、及び0kPaの垂直応力時の剪断応力が高くなっていることが分かる。つまり、ペクチンの添加により流動性及び付着性が改善し、さらに、乳酸カルシウム水溶液の添加により流動性及び付着性がさらに改善することが分かった。
From Table 3 above, the compositions of Examples 1 to 5 satisfying the requirements of the above embodiments have a shear stress at a normal stress of 5 kPa as compared with the compositions of Comparative Examples 4 to 6 not satisfying the requirements. It was also found that the shear stress at normal stress of 0 kPa was low, that is, the fluidity and adhesiveness were improved. Specifically, it was found that the fluidity and adhesiveness were improved by using an aqueous solution of calcium lactate.
Further, considering Table 1 in Experiment 1 above, from the comparison of the compositions of Example 4, Comparative Example 2 and Comparative Example 5 in which the water content of the composition is about 45% by weight, the normal stress of 5 kPa is in this order. It can be seen that the shear stress at the time and the shear stress at the normal stress of 0 kPa are high. That is, it was found that the addition of pectin improved the fluidity and adhesiveness, and the addition of the calcium lactate aqueous solution further improved the fluidity and adhesiveness.
<実験3>
[組成物の作製]
(比較例4~6)
 本実験では、上記の比較例4~6を用いた。
<Experiment 3>
[Preparation of composition]
(Comparative Examples 4 to 6)
In this experiment, Comparative Examples 4 to 6 described above were used.
(比較例7)
 ペクチン 7.7g(H&F社製のClassic CU902)、ニコチンポラクリレックス 2.2g(Contraf nicotex社製のNicotine Polacrilex 20%)、微結晶セルロース 32.8g(Brenntag Nordic社製のHICEL 90M MCC)、炭酸ナトリウム 6.3g(UNIVAR社製のSODIUM CARBONATE ANHYDROUS)、マルチトール 41.2g(CALDIC NORDIC社製のC*Maltidex CH 16385)を均一になるまで混合して比較例7の組成物12(pH8.6、含水率7.0重量%)100gを得た。
 本比較例7は、上記の製造方法から分かるように、水溶液や水の添加、加熱処理を行っていない。上記の含水率で示される水は、上記各原料中に元々含まれている水に由来する。
(Comparative Example 7)
Pectin 7.7 g (H & F Classic CU902), Nicotine Polacrilex 2.2 g (Contraf nicotex Nicotine Polacrilex 20%), Microcrystalline Cellulose 32.8 g (Brenntag Nordic HICEL 90M MCC), Carbonate Sodium 6.3 g (SODIUM CARBONATE ANHYDROUS manufactured by UNIVAR) and 41.2 g (C * Maltidex CH 16385 manufactured by CALDIC NORDIC) were mixed until uniform, and the composition 12 (pH 8.6) of Comparative Example 7 was mixed. , Water content 7.0% by weight) 100 g was obtained.
As can be seen from the above production method, Comparative Example 7 is not subjected to addition of an aqueous solution or water, or heat treatment. The water indicated by the above water content is derived from the water originally contained in each of the above raw materials.
[特性評価]
(官能性評価)
 上記の比較例4~7の各組成物を、0.65g/個となるように不織布(BFF technical fabrics社製、坪量27.0g/m)に投入した後、ヒートシールでシールして密封することによりパウチ製品を作製し、官能評価を行った。官能評価は、以下の方法により行った。パウチ製品の官能評価の専門パネラー5名により、前記組成物を用いて作成したパウチを各々口に含んで、口触り、風味、満足度等の各種指標で良好なもの~好ましくないものの段階評価を行った。
[Characteristic evaluation]
(Evaluation of sensuality)
Each of the above compositions of Comparative Examples 4 to 7 was put into a non-woven fabric (manufactured by BFF technical fabrics, with a basis weight of 27.0 g / m 2 ) so as to be 0.65 g / piece, and then sealed with a heat seal. A pouch product was prepared by sealing and sensory evaluation was performed. The sensory evaluation was performed by the following method. Five panelists specializing in sensory evaluation of pouch products put pouches prepared using the above composition in their mouths, and graded evaluations of good to unfavorable items in various indicators such as texture, flavor, and satisfaction. went.
 上記の官能性評価の結果、水の添加(水溶液としての水の添加も含む)を行った比較例4、5、6と比較し、水の添加を行わなかった比較例7では、口に含んだ際の口腔内において、異物感があり、口が乾く感じがあり、また、唾液がなじみにくい、といった傾向がみられた。 As a result of the above functionality evaluation, it was compared with Comparative Examples 4, 5 and 6 in which water was added (including addition of water as an aqueous solution), and in Comparative Example 7 in which water was not added, it was contained in the mouth. In the oral cavity, there was a tendency for foreign substances to be felt, the mouth to be dry, and saliva to be difficult to get used to.
<実験4>
[組成物の作製]
(実施例6)
 セルロース 885g(J.RETTENMAIER & SOHNE社製の VITACEL L600-30)、ニコチンポラクリレックス 120.0g(Contraf nicotex社製のNicotine Polacrilex 20%)、たばこ粉 0.6g、リン酸二水素ナトリウム 339g(Fosfa社製のOMNISAL)、炭酸ナトリウム 282.0g(UNIVAR社製のSODIUM CARBONATE ANHYDROUS)、グリセリン脂肪酸エステル 87.0g(理研ビタミン社製のポエム DO-100V)、塩化ナトリウム 171g(Nouryon社製のSuprasel Classic)、乳酸カルシウム 45g(太平化学産業株式会社製の乳酸カルシウム(顆粒))、及び甘味料 66gを均一になるまで混合して混合物Dを得た。その後、得られた混合物Dに香料 84gを添加し、さらに、ジェランガム(三栄源エフ・エフ・アイ社製のケルコゲル) 7.5g、及び水 909gを添加して混合し、組成物13(含水率30.3重量%)を得た。
<Experiment 4>
[Preparation of composition]
(Example 6)
885 g of cellulose (VITACEL L600-30 manufactured by J.RETTENMAIER & SOHNE), 120.0 g of Nicotine Polacrilex (20% manufactured by Contraf nicotex), 0.6 g of tobacco powder, 339 g of sodium dihydrogen phosphate (Fosfa) OMNISAL), sodium carbonate 282.0 g (UNIVAR SODIUM CARBONATE ANHYDROUS), glycerin fatty acid ester 87.0 g (RIKEN Vitamin Poem DO-100V), sodium chloride 171 g (Nouryon Suprasel Classic) , 45 g of calcium lactate (calcium lactate (granule) manufactured by Taihei Kagaku Sangyo Co., Ltd.) and 66 g of sweetener were mixed until uniform to obtain a mixture D. Then, 84 g of the fragrance was added to the obtained mixture D, 7.5 g of gellan gum (Kercogel manufactured by Saneigen FFI) and 909 g of water were added and mixed, and the composition 13 (moisture content) was added. 30.3% by weight) was obtained.
(比較例8)
 セルロースの量を885gから888gに、また、リン酸二水素ナトリウムの量を339gから342gに変更したこと以外は実施例6と同様に混合物Dを作製した。その後、得られた混合物Dに香料 84gを添加し、さらに、水 912gを添加して混合し、組成物13(含水率30.3重量%)を得た。
(Comparative Example 8)
A mixture D was prepared in the same manner as in Example 6 except that the amount of cellulose was changed from 885 g to 888 g and the amount of sodium dihydrogen phosphate was changed from 339 g to 342 g. Then, 84 g of a fragrance was added to the obtained mixture D, and 912 g of water was further added and mixed to obtain a composition 13 (moisture content: 30.3% by weight).
 上記の各実施例の原料の配合をまとめたものを表5に示す。 Table 5 shows a summary of the composition of the raw materials of each of the above examples.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
[特性評価]
(流動性及び付着性)
 上記の各組成物に対して、測定容器の内径を25mmから50mmに、容積を10mlから85mlに変更したこと以外は上記の実験1と同様の方法で流動性及び付着性の評価を行った。この評価結果を下記表6及び図7に示す。ただし、剪断応力は、垂直応力3kPa、4kPa、5kPa、6kPaでの組成物の剪断応力を評価した。
[Characteristic evaluation]
(Liquidity and adhesion)
The fluidity and adhesiveness of each of the above compositions were evaluated in the same manner as in Experiment 1 above, except that the inner diameter of the measuring container was changed from 25 mm to 50 mm and the volume was changed from 10 ml to 85 ml. The evaluation results are shown in Table 6 and FIG. 7 below. However, as the shear stress, the shear stress of the composition at normal stresses of 3 kPa, 4 kPa, 5 kPa, and 6 kPa was evaluated.
Figure JPOXMLDOC01-appb-T000006
Figure JPOXMLDOC01-appb-T000006
 上記の表6及び図7より、上記の実施形態の要件を充たす実施例6の組成物は、該要件を充たしていない比較例8の組成物よりも、5kPaの垂直応力時の剪断応力、及び0kPaの垂直応力時の剪断応力が低い、つまり、流動性及び付着性が向上していることが分かった。具体的には、ジェランガムと乳酸カルシウム水溶液を併用する組成により、流動性及び付着性が改善することが分かった。
 また、実施例6~7が、比較例8と比較し、低い垂直応力における剪断応力が低いことが分かった。これは、低い垂直応力における粒子間の付着力の低減によるものと考えられる。
From Table 6 and FIG. 7 above, the composition of Example 6 satisfying the requirements of the above-described embodiment has a shear stress at a normal stress of 5 kPa and a shear stress at a normal stress of 5 kPa as compared with the composition of Comparative Example 8 not satisfying the requirements. It was found that the shear stress at the time of normal stress of 0 kPa was low, that is, the fluidity and adhesiveness were improved. Specifically, it was found that the composition in which gellan gum and the calcium lactate aqueous solution were used in combination improved the fluidity and adhesiveness.
Further, it was found that Examples 6 to 7 had lower shear stress at low normal stress as compared with Comparative Example 8. This is considered to be due to the reduction of the adhesive force between the particles at low normal stress.
[特性評価]
(Flow Function)
 上記の付着性の評価において垂直応力0kPaにおける剪断応力を算出するために用いたフィッティングに係る1次線形にMohrの応力円のフィッティングを行い、最大主応力及び単軸崩壊強度を求め、単独崩壊強度に対する最大主応力の比率(最大主応力/単独崩壊強度)を算出し、Flow Functionとして評価した。この評価結果を表7に示す。
[Characteristic evaluation]
(Flow Function)
In the above evaluation of adhesiveness, the Mohr stress circle was fitted linearly with respect to the fitting used to calculate the shear stress at a normal stress of 0 kPa, and the maximum principal stress and uniaxial collapse strength were obtained to obtain the single-axis collapse strength. The ratio of the maximum principal stress to the maximum principal stress (maximum principal stress / single decay strength) was calculated and evaluated as Flow Function. The evaluation results are shown in Table 7.
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000007
 上記の表7より、上記の実施形態の要件を充たす実施例6の組成物は、該要件を充たしていない比較例8の組成物よりも、流動性が高いことが分かった。 From Table 7 above, it was found that the composition of Example 6 satisfying the requirements of the above-described embodiment has higher fluidity than the composition of Comparative Example 8 not satisfying the requirements.
 以上に示す通り、本発明によれば、流動性が改善された、又は、付着性が改善されたニコチン供給オーラルパウチ製品、及びその製造方法を提供することができる。 As described above, according to the present invention, it is possible to provide a nicotine-supplied oral pouch product having improved fluidity or improved adhesiveness, and a method for producing the same.

Claims (9)

  1.  ゲル粒子を含む組成物と、該組成物を包装するパウチとを有するニコチン供給オーラルパウチ製品であって、
     該ゲル粒子が、少なくともアニオン天然ポリマー炭水化物、カルシウムイオン、及び水を含み、
     該組成物がニコチンを含み、
     該組成物中の水の含有率が15重量%以上である、
     ニコチン供給オーラルパウチ製品。
    A nicotine-supplied oral pouch product comprising a composition containing gel particles and a pouch for packaging the composition.
    The gel particles contain at least anionic natural polymer carbohydrates, calcium ions, and water.
    The composition comprises nicotine
    The content of water in the composition is 15% by weight or more.
    Nicotine-supplied oral pouch products.
  2.  前記アニオン天然ポリマー炭水化物が、カルボキシル基を有する、請求項1に記載のニコチン供給オーラルパウチ製品。 The nicotine-supplied oral pouch product according to claim 1, wherein the anionic natural polymer carbohydrate has a carboxyl group.
  3.  前記アニオン天然ポリマー炭水化物が、LMペクチンである、請求項2に記載のニコチン供給オーラルパウチ製品。 The nicotine-supplied oral pouch product according to claim 2, wherein the anionic natural polymer carbohydrate is LM pectin.
  4.  前記組成物において、前記アニオン天然ポリマー炭水化物が有する総カルボキシル基数と、前記カルシウムイオンの総個数との比が、100:1~2:1である、請求項3又は4に記載のニコチン供給オーラルパウチ製品。 The nicotine-supplied oral pouch according to claim 3 or 4, wherein in the composition, the ratio of the total number of carboxyl groups of the anionic natural polymer carbohydrate to the total number of calcium ions is 100: 1 to 2: 1. product.
  5.  前記組成物の構成物の乾燥時の最大粒度が、15mm以下である、請求項1~4のいずれか1項に記載のニコチン供給オーラルパウチ製品。 The nicotine-supplied oral pouch product according to any one of claims 1 to 4, wherein the maximum particle size of the composition of the composition when dried is 15 mm or less.
  6.  前記パウチが不織布である、請求項1~5のいずれか1項に記載のニコチン供給オーラルパウチ製品。 The nicotine-supplied oral pouch product according to any one of claims 1 to 5, wherein the pouch is a non-woven fabric.
  7.  少なくともアニオン天然ポリマー炭水化物、カルシウムイオン供給剤、及び水を含むゲル粒子を含む組成物を製造する組成物製造工程を有し、
     該組成物がニコチンを含み、かつ、
     該組成物中の水の含有率が、15重量%以上である、ニコチン供給オーラルパウチ製品の製造方法。
    It has a composition manufacturing process for producing a composition containing at least anionic natural polymer carbohydrates, a calcium ion feeder, and gel particles containing water.
    The composition contains nicotine and
    A method for producing a nicotine-supplied oral pouch product, wherein the content of water in the composition is 15% by weight or more.
  8.  前記カルシウムイオン供給剤が液体である、請求項7に記載のニコチン供給オーラルパウチ製品の製造方法。 The method for producing a nicotine-supplied oral pouch product according to claim 7, wherein the calcium ion feeder is a liquid.
  9.  前記カルシウムイオン供給剤が、乳酸カルシウムを含む、請求項7又は8に記載のニコチン供給オーラルパウチ製品の製造方法。 The method for producing a nicotine-supplied oral pouch product according to claim 7 or 8, wherein the calcium ion feeder contains calcium lactate.
PCT/JP2021/016101 2020-04-28 2021-04-20 Nicotine supply oral pouch product and production method therefor WO2021220898A1 (en)

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Publication number Priority date Publication date Assignee Title
EP3809884B1 (en) 2019-06-07 2022-09-21 Philip Morris Products S.A. Nicotine pouch product
WO2023106407A1 (en) * 2021-12-09 2023-06-15 日本たばこ産業株式会社 Composition for oral cavity and pouch product for oral cavity

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JP2009545315A (en) * 2006-08-01 2009-12-24 アール・ジェイ・レノルズ・タバコ・カンパニー Smokeless tobacco
US20100303969A1 (en) * 2008-12-30 2010-12-02 Philip Morris Usa Inc. Dissolvable Films Impregnated with Encapsulated Tobacco, Tea, Coffee, Botanicals, and Flavors for Oral Products
JP2015536688A (en) * 2012-12-20 2015-12-24 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 Americantobacco (Investments) Limited Smokeless oral tobacco products and their preparation

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JP2009545315A (en) * 2006-08-01 2009-12-24 アール・ジェイ・レノルズ・タバコ・カンパニー Smokeless tobacco
US20100303969A1 (en) * 2008-12-30 2010-12-02 Philip Morris Usa Inc. Dissolvable Films Impregnated with Encapsulated Tobacco, Tea, Coffee, Botanicals, and Flavors for Oral Products
JP2015536688A (en) * 2012-12-20 2015-12-24 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 Americantobacco (Investments) Limited Smokeless oral tobacco products and their preparation

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Publication number Priority date Publication date Assignee Title
EP3809884B1 (en) 2019-06-07 2022-09-21 Philip Morris Products S.A. Nicotine pouch product
WO2023106407A1 (en) * 2021-12-09 2023-06-15 日本たばこ産業株式会社 Composition for oral cavity and pouch product for oral cavity

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