JP2023113973A - Nicotine supply oral pouch product and production method therefor - Google Patents

Abstract

To provide a nicotine supply oral pouch product having improved fluidity or improved adhesion and a method for producing the nicotine supply oral pouch product.SOLUTION: 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 wt.% or more.SELECTED DRAWING: Figure 1

Description

The present invention relates to nicotine-delivery oral pouch products and methods of making the same.

Nicotine-supplying oral pouch products such as oral tobacco products are packages in which a composition containing nicotine is housed in a pouch (packaging material) formed of a material such as non-woven fabric. put it inside and use it.
When a nicotine-supplying oral pouch product is put into the user's oral cavity, components such as nicotine in the composition seep out of the packaging material, thereby delivering flavor and taste components to the user. be.

In nicotine-supplying oral pouch products, the feeling of use in the oral cavity during use is important, and techniques for improving the palatability and the compatibility between products and saliva are known. For example, the development of technology to improve mouthfeel in the oral cavity by making the sealing area smaller and reducing the amount of excess air in the product, thereby enabling the desired release of flavor during use (Patent Document 1) In addition, by including a specific substance in the composition, the compatibility of the product with saliva is improved, and technology is being developed to promote rapid transmucosal delivery of the substance in the composition in the oral cavity. (Patent Document 2).

Japanese Patent Publication No. 2019-505174 Japanese Patent Publication No. 2012-522765

As described above, in addition to the ease of release of substances in the composition and the ease of compatibility between the product and saliva, factors that affect the feeling of use in the oral cavity when using the nicotine-delivery oral pouch product include: There is still room for improving the usability.
The present inventors paid attention to the fluidity of the composition in the pouch during use and the adhesion between the materials constituting the composition in general nicotine-delivery oral pouch products. 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 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 adhesiveness 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. It can be thinly deformed.
The above-mentioned improvement in fluidity is an improvement in the feeling of use from when the user holds the pouch product in his mouth and saliva soaks into it until he finishes using it and takes it out of his mouth. , the improvement of the feeling of use in the initial stage from when the user puts the pouch product in his mouth until saliva soaks in, and the improvement of the characteristics is also an advantage for the user. None of the aforementioned patent documents 1 and 2 disclose these characteristics.

Accordingly, an object of the present invention is to provide a nicotine-supplying oral pouch product with improved fluidity or improved adhesion, and a method for producing the same.

As a result of intensive studies, the present inventors have found that the above problems can be solved by using a composition containing gel particles containing a specific substance and setting the water content in the composition to a specific value or higher. and arrived at the present invention.

[1] A nicotine delivery oral pouch product comprising a composition containing gel particles and a pouch for packaging the composition,
the gel particles comprise at least an anionic natural polymeric carbohydrate, calcium ions, and water;
the composition comprises nicotine;
The content of water in the composition is 15% by weight or more,
Nicotine delivery oral pouch product.
[2] The nicotine-delivering oral pouch product of [1], wherein the anionic natural polymeric carbohydrate has a carboxyl group.
[3] The nicotine delivery oral pouch product of [2], wherein the anionic natural polymeric carbohydrate is LM pectin.
[4] The composition according to [2] or [3], wherein the ratio of the total number of carboxyl groups possessed by the anionic natural polymer carbohydrate to the total number of calcium ions is 100:1 to 2:1. of nicotine delivery oral pouch products.
[5] The nicotine-delivering oral pouch product according to any one of [1] to [4], wherein the constituents of the composition have a maximum dry particle size of 15 mm or less.
[6] The nicotine-delivering oral pouch product according to any one of [1] to [5], wherein the pouch is a non-woven fabric.
[7] having a composition manufacturing step of manufacturing a composition comprising at least an anionic natural polymer carbohydrate, a calcium ion donor, and gel particles containing water;
the composition comprises nicotine, and
A method for producing a nicotine-delivering oral pouch product, wherein the water content in the composition is 15% by weight or more.
[8] The method for producing a nicotine-supplying oral pouch product according to [7], wherein the calcium ion supplying agent is liquid.
[9] The method for producing a nicotine-supplying oral pouch product according to [7] or [8], wherein the calcium ion supplying agent contains calcium lactate.

INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide a nicotine-delivering oral pouch product with improved fluidity or improved adhesion, and a method for producing the same.

2 is a diagram showing the relationship between normal stress and shear stress in each composition of Example 2 and Comparative Example 1. FIG. 2 is a diagram showing the relationship between normal stress and shear stress in each composition of Example 3 and Comparative Example 2. FIG. FIG. 4 is a diagram showing the relationship between normal stress and shear stress in each composition of Example 4 and Comparative Example 3. FIG. 1 is a diagram showing the relationship between normal stress and shear stress in each composition of Example 1 and Comparative Example 4. FIG. FIG. 4 is a diagram showing the relationship between normal stress and shear stress in each composition of Example 4 and Comparative Example 5. FIG. FIG. 10 is a diagram showing the relationship between normal stress and shear stress in each composition of Example 5 and Comparative Example 6. FIG.

Embodiments of the present invention will be described in detail below, but these descriptions are examples (representative examples) of embodiments of the present invention, and the present invention is not limited to these contents as long as they do not exceed the gist of the present invention.
In the present specification, the numerical range represented using "to" means a range including the numerical values described before and after "to" as lower and upper limits, and "A to B" is A or more B or less.

<Nicotine supply oral pouch product>
A nicotine-delivering oral pouch product that is an embodiment of the present invention is a nicotine-delivering oral pouch product having a composition containing gel particles and a pouch for packaging the composition,
the gel particles comprise at least an anionic natural polymeric carbohydrate, 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 delivery oral pouch product.

In the above oral pouch product, gel particles are included in the composition in the pouch, and the gel particles have a structure in which at least an anionic natural polymer carbohydrate is 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, the fluidity and/or adhesion of the composition can be improved. Specifically, the fluidity or/and adhesion of anionic natural polymeric 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 an anionic natural polymeric carbohydrate, calcium ions, gel particles containing water, and nicotine. A composition in the present invention is a generic term for any substance contained within a pouch. Moreover, from the viewpoint of preventing the composition from leaking out of the pouch, the composition is preferably not liquid. For example, it preferably consists of only gel particles or gel particles and a solid substance. Moreover, in order to satisfy the preferred embodiment of the particle size described later, it is preferable that the powder is in a particle shape (a plurality of particles) after drying.

The oral pouch product has a composition that includes 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” refers to small particles, which may not be in the form of a perfect sphere. including similar shapes.
In the present specification, the term "gel-like" refers to a state in which a fluid sol-like decomposition product solidifies and spontaneously loses its fluidity while maintaining its elasticity. A substance is called a "gel" and a substance consisting of a gel is called a "gel substance".

The content of 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. , more preferably 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.

Gel particles are not particularly limited as long as they contain at least an anionic natural polymeric carbohydrate, calcium ions, and water.
(Gelling agent)
The anionic natural polymer carbohydrate is a gelling agent, and the type thereof is not particularly limited, but polysaccharides having carboxyl groups are preferred, such as carrageenan, pectin, gum arabic, xanthan, gellan, gum tragacanth, and alginic acid. , carrageenan, pectin, gellan, and alginic acid are preferred from the viewpoints that gelation is likely to occur in the presence of calcium ions and that a junction zone can be formed between carboxyl groups and cations to form a crosslinked structure. Among these, LM pectin is preferred for the reasons described below. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

“Pectin” is a polysaccharide composed of galacturonic acid and galacturonic acid methyl ester as structural units, which are α1,4-linked. In addition to galacturonic acid, it is known to contain several diverse sugars. Pectin is generally classified into LM pectin with a degree of esterification of less than 50% and HM pectin with a degree of esterification of 50% or more, and as described above, LM pectin is preferred in the present embodiment.
Pectin gels particularly in the presence of divalent cations such as calcium ions, and the carboxyl groups of galacturonic acid in pectin and cations form junction zones to form gels. A pectin with a large number of junction zones, that is, a pectin with 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, and even more preferably 10% or less, and there is no need to set a lower limit for the degree of esterification. , usually more than 6%.

"Gellan" is known as a water-soluble polysaccharide synthesized by Pseudomonas elodea, one of the eubacteria. When cations are added to the aqueous solution, they are electrically neutralized and gellan gum becomes less water-soluble and gels. Gellan is a polymer compound in which repeating units each consisting of two D-glucose residues, one L-rhamnose residue and one D-glucuronic acid tetrasaccharide are linked in a straight chain. The repeating structure of the tetrasaccharide is as follows.
[D-Glc(β1→4)D-GlcA(β1→4)D-Glc(β1→4)L-Rha(α1→3)]n

“Carrageenan” is a kind of linear sulfur-containing polysaccharides and is an anionic polymer compound composed of D-galactose (or 3,6-anhydro-D-galactose) and sulfuric acid.

"Alginic acid" is a kind of polysaccharide mainly contained in brown algae. It has a pyranose-type structure in which α-L-guluronic acid and β-D-mannuronic acid are linked via 1,4-glycosidic bonds (CAS 9005-38-3). It has the property of gelling when a cation is added.

"Gum arabic", also called "gum arabic" or "arabic resin", is obtained by drying the secretion from wounds of the bark of Acacia senegal, a plant of the Fabaceae Columbine subfamily Acacia senegal, or a related plant of the same genus. It is a thing. The main component is polysaccharide (polyuronic acid), a mixture of arabinogalactan (75-94%), arabinogalactan-protein (5-20%), glycoprotein (1-5%). The structure of polysaccharides has galactose in the main chain and galactose, arabinose, rhamnose and glucuronic acid in the side chains. Unlike the hemicellulose that constitutes the cell wall, it has free carboxyl groups and is usually a calcium salt.

“Xanthan” is one of polysaccharides and is generally produced by fermenting corn sugar starch with bacteria. It has a repeating structure with units of 2 glucose molecules, 2 mannose molecules and glucuronic acid molecules (CAS 11138-66-2).

"Gum tragacanth" is a polysaccharide thickener obtained by drying the exudate of tragacanth, a leguminous plant, 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, including 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 standard polystyrene calibration curve 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. The weight average molecular weight can be increased by the addition of divalent cations and can be decreased by the addition of 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 2.0% by weight or more, and usually 50.0% by weight or less, preferably 20% by weight or less, more preferably 10% by weight or less; % by weight or less is more preferable.
The content of anionic natural polymer carbohydrates in the composition can be measured by various fractionation separation methods and detection methods using liquid chromatography, liquid chromatography mass spectrometry, and the like.

(Gelling aid component)
Calcium ion is a gelation aid component, and its source (gelling aid) is not particularly limited. Among these, calcium lactate, calcium carbonate, and calcium phosphate are preferred from the viewpoints of little influence on the taste of pouch products, high solubility, and pH after dissolution. Calcium lactate is preferred. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

The content of calcium ions in the composition is not particularly limited, but from the viewpoint of ensuring good fluidity and adhesion, the molar ratio to the weight of the composition is usually 0.00023 mol/kg or more. 0023 mol/kg or more, more preferably 0.023 mol/kg or more, still more preferably 0.046 mol/kg or more, and usually 1.15 mol/kg or less, and 0.046 mol/kg or more. 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.

When a compound having a carboxyl group is used as the anionic natural polymer carbohydrate, the anionic natural polymer carbohydrate constituting the gelling agent is likely to gel in the presence of a divalent cation, and the carboxyl group and the cation form a junction zone. to form a gel. The presence of junction zones in the gel results in a network structure in the composition containing the gel. It is desirable that the carboxyl group and the compound containing a divalent cation, which is a gelation-promoting component, are efficiently gelled, and that the two are present in a number ratio of 2:1. This corresponds to a 2:1 molar ratio of carboxyl-containing monomers to cations in the anionic natural polymeric carbohydrate. Therefore, the ratio of the total number of carboxyl groups possessed by the anionic natural polymer carbohydrate to the total number of calcium ions is preferably 100:1 to 2:1, 50:1 to 2:1.
, in the range of 10:1 to 2:1.

(Other gelling aid ingredients)
The composition may contain gelation aids other than calcium ions, such as magnesium, silver, zinc, copper, gold, aluminum, etc., which can bind gelling agents with ionic bonds in the same manner as calcium ions. metal ions, ions of cationic polymers, etc. Sources of these (other gelation aids) include, for example, halides (chlorides, etc.) of these metal ions, citric acid, carbonate Salts, sulfates, phosphates, cationic polymers and the like are included. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

(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 will be rough and the production of the composition will be difficult. Furthermore, from the viewpoint of ensuring good fluidity and adhesion of the composition and easiness of manufacturing the composition, the content is preferably 30% by weight or more, more preferably 45% by weight or more, and usually It is 55% by weight or less, preferably 50% by weight or less. The water content can be adjusted by adjusting the amount of water to be added, or by providing heat treatment or drying treatment in the production stage.

The water content (moisture content) of the above composition is measured using a heat drying moisture meter (eg, HB 43-S manufactured by METER TOLEDO). At the time of measurement, the sample is placed in a predetermined container and heated to reach a temperature of 100°C. The measurement is terminated when the amount of change becomes 1 mg or less in 60 seconds, and the moisture content is calculated from the weighed values before and after heating.
The method for measuring the moisture content in the present specification is similarly applied to the measurement of the moisture content of objects other than the composition, for example, the mixture in the method for producing the composition described below.

(nicotine)
The composition contains nicotine, but the embodiment containing nicotine is not particularly limited. ), tobacco leaves may be added as a nicotine source, and a nicotine-containing extract obtained by extracting nicotine-containing substances such as tobacco leaves may be included. good too. In addition, the manner in which nicotine is contained is not particularly limited, and the above-described 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 modes, the addition of a nicotine-containing compound is preferable from the viewpoint of accurate supply of nicotine and ease of handling. Generally, when tobacco leaves are added, the color of the composition or pouch product tends to be the color of tobacco leaves, whereas when a colorless nicotine-containing compound is used, a white composition or pouch product is provided. It becomes possible to Such an aspect is an advantage for users who prefer white pouch products.
One of the above aspects may be applied alone, or two or more aspects may be applied in combination.

Although the content of nicotine in the composition is not particularly limited, it is usually 0.1% by weight or more and usually 6.7% by weight or less from the viewpoint of user's preference. In addition, when nicotine exists as an ion, said content rate is a content rate as a nicotine ion.
The content of nicotine in the composition can be measured with a gas chromatography-mass spectrometer (GC-MS).

(other substances)
The composition may contain substances other than the above-described anionic natural polymeric carbohydrates, calcium ions, other gelling aids, water, nicotine (also referred to as "other substances"), said other substances comprising: It may be contained in the gel particles, or may be contained in the composition separately from the gel particles. Other substances include, for example, base materials, fragrances, pH adjusters, sweeteners, humectants, bitterness inhibitors, whitening agents and the like.
The content of other substances in the composition is not particularly limited, and the formulation can be appropriately adjusted according to product design.

The type of substrate is not particularly limited, and examples thereof include cellulose, microcrystalline cellulose, spherical cellulose, porous cellulose and the like, and cellulose is preferred from the viewpoint of flexibility in adjusting the bulk density of the composition. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.
The content of the base material in the composition is not particularly limited, but is usually 24% by weight or more, and should be 27% by weight or more, from the viewpoint of quality improvement such as suppression of water elution during production or product storage. is preferred, and it is more preferably 30% by weight or more, and there is no need to limit the upper limit, but from the viewpoint of the limit that other raw materials can be blended, it is usually 65% by weight or less, and 55% by weight or less. It is preferably 50% by weight or less, more preferably 50% by weight or less.

The type of fragrance is not particularly limited, and examples thereof include menthol, leaf tobacco extract, natural plant fragrance (e.g., cinnamon, sage, herb, chamomile, arrowroot, sweet tea, clove, lavender, cardamom, clove, nutmeg, bergamot, Geranium, Honey Essence, Rose Oil, Lemon, Orange, Cinnamon, Caraway, Jasmine, Ginger, Coriander, Vanilla Extract, Spearmint, Peppermint, Cassia, Coffee, Celery, Cascarilla, Sandalwood, Cocoa, Ylang Ylang, Fennel, Anise. , licorice, St. John's bread, plum extract, peach extract, etc.), sugars (e.g., glucose, fructose, isomerized sugar, caramel, honey, molasses, etc.), cocoa (powder, extract, etc.), esters (e.g., acetic acid isoamyl, linalyl acetate, isoamyl propionate, linalyl butyrate, etc.), ketones (e.g., menthone, ionone, damascenone, ethyl maltol, etc.), alcohols (e.g., geraniol, linalool, anethole, eugenol, etc.), aldehydes (e.g., vanillin, benzaldehyde, anisaldehyde, etc.), lactones (e.g., γ-undecalactone, γ-nonalactone, etc.), animal fragrances (e.g., musk, ambergris, civet, castoreum, etc.), hydrocarbons (e.g., limonene) , pinene, etc.). One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

The type of pH adjuster is not particularly limited, and examples thereof include sodium carbonate, sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate, anhydrous sodium phosphate, sodium dihydrogen phosphate, sodium citrate, and the like. Sodium carbonate, potassium carbonate and sodium dihydrogen phosphate are preferred from the viewpoint of influence on taste. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type 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 preferred from the viewpoint of taste control. . One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

The bitterness inhibitor is not particularly limited, and examples thereof include soybean lecithin. Soybean lecithin is a phospholipid and includes phosphatidylcholine, phosphatidylethanolamine, phosphatidic acid and the like. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

The type of moisturizing agent is not particularly limited, and examples thereof include glycerin and propylene glycol, and glycerin is preferable from the viewpoint of product storage stability. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

The type of the whitening agent is not particularly limited, and examples thereof include fine silicon dioxide, titanium dioxide, calcium carbonate, etc. Fine silicon dioxide is preferable from the viewpoint of the influence on the taste of the product. One type of these substances may be used alone, or two or more types may be used in combination in an arbitrary type and ratio.

The content of each component described above (excluding the content of water) can also be calculated from the charged amount of raw materials.

(pH of composition)
The pH of the composition at a measurement temperature of 22 ° C. is not particularly limited, but from the viewpoint of the effect on the taste of the product, it is usually 6.0 or more, preferably 7.0 or more, and 8.0 or more. is more preferably 10.0 or less, preferably 9.0 or less. The pH can be adjusted by controlling the amount of pH adjuster added. In addition to the above pH value, the pH value in this specification is a value measured at a measurement temperature of 22°C.

The pH of the composition at the above measurement temperature of 22 ° C. is measured using a pH analyzer (for example, LAQUA F-72 flat ISFET pH electrode manufactured by Horiba Ltd.). , measure the supernatant.
For calibration of the device, 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 Wako Pure Chemical Industries) Perform a three-point calibration using

(Fluidity of composition)
As described above, the fluidity of the composition is expressed herein in terms of shear stress at a normal stress of 5 kPa at a measurement temperature of 22°C. When the user puts the pouch product into 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, the pressure applied to the pouch product is usually a normal stress of 3 to 7 kPa, so 5 kPa. adopt the normal stress of From the viewpoint of improving fluidity and/or adhesion, the shear stress is usually 5.99 kPa or less, preferably 5.93 kPa or less, and usually 5.02 kPa or more, and 5.13 kPa or more. and more preferably 5.42 kPa or more. The shear stress can be increased/decreased with the incorporation of anionic natural polysaccharides (pectin) and Ca ions.

The shear stress of the composition at the above normal stress of 5 kPa can be measured using a rheometer. For example, when powder rheometer FT4 manufactured by Freeman Technology Co., Ltd. is used as the rheometer, measurement is performed under the following measurement conditions.
・Measurement mode: standard program (25mm_shear_9kPa)
・Measurement temperature: 22°C
・Measurement humidity: 60% RH
・Measurement container: Cylindrical container with an inner diameter of 25 mm and a volume of 10 ml
・Vertical load: 3 to 9 kPa
Each raw material to be measured is passed through a sieve (1.18 mm mesh size) to make fine and uniform particles, which is used as a measurement sample, and the measurement is performed according to the procedure of the rheometer described above.

(Adhesion of composition)
As described above, the adhesion of the composition is expressed herein in terms of shear stress at a normal stress of 0 kPa at a measurement temperature of 22°C. The normal stress of 0 kPa is assumed to be the pressure when the pouch product is crushed in the thickness direction after the user puts the pouch product in the mouth and before it is soaked in saliva, that is, the state where no pressure is applied in other than the thickness direction. It is a numerical value. From the viewpoint of improving fluidity and/or adhesion, the shear stress is usually 1.83 kPa or less, preferably 1.78 kPa or less, and usually 0.88 kPa or more, and 1.12 kPa or more. and more preferably 1.26 kPa or more. The shear rate can be increased/decreased with the incorporation of anionic natural polysaccharides (pectin) and Ca ions.

The shear stress of the composition was measured at normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa in the same manner as in the measurement of fluidity described above, and a graph was created by plotting the normal stress on the horizontal axis and the shear stress on the vertical axis. do. Since the shear stress changes linearly with respect to the normal stress, this graph is fitted, and the shear stress at a normal stress of 0 kPa is calculated from the fitting results. The fitting conditions are shown below.
From each value of shear stress for each normal stress (3 kPa, 4 kPa, 5 kPa, 6 kPa, 7 kPa), a linear linear regression line is derived by calculation. Calculate its slope and Y-intercept values. The calculated Y-intercept value is taken as the shear stress at a normal stress of 0 kPa.

(Particle size of constituents of composition when dry)
The size of the components of the composition (simply referred to as "composition") is not particularly limited, but for example, the dried components of the composition preferably satisfy the following classification conditions.
The dried composition is preferably classified by a sieve having the following meshes. From the viewpoint of the user's good texture during use, ease of handling during manufacturing, and control of quality variation, it is usually passed through a sieve having a sieve mesh of 15 mm (≤ 15 mm), and a 10 mm sieve. It is preferable to pass through a sieve having meshes (≦10 mm), more preferably to pass through a sieve having meshes of 5 mm (≦5 mm), and a sieve having meshes of 3.2 mm. More preferably, it passes through (≦3.2 mm). For example, when all of the dried gel particles pass through a sieve with a sieve mesh of X mm, it means that the maximum particle size of the gel particles when dried is X mm or less.
The above dried composition is obtained by drying the composition by holding it at 70° C. to 80° C. for about 3 hours.
The maximum particle size of the composition can be appropriately increased/decreased by blending the anionic natural polysaccharide (pectin) and Ca ion and the amount of water to be contained.
From the viewpoint of improving fluidity and/or adhesion, it is not necessary to set the lower limit of the particle size of the dry composition, but from the viewpoint of preventing leakage from the pouch, it is usually 0.3 μm or more.

[Pouch]
The pouch (packaging material) can pack the above composition, is insoluble in water, and is permeable to liquids (water, saliva, etc.) and water-soluble components in the composition. If there is, it is not particularly limited, and a known one can be used. Materials for the pouch include, for example, cellulose-based nonwoven fabrics, and commercially available nonwoven fabrics 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 bag by a means such as heat sealing.
The basis weight of the sheet is not particularly limited, and is usually 12 gsm or more and 54 gsm or less, preferably 24 gsm or more and 30 gsm or less.
The thickness of the sheet is not particularly limited, and is usually 100 μm or more and 300 μm or less, preferably 175 μm or more and 215 μm or less.

At least one of the inner and outer surfaces of the pouch may be partially coated with a water-repellent material. A water-repellent fluorine-based resin is suitable as the water-repellent material. Specifically, this type of water-repellent fluororesin includes Asahi Guard (registered trademark) manufactured by Asahi Glass Co., Ltd. Water-repellent fluorine-based resins are applied to packaging materials for foods and products containing oils and fats, such as confectionery, dairy products, side dishes, fast food, and pet food. Therefore, this type of water-repellent fluororesin is safe even when applied to pouches placed in the oral cavity. The water-repellent material is not limited to the fluorine-based resin, and may be, for example, a paraffin resin, a silicon-based resin, an epoxy-based resin, or the like, as long as it has a water-repellent action.

The pouch may contain optional ingredients, such as raw materials for adjusting fragrance and taste, flavors, additives, tobacco extracts, pigments, and the like. In addition, there are no particular restrictions on the manner in which these components are contained, and examples include the manner in which they are applied to the surface of the pouch, the manner in which they are impregnated, and the manner in which they are contained in the fibers when they are made of fibers.
Furthermore, the appearance of the pouch is not particularly limited, and may be not only non-transparent but also translucent or transparent, in which case the composition packed in the pouch can be seen through.

[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 enclosing the above composition).
The size and weight of the pouch product are not particularly limited. The short side may be 10 mm or more and 20 mm or less, or 14 mm or more and 18 mm or less. Moreover, the weight of the pouch product before use may be 0.1 g or more and 2.0 g or less, or may be 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 It is usually 99% by weight or less, preferably 97% by weight or less, more preferably 95% by weight or less.

In the measurement of each characteristic in this specification, the measurement sample is kept in the same environment as the environment to be measured for 48 hours or more before the measurement. In addition, the measurement temperature, measurement humidity, and measurement pressure are normal temperature (22 ± 2 ° C), normal humidity (60 ± 5% RH), and normal pressure (atmospheric pressure) unless otherwise specified. .

<Manufacturing method of nicotine supply oral pouch product>
Another embodiment of the present invention, a method for producing a nicotine-delivering oral pouch product (also referred to simply as "a method for producing a nicotine-delivering oral pouch product" or "a production method") comprises at least an anionic natural polymeric carbohydrate, a calcium ion supplying agent, , and a composition manufacturing step of manufacturing a composition containing gel particles containing water,
the composition comprises nicotine, and
A method for producing a nicotine-supplying oral pouch product, wherein the content of water in the composition is 15% by weight or more.

[Composition manufacturing process]
The above composition manufacturing process is not particularly limited as long as the above composition can be manufactured. An example of the method for producing the composition is shown below. Each raw material mentioned below can be used for each raw material shown below.
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 whitening agent such as silicon dioxide are mixed to obtain a mixture (mixture before addition of calcium source) (calcium supply source). mixture preparation step before source addition). Thereafter, 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, by spraying) and mixed to obtain a mixture (pre-heating mixture). (Mixture preparation step before heating).
The calcium supply source may be supplied as an aqueous solution or as a solid. 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 can be solid. It is preferable to supply as an aqueous solution from the viewpoint that the contact efficiency with the anionic natural polymer carbohydrate is higher than that supplied as an aqueous solution. Also, the calcium source may be added after making the mixture containing the anionic natural polymeric carbohydrate, as described above, or mixed with the anionic natural polymeric carbohydrate first, but produces fine, uniform gel particles. From the viewpoint of allowing the addition of anionic natural polymer carbohydrates, it is preferable to add them after preparing a mixture containing the anionic natural polymer carbohydrates. 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 addition of the calcium source, water may be added together with each aqueous solution in order to obtain the desired amount of water.
In addition, from the viewpoint of sufficiently dissolving the anionic natural polymer carbohydrate in advance, it is preferable to incorporate a sufficient amount of water into the mixture before the following heating step (step of forming gel particles). After completion of the production process, the water content of the mixture is preferably 10% by weight or more and 50% by weight or less, more preferably 20% by weight or more and 40% by weight or less.
The pre-heating mixture is preferably pH-adjusted. For example, a pH adjuster such as sodium dihydrogen phosphate is preferably used to adjust the amount added so that the pre-heating mixture becomes acidic. Specifically, the pH of the mixture before heating is preferably 3.0 or more and 6.0 or less, more preferably 4.0 or more and 6.0 or less.
In this step, by adjusting the pH to 6.0 or less, the heating step can be proceeded while maintaining the nicotine contained in the pre-heating mixture in a stable state.

By heating the above pre-heating mixture to hydrate the anionic natural polymer carbohydrates and promote contact between the anionic natural polymer carbohydrates and calcium ions, gel particles are made and a mixture containing gel particles (gel particle-containing mixture ) is obtained (heating step).
The heating method in the heating step is not particularly limited, and includes, for example, 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 mixture. . The temperature of the mixture during heating is not particularly limited, but from the viewpoint of efficiently hydrating the anionic natural polymer carbohydrate, it is preferably 60° C. or higher and 90° C. or lower, and preferably 70° C. or higher and 80° C. or lower. 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 and Ca ion and from the viewpoint of appropriately adjusting the water content in the composition. , more preferably 1 hour or more and 2 hours or less.

After the heating step, the mixture may be dried (drying step). After that, a cooling process may be performed. Cooling may be natural cooling, or may be performed using some cooling means (cooling step). By drying, it is possible, for example, to adjust the water content of the mixture to 5 to 45% by weight. This facilitates adjustment of the water content in the target composition.

An aqueous solution containing a pH adjuster such as potassium carbonate is further added to the gel particle-containing mixture obtained in the heating step (or drying step or cooling step).
It is preferable to adjust the amount added 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. is preferred, and 8.0 or more and 9.0 or less is more preferred.
A sweetener such as acesulfame potassium, a flavoring agent such as menthol, a bitterness inhibitor such as soybean lecithin, and a humectant such as glycerin are added (the step of adding additives to the gel particle-containing mixture) to obtain a desired composition.
When adding the above-mentioned additives, etc., they may be solid or may be added in the form of an aqueous solution dissolved in water. When it is added in the form of an aqueous solution, it may be dissolved in a predetermined amount of water in advance and added so as to obtain the final moisture content of the pouch product.

[Packaging process]
A pouch product is obtained by packaging the composition obtained in the above composition preparation step with a packaging agent (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 nonwoven fabric and then sealing can be used.
In the packaging step, water may be added to obtain a composition having a desired moisture content after the composition is put into the packaging agent and after the packaging agent is sealed (water addition step). For example, when the target composition has a water content of 50% by weight and the composition obtained in the above composition preparation step has a water content of 15% by weight, the remaining 35% by weight Add water.

<Uses of pouch products>
Applications (modes of use) of pouch products are not particularly limited. These are inserted between the lips and gums in the oral cavity to enjoy the taste and aroma.

EXAMPLES Hereinafter, the present invention will be described more specifically with reference to Examples. However, the present invention should not be construed as being limited to the following examples.

<Experiment 1>
[Preparation of composition]
(Example 1)
Pectin 75.0 g (Classic CU902 from H&F), Nicotine Polacrilex 680.0 g (Nicotine Polacrilex 20% from Contraf nicotex), Cellulose 2175 g (VITACEL L600-30 from J. RETTENMAIER & SOHNE), Dioxide After mixing 75.0 g of silicon (silica) (SYLOPAGE 720 manufactured by Fuji Silysia Co., Ltd.), 35.3 g of calcium lactate aqueous solution (calcium lactate (granules) manufactured by Taihei Kagaku Sangyo Co., Ltd.) and anhydrous phosphoric acid were added to the mixture. 302.1 g of an aqueous sodium solution (Monosodium phosphate anhydrous, FG (MSP A FG) manufactured by Univar BV) was added and mixed until uniform to form mixture A at pH 6.2 (moisture content 23.5% by weight). ).
The resulting mixture A was subjected to jacket heating (can wall temperature 100 ° C.) for 1 hour so that the material temperature of the raw material was 70 ° C. to 80 ° C. (water content after heating was 6.2 wt%, pH was 6.0 (measured by the same measurement method as for the tobacco filling described above)). After that, it 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 (manufactured by Univar BV) was added to the mixture B obtained on cooling.
POTASSIUM CARBONATE) was added to obtain a mixture C.
Finally, to adjust the water content, 0 g of water was added to Mixture C (i.e. no additional water was added) and 200 g of Composition 1 of Example 1 (water content of 15.10 wt%, pH 7.8). got

(Example 2)
Composition 2 of Example 2 (water content: 18.47 wt. %) was prepared in an amount of 100 g.

(Example 3)
Composition 3 of Example 3 (water content: 32.06 wt. %) was prepared.

(Example 4)
Composition 4 of Example 4 (water content: 46.98 wt. %) was prepared.

(Example 5)
Composition 5 of Example 5 (water content: 52.49 wt. %) was prepared in an amount of 100 g.

(Comparative example 1)
In the same manner as composition 1 above, except that pectin and an aqueous solution of calcium lactate were not added, and that the amount of water added to mixture C was changed from 0 g to 3.46 g, comparison was performed. 100 g of Composition 6 of Example 1 (water content: 18.18% by weight, pH: 7.8) was prepared.

(Comparative example 2)
In the same manner as composition 1 above, except that pectin and an aqueous solution of calcium lactate were not added, and that the amount of water added to mixture C was changed from 0 g to 43.00 g, comparison was performed. 200 g of composition 7 (water content: 31.46% by weight) of Example 2 was prepared.

(Comparative Example 3)
In the same manner as composition 1 above, except that pectin and an aqueous solution of calcium lactate were not added and the amount of water added to mixture C was changed from 0 g to 109.27 g. 200 g of composition 8 (water content: 46.60% by weight) of Example 3 was prepared.

[Characteristic evaluation]
(moisture content)
The water content (moisture content) of each composition was measured using a heat drying moisture meter (eg, HB 43-S manufactured by METER TOLEDO).
・Measurement mode: FAST
・Achievement temperature (when stable): 100°C
・ Measurement end condition: AUTO60 (amount of change of 1 mg or less in 60 seconds)
・Result display: Moisture%

(pH)
The pH of the composition at a measurement temperature of 22° C. was measured using a pH analyzer (for example, LAQUA F-72 flat ISFET pH electrode manufactured by Horiba Ltd.).
For calibration of the device, 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 Wako Pure Chemical Industries) A three-point calibration using

(Liquidity)
The shear stress of the composition at a normal stress of 5 kPa was measured under the following measurement conditions using a powder rheometer FT4 manufactured by Freeman Technology Co., Ltd. as a rheometer.
・Measurement mode: standard program (25mm_shear_9kPa)
・Measurement temperature: 22°C
・Measurement humidity: 60% RH
・Measurement container: Cylindrical container with an inner diameter of 25 mm and a volume of 10 ml
・Vertical load: 3 to 9 kPa
Each raw material to be measured was passed through a sieve (1.18 mm mesh size) to make fine and uniform particles, which was used as a measurement sample, and measured according to the procedure of the rheometer described above.

(Adhesion)
The shear stress of the composition was measured at normal stresses of 3 kPa, 4 kPa, 5 kPa, 6 kPa, and 7 kPa in the same manner as in the measurement of fluidity described above, and a graph was created by plotting the normal stress on the horizontal axis and the shear stress on the vertical axis. did. Since the shear stress changes linearly with respect to the normal stress, this graph was fitted, and the shear stress at a normal stress of 0 kPa was calculated from the fitting results. The fitting conditions are shown below.
From each value of shear stress for each normal stress (3 kPa, 4 kPa, 5 kPa, 6 kPa, 7 kPa), a linear linear regression line is derived by calculation. Calculate its slope and Y-intercept values. The calculated Y-intercept value is taken as the shear stress at a normal stress of 0 kPa.

Table 1 below summarizes the ratio of raw materials used in each of the above compositions and the evaluation results of each property. In addition, the raw materials listed in Table 1 do not indicate all the raw materials contained, but show a part of the raw materials contained. In addition, the numerical values of the raw materials shown in the table are not the content of each component in the composition, but the charged amount. In Table 1, the notation "≦X" in the maximum particle size of the composition means that the maximum particle size of the composition when dried is X or less.
In addition, the notation of "-" in Table 1 indicates no addition.
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 adhesion property, and Example 2 and Comparative Example 1 (water content: about 18 %), Example 3 and Comparative Example 2 (water content of about 30% by weight), and Example 4 and Comparative Example 3 (water content of about 45% by weight) are plotted in the graphs shown in FIGS. .

From Table 1 above, the compositions of Examples 1 to 5, which satisfy the requirements of the above embodiments, have a higher shear stress at a normal stress of 5 kPa than the compositions of Comparative Examples 1 to 3, which do not satisfy the requirements. and the shear stress at a normal stress of 0 kPa is low, that is, the fluidity and adhesion are improved. Specifically, it was found that the combined use of pectin and an aqueous solution of calcium lactate improves fluidity and adhesion.

<Experiment 2>
[Preparation of composition]
(Examples 1 to 5)
Compositions 1 to 5 in Examples 1 to 5 above were used as compositions of Examples.

(Comparative Example 4)
200 g of Composition 9 of Comparative Example 4 (water content: 16.12% by weight, pH: 7.8) was prepared in the same manner as Composition 1, except that no aqueous calcium lactate solution was added. did.

(Comparative Example 5)
Comparative Example 5 was prepared in the same manner as in Composition 1 except that the aqueous calcium lactate solution was not added and the amount of water added to Mixture C was changed from 0 g to 105.33 g. 200 g of composition 10 (water content: 47.06% by weight) was prepared.

(Comparative Example 6)
Comparative Example 6 was prepared in the same manner as in Composition 1 except that the aqueous calcium lactate solution was not added and the amount of water added to Mixture C was changed from 0 g to 86.09 g. 100 g of composition 11 (water content: 55.97% by weight) was prepared.

[Characteristic evaluation]
For each of the above compositions, the same property evaluation as in Experiment 1 above was performed. The evaluation results of this property are shown in Table 3 below. It should be noted that the raw materials listed in Table 3 do not indicate all of the raw materials contained, but only some of the raw materials contained. In addition, the numerical values of the raw materials shown in the table are not the content of each component in the composition, but the charged amount. In Table 3, the notation "≦X" in the maximum particle size of the composition means that the maximum particle size of the composition when dried 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 adhesion property, and Example 1 and Comparative Example 4 (water content: about 15 %), 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) are plotted respectively in graphs shown in FIGS. .

From Table 3 above, the compositions of Examples 1 to 5 that satisfy the requirements of the above embodiments have a shear stress at a normal stress of 5 kPa, and the shear stress at a normal stress of 0 kPa is low, that is, the fluidity and adhesion are improved. Specifically, it was found that the use of an aqueous calcium lactate solution improved fluidity and adhesion.
Furthermore, considering Table 1 in Experiment 1 above, from the comparison of Example 4, Comparative Example 2, and Comparative Example 5 in which the composition has a water content of about 45%, shear stress at a normal stress of 5 kPa in this order , and shear stress at a normal stress of 0 kPa are higher. In other words, it was found that the addition of pectin improved the fluidity and adhesion, and the addition of the calcium lactate aqueous solution further improved the fluidity and adhesion.

<Experiment 3>
[Preparation of composition]
(Comparative Examples 4-6)
In this experiment, Comparative Examples 4 to 6 above were used.

(Comparative Example 7)
7.7 g pectin (Classic CU902 from H&F), 2.2 g nicotine Polacrilex (20% Nicotine Polacrilex from Contraf nicotex), 32.8 g microcrystalline cellulose (HICEL 90M MCC from Brenntag Nordic), carbonate 6.3 g of sodium (SODIUM CARBONATE ANHYDROUS manufactured by UNIVAR) and 41.2 g of maltitol (C*Maltidex CH 16385 manufactured by CALDIC NORDIC) were mixed until uniform to prepare composition 12 of Comparative Example 7 (pH 8.6). , moisture content 7.0% by weight).
As can be seen from the above manufacturing method, in Comparative Example 7, no aqueous solution or water was added, and heat treatment was not performed. The water indicated by the above moisture content is derived from the water originally contained in each raw material.

[Characteristic evaluation]
(Sensory evaluation)
Sensory evaluation was performed using each composition of Comparative Examples 4 to 7 above. Sensory evaluation was performed by the following method. Five panelists specializing in sensory evaluation of pouch products held each pouch made using the above composition in their mouths, and graded evaluation from good to unfavorable in terms of various indicators such as texture, flavor, and satisfaction. went.

As a result of the above sensory evaluation, compared with Comparative Examples 4, 5, and 6 in which water was added (including the addition of water as an aqueous solution), Comparative Example 7 in which water was not added In the oral cavity, there was a feeling of a foreign body, a feeling of dryness in the mouth, and a tendency that saliva was difficult to absorb.

<Production of pouch products>
For example, each of the above compositions is put into a nonwoven fabric (manufactured by BFF technical fabrics, basis weight 27.0 g/m ² ) so as to be 0.65 g / piece, and then sealed by heat sealing. Pouch products can be made.

INDUSTRIAL APPLICABILITY As described above, according to the present invention, it is possible to provide a nicotine-delivering oral pouch product with improved fluidity or improved adhesion, and a method for producing the same.

Claims (9)

A nicotine delivery oral pouch product comprising a composition comprising gel particles and a pouch for packaging the composition,
the gel particles comprise at least an anionic natural polymeric carbohydrate, calcium ions, and water;
the composition comprises nicotine;
The content of water in the composition is 15% by weight or more,
Nicotine delivery oral pouch product. 2. The nicotine delivery oral pouch product of claim 1, wherein said anionic natural polymeric carbohydrates have carboxyl groups. 3. The nicotine delivery oral pouch product of claim 2, wherein said anionic natural polymeric carbohydrate is LM pectin. 5. The nicotine-supplying oral pouch according to claim 3 or 4, wherein the ratio of the total number of carboxyl groups possessed by the anionic natural polymer carbohydrate to the total number of calcium ions in the composition is 100:1 to 2:1. product. A nicotine delivery oral pouch product according to any one of claims 1 to 4, wherein the composition constituents have a maximum dry particle size of 15 mm or less. The nicotine delivery oral pouch product of any one of claims 1-5, wherein said pouch is a non-woven fabric. a composition manufacturing step for manufacturing a composition comprising gel particles comprising at least an anionic natural polymeric carbohydrate, a calcium ion donor, and water;
the composition comprises nicotine, and
A method for producing a nicotine-delivering oral pouch product, wherein the water content in the composition is 15% by weight or more. 8. The method of manufacturing a nicotine-delivering oral pouch product according to claim 7, wherein said calcium ion donor is liquid. 9. The method for producing a nicotine-delivering oral pouch product according to claim 7 or 8, wherein said calcium ion donor comprises calcium lactate.

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