Dentifrice composition

Abstract

To provide a dentifrice excellent in usability and storage stability when containing a specific water-soluble polymer and a fluoride ion together with sorbitol or glycerin.SOLUTION: The present invention provides a toothpaste composition comprising (A) at least one of sorbitol and glycerin, (B) at least one selected from the group consisting of xanthan gums, sodium carboxymethyl celluloses, and sodium alginates, and (C) a fluorine-containing compound, wherein the content of ingredient (A) is 15 to 47 mass%, the content of ingredient (B) is 0.7 to 4 mass%, and the content of ingredient (C) is 3500 to 20000ppm in terms of fluoride ion concentration.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention relates to dentifrice compositions. [Background technology]

[0002] Toothpaste is often packed in tubes or pumps, and contains humectants such as sorbitol or glycerin to prevent the opening of the tube from drying out.

[0003] Furthermore, when cleaning the mouth with a dentifrice, a toothbrush or an interdental brush is used, and from the viewpoint of ease of use, the dentifrice is usually prepared as a somewhat viscous liquid or a shape-retaining paste. To maintain shape retention, it is common to incorporate a water-soluble polymer into the dentifrice, which is a well-known technique.

[0004] For example, Patent Document 1 describes a dentifrice containing 20.5 to 23.9 mass % of sorbitol and glycerin in total, 0.2 to 0.7 mass % of xanthan gum, and about 5,000 (4976) ppm of sodium fluoride as fluoride ions. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Special Publication No. 2011-513436 Summary of the Invention [Problem to be solved by the invention]

[0006] Even when dentifrice contains sorbitol or glycerin and a water-soluble polymer such as xanthan gum, sodium carboxymethylcellulose, or sodium alginate, as in the dentifrice described in Patent Document 1, the dentifrice remaining at the opening of the tube may dry out. Furthermore, issues with usability may arise, such as stringiness when dispensed from the tube or pump onto the toothbrush, or stickiness in the oral cavity after rinsing.

[0007] The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a dentifrice that is easy to use and has excellent storage stability when it contains a specific water-soluble polymer and fluoride ions together with sorbitol or glycerin. [Means for solving the problem]

[0008] The present invention provides the following [1] to [8]. [1] (A) at least one of sorbitol and glycerin, (B) at least one selected from the group consisting of xanthan gum, sodium carboxymethylcellulose, and sodium alginate; and (C) Fluorine-containing compounds Contains The content of component (A) is 15 to 47 mass %; The content of component (B) is 0.7 to 4 mass %, and A dentifrice composition having a content of component (C) of 3500 to 20000 ppm when converted into a fluoride ion concentration. [2] The dentifrice composition according to [1], wherein the content of component (C) is 4500 to 15000 ppm when converted into a fluoride ion concentration. [3] The dentifrice composition according to [1] or [2], wherein the ratio (C / B) of the content (ppm) of component (C) converted into fluoride ion concentration to the content (mass%) of component (B) is 1500 to 14000. [4] (D1) The dentifrice composition according to any one of [1] to [3], further comprising at least one selected from the group consisting of anhydrous silicic acid, hydroxyapatite, cellulose powder, and granules. [5] The dentifrice composition according to any one of [1] to [4], further comprising (D2) an amino acid-derived anionic surfactant. [6] The dentifrice composition according to any one of [1] to [5], further comprising (D3) a sugar-based nonionic surfactant. [7] The dentifrice composition according to any one of [1] to [6], further comprising (D4) a chelating agent. [8] (D5) The dentifrice composition according to any one of [1] to [7], further comprising a water-soluble calcium compound. [Effects of the Invention]

[0009] According to the present invention, by containing glycerin, sorbitol, a specific water-soluble polymer, and a fluorine-containing compound, a dentifrice can be produced that is easy to use (easy to apply to a toothbrush, no stickiness in the oral cavity after rinsing) and has excellent storage stability (prevention of adhesion to the opening of the container). DETAILED DESCRIPTION OF THE INVENTION

[0010] The present invention will be described in detail below. [1. Components (A) to (D5) of Dentifrice Composition] The dentifrice composition contains components (A) to (C), and preferably further contains at least one of components (D1) to (D5).

[0011] [1.1 (A) Component: Sorbitol and / or glycerin] Component (A) is sorbitol and / or glycerin. The inclusion of component (A) not only imparts plasticity to the dentifrice composition, but also prevents the dentifrice from drying out at the opening of the container (e.g., the mouth of the tube) after it is filled into a container with an opening (e.g., a tube) and stored.

[0012] Component (A) may be either sorbitol or glycerin, or a combination of the two. In the case of a combination of the two, the blending ratio can be appropriately selected.

[0013] The content of component (A) is usually 15% by mass or more, preferably 20% by mass or more, and more preferably 25% by mass or more. This can further prevent drying at the container opening after filling and storage in a container. The upper limit is usually 47% by mass or less, preferably 45% by mass or less, and even more preferably 40% by mass or less. This can further prevent stringiness and sticky feeling after rinsing. It is usually 15 to 47% by mass, therefore, preferably 20 to 45% by mass, more preferably 25 to 45% by mass, and even more preferably 25 to 40% by mass.

[0014] [1.2 (B) Xanthan gum, sodium carboxymethylcellulose, sodium alginate] Component (B) is at least one selected from the group consisting of xanthan gum, sodium carboxymethylcellulose, and sodium alginate. By including component (B), syneresis of the dentifrice composition can be suppressed and shape retention can be improved.

[0015] Carboxymethyl cellulose sodium with an average degree of carboxymethyl group substitution (DS degree) of 0.5 to 1.5 is preferably used. Carboxymethyl cellulose sodium with a viscosity of 15 to 3,000 mPa·s (measured using a Brookfield viscometer at 20°C for a 2% aqueous solution; the same applies below). The above viscosity is measured using a Brookfield viscometer (e.g., manufactured by Toki Sangyo Co., Ltd.) with rotors 1 to 7 appropriate for the viscosity range. For example, when the viscosity is less than 100 mPa·s, the viscosity can be measured after 3 minutes at 50 rpm using rotor 1; when the viscosity is 100 mPa·s or higher, the viscosity can be measured after 3 minutes at 20 rpm using rotors 1 to 7. Examples of such carboxymethyl cellulose sodium include commercially available products such as CMC Daicel (sold by Daicel Miraize), Cellogen (sold by Daiichi Kogyo Seiyaku Co., Ltd.), and Sunrose (sold by Nippon Paper Industries Co., Ltd.).

[0016] Component (B) may be any one of xanthan gum, sodium carboxymethylcellulose, and sodium alginate, or a combination of two or more. When two or more are combined, the blending ratio can be selected appropriately. For example, when combining xanthan gum and sodium carboxymethylcellulose, the ratio of the two is usually xanthan gum:sodium carboxymethylcellulose=5-95:95-5, preferably 10-90:90-10, and more preferably 15-85:85-15. For example, in the case of a combination of xanthan gum and sodium alginate, the ratio of the two is usually xanthan gum:sodium alginate=10-90:90-10, preferably 15-85:85-15, more preferably 20-80:80-20. Furthermore, for example, in the case of a combination of sodium carboxymethylcellulose and sodium alginate, the ratio of sodium carboxymethylcellulose:sodium alginate is usually 5-95:95-5, preferably 10-90:90-10, more preferably 15-85:85-15.

[0017] The content of component (B) is usually 0.7% by mass or more, preferably 0.8% by mass or more, and more preferably 1% by mass or more. This can further prevent drying at the opening of the container after filling and storage in a container. The upper limit is usually 4% by mass or less, preferably 3% by mass or less, and more preferably 2.5% by mass or less. Therefore, it is usually 0.7 to 4% by mass, preferably 0.8 to 3% by mass, and more preferably 1 to 2.5% by mass. This can suppress stringiness and further prevent deterioration of the feel in use.

[0018] [1.3 Fluorine-containing compounds] Component (C) is a fluorine-containing compound. By including component (C), the feel of use of the dentifrice composition can be improved.

[0019] Examples of fluorine-containing compounds include sodium fluoride, sodium monofluorophosphate, and stannous fluoride.

[0020] The content of component (C), in terms of the amount of fluorine ions, is preferably 3,500 ppm or more, more preferably 4,500 ppm or more, and even more preferably 5,000 ppm or more. This further improves the feel during use. The upper limit is preferably 20,000 ppm or less, more preferably 15,000 ppm or less, and even more preferably 10,000 ppm or less. This further prevents drying at the opening of the container after filling and storage. Therefore, the content is preferably 3,500 to 20,000 ppm, more preferably 4,500 to 15,000 ppm, and even more preferably 5,000 to 10,000 ppm.

[0021] When component (C) contains sodium fluoride, its content is preferably 0.8% by mass or more, more preferably 1.0% by mass or more, and even more preferably 1.1% by mass or more, based on the total amount of the composition. The upper limit is preferably 4.4% by mass or less, more preferably 3.3% by mass or less, and even more preferably 2.2% by mass or less. Therefore, the content is preferably 0.8 to 4.4% by mass, more preferably 1.0 to 3.3% by mass, and even more preferably 1.1 to 2.2% by mass.

[0022] When component (C) contains sodium monofluorophosphate, its content is preferably 2.7% by mass or more, more preferably 3.4% by mass or more, and even more preferably 3.8% by mass or more, based on the total amount of the composition. The upper limit is preferably 15.2% by mass or less, more preferably 11.4% by mass or less, and even more preferably 7.6% by mass or less. Therefore, the content is preferably 2.7 to 15.2% by mass, more preferably 3.4 to 11.4% by mass, and even more preferably 3.8 to 7.6% by mass.

[0023] When component (C) contains stannous fluoride, its content is preferably 1.5% by mass or more, more preferably 1.9% by mass or more, and even more preferably 2.1% by mass or more, based on the total amount of the composition. The upper limit is preferably 8.3% by mass or less, more preferably 6.2% by mass or less, and even more preferably 4.1% by mass or less. Therefore, the content is preferably 1.5 to 8.3% by mass, more preferably 1.9 to 6.2% by mass, and even more preferably 2.1 to 4.1% by mass.

[0024] [1.4 C / B ratio] The ratio of the content of component (C) to component (B) can be expressed as the ratio of the fluorine ion amount (ppm) of component (C) to the content (% by mass) of component (B) (C / B ratio). The C / B ratio is preferably 1500 or more, more preferably 2000 or more. This can suppress spinnability, and in the case of a tube-shaped container, this can suppress a decrease in extrudability from the tube, thereby suppressing a sticky feeling after rinsing. The upper limit is preferably 20,000 or less, more preferably 10,000 or less, and even more preferably 6,000 or less. This can further improve the feel in use and prevent a decrease in storage stability (occurrence of liquid separation). Therefore, the C / B ratio is preferably 1500 to 20,000, more preferably 2,000 to 10,000, and even more preferably 2,000 to 6,000.

[0025] [1.5 (D1)~(D5)] The dentifrice composition may further contain at least one selected from the group consisting of the following components (D1) to (D5), thereby imparting the functionality attributable to each component to the dentifrice composition.

[0026] -(D1) Silica anhydride / hydroxyapatite / cellulose powder / granules- Component (D1) is an anhydrous silicic acid, hydroxyapatite, cellulose powder, or other granules. The inclusion of component (D1) can impart shape retention, stain removal, plaque removal, a clean feeling when brushing teeth, ease of rinsing, and the effect of inhibiting liquid separation to the dentifrice composition.

[0027] Examples of silicic anhydride include precipitated silica, pyrogenic silica, silica gel, titanium-bonded silica, aluminosilicate, and zirconosilicate, and may be abrasive silicic anhydride (abrasive silica) or thickening silicic anhydride (thickening silica). Examples of abrasive silica include those with a particle size of 1 μm to 40 μm and a BET specific surface area of ​​10 to 250 square meters per gram. Examples include Zeodent (registered trademark, hereinafter the same) 124, Zeodent 113, Zeodent 103, Zeodent 115, Sident (registered trademark, hereinafter the same) 3, Sident 9, and Sident 20, all manufactured by EVONIK; TIXOSIL (registered trademark, hereinafter the same) 73 and TIXOSIL 63, all manufactured by Rhodia; and zirconosilicate and aluminosilicate, all manufactured by Taki Chemical Industry Co., Ltd.

[0028] Examples of thickening silicic anhydride include thickening silica and aluminum silicate. Thickening silica can be silica obtained by a known manufacturing method and has a liquid absorption capacity in the range of 2 to 5 ml / g. The liquid absorption capacity is measured as follows: 1.0 g of sample is weighed onto a clean glass plate, and 42.5% glycerin is added dropwise using a microburette while the sample is mixed with a stainless steel spatula until the liquid becomes uniform. The end point is when the sample becomes a single mass and can be cleanly peeled off the glass plate with a spatula, and the amount of liquid (ml) consumed is recorded as the liquid absorption capacity. Examples of thickening silica include Tokusil manufactured by Tokuyama Corporation, SORBOSIL TC15 manufactured by PQ Corporation, TIXOSIL 43 manufactured by Rhodia, Zeodent 153 and Zeodent 165 manufactured by EVONIK, Carplex #67Q manufactured by DSL Japan, and Sylopure (registered trademark, the same applies hereinafter) 25 manufactured by Fuji Silysia Chemical Ltd.

[0029] The cellulose powder may be crystalline.

[0030] In this specification, granules refer to granulated particles formed by forming water-insoluble powders into granules. Granules may or may not contain a binder for granulation. Examples of granules include abrasive granules. Examples of water-insoluble powders include inorganic powders such as dibasic calcium phosphate, tribasic calcium phosphate, water-insoluble calcium metaphosphate, silica, aluminum hydroxide, magnesium phosphate, red iron oxide, calcium carbonate, calcium pyrophosphate, zeolite, aluminosilicate, magnesium carbonate, zirconosilicate, and calcium sulfate, as well as mixtures thereof.

[0031] Granules made from silica, zeolite, or titanium oxide are preferred, with silica granules, silica / zeolite / titanium oxide granules, and colored granules thereof being more preferred. The volume-average particle size (median diameter d50) of the granules is preferably 50 to 500 μm, and the average disintegration strength is preferably 10 to 200 g / granule. The average disintegration strength is the average of the automatic breaking strength values ​​(measured as the load at which one granule disintegrates when compressed at a rate of 10 mm / min) of 30 granules measured using a rheometer (e.g., Sun Rheometer CR-200D, manufactured by Sun Scientific Co., Ltd.).

[0032] Preferred silica granules are wet-processed gel silica and precipitated silica. The primary particle size of silica granules is typically 3 to 15 nm, preferably 4 to 10 nm. Examples of methods for producing silica granules include: a method in which silica gel lumps grown by the gel process to a primary particle size of approximately 4 to 10 nm are washed, dried, pulverized, and classified to produce silica granules with an average particle size of 50 to 500 μm; a method in which silica hydrosol is sprayed into air to gel; and a method in which primary particles are aggregated by the precipitation process while suppressing their growth, and then grown to a primary particle size of approximately 4 to 10 nm. Among these, a method in which silica gel lumps prepared by the gel process are pulverized is preferred. This method is simple to produce and allows for easy control of the average particle size by classification. Granules with appropriate average disintegration strength can be obtained by preparing the granules using the above methods.

[0033] Commercially available silica granules having such average particle size and average disintegration strength can be used, such as SORBOSIL BFG10 and SORBOSIL BFG50 manufactured by PQ Corporation, NIPGEL (registered trademark, the same applies hereinafter) AY and NIPGEL BY-001 manufactured by Tosoh Silica Corporation, and SYLOPURE30, SYLOPURE39, SYLOPURE40, SYLOPURE50, and SYLOPURE60 manufactured by Fuji Silysia Chemical Ltd.

[0034] An example of a silica / zeolite / titanium oxide granule is COLITE TG manufactured by Cosmo Co., Ltd. Examples of colored granules include SORBOSIL BFG51, SORBOSIL BFG52, and SORBOSIL BFG54 manufactured by PQ Corporation.

[0035] The component (D1) may be one selected from the above granules, or a combination of two or more selected from them. In the case of a combination of two or more selected from them, the blending ratio can be appropriately selected.

[0036] The content of component (D1) is preferably 5% by mass or more, more preferably 7% by mass or more, and even more preferably 10% by mass or more. The upper limit is preferably 30% by mass or less, more preferably 25% by mass or less, and even more preferably 20% by mass or less. Therefore, it is preferably 5 to 30% by mass, more preferably 7 to 25% by mass, and even more preferably 10 to 20% by mass. By keeping it within the above range, the effects of containing component (D1) can be more efficiently exerted.

[0037] The ratio of the contents of component (C) and component (D1) can be expressed as the ratio (C / D1 ratio) of the amount of fluorine ions (ppm) in component (C) to the amount (mass%) of component (D1). The C / D1 ratio is preferably 100 or more, more preferably 150 or more, and even more preferably 200 or more. The upper limit is preferably 2000 or less, more preferably 1500 or less, and even more preferably 1000 or less. Therefore, the range is preferably 100 to 2000, more preferably 150 to 1500, and even more preferably 200 to 1000. By keeping the ratio within the above range, the effects of the present invention can be more efficiently exhibited.

[0038] -(D2) Amino acid-based anionic surfactants- Component (D2) is an amino acid-based anionic surfactant. The inclusion of component (D2) can impart to the dentifrice composition the following benefits: sterilization, a soft foaming sensation during brushing, a refreshing feeling after brushing, fluoride stability, and the stability of oil-soluble ingredients such as vitamin E and isopropylmethylphenol.

[0039] Amino acid-based anionic surfactant is usually acylamino acid salt, acyltaurine salt.As acylamino acid salt, for example, acylsarcosine salt such as lauroyl sarcosine salt, myristoyl sarcosine salt; acylglutamate such as lauroyl glutamate, myristoyl glutamate, palmitoyl glutamate; acylglycine salt such as N-lauroyl-N-methylglycine salt, cocoylglycine salt; acylalanine salt such as N-lauroyl-β-alanine salt, N-myristyl-β-alanine salt, N-cocoyl-β-alanine salt, N-lauroyl-N-methyl-β-alanine salt, N-myristoyl-N-methyl-β-alanine salt, N-methyl-N-acylalanine salt; acyl aspartate such as lauroyl aspartate. Examples of acyltaurine salts include lauroyl methyl taurine salt, N-methyl-N-acyltaurine salt, and N-cocoyl methyl taurine salt. Among these, lauroyl sarcosine salt (for example, sodium lauroyl sarcosine) and lauroyl methyl taurine salt (for example, sodium lauroyl methyl taurine) are preferred, and sodium lauroyl sarcosine, lauroyl methyl taurine salt (for example, sodium lauroyl methyl taurine) and sodium lauroyl glutamate are more preferred.

[0040] The component (D2) may be one type of amino acid-based anionic surfactant, or a combination of two or more types. In the case of a combination of two or more types, the blending ratio can be selected appropriately.

[0041] The content of component (D2) is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, and even more preferably 0.3% by mass or more. The upper limit is preferably 2% by mass or less, more preferably 1.8% by mass or less, and even more preferably 1.5% by mass or less. Therefore, it is preferably 0.1 to 2% by mass, more preferably 0.2 to 1.8% by mass, and even more preferably 0.3 to 1.5% by mass. By keeping it within the above range, the effects of containing component (D2) can be more efficiently exerted.

[0042] The ratio of the contents of component (C) and component (D2) can be expressed as the ratio (C / D2 ratio) of the amount of fluorine ions (ppm) in component (C) to the amount (mass%) of component (D2). The C / D2 ratio is preferably 2,000 or more, more preferably 3,000 or more. The upper limit is preferably 150,000 or less, more preferably 100,000 or less, and even more preferably 50,000 or less. Therefore, the range is preferably 2,000 to 150,000, more preferably 2,000 to 100,000, and even more preferably 3,000 to 50,000. By keeping the ratio within the above range, the effects of the present invention can be more efficiently exhibited.

[0043] -(D3) Sugar-based nonionic surfactant- Component (D3) is a sugar-based nonionic surfactant. The inclusion of component (D3) can impart to the dentifrice composition storage stability of cationic disinfectants, suppression of liquid separation, a smooth feeling during brushing, stability of oil-soluble ingredients such as vitamin E, isopropylmethylphenol, β-glycyrrhetinic acid or a salt thereof (e.g., stearyl β-glycyrrhetinate), promotion of gum adsorption of oil-soluble ingredients such as vitamin E, isopropylmethylphenol, β-glycyrrhetinic acid, and the like, and good foam retention during brushing.

[0044] Sugar-based nonionic surfactants are nonionic surfactants that contain a sugar-derived moiety in their structure. Examples of sugars include glucose and sucrose. Examples of sugar-based nonionic surfactants include alkyl glucosides and sucrose fatty acid esters (e.g., sucrose laurate). The component (D3) may be one type of sugar-based nonionic surfactant, or a combination of two or more types. When two or more types are combined, the blending ratio can be selected appropriately.

[0045] The content of component (D3) is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, and even more preferably 0.3% by mass or more. The upper limit is preferably 5% by mass or less, more preferably 3% by mass or less, and even more preferably 2% by mass or less. Therefore, it is preferably 0.1 to 5% by mass, more preferably 0.2 to 3% by mass, and even more preferably 0.3 to 2% by mass. By keeping it within the above range, the effects of containing component (D3) can be more efficiently exerted.

[0046] The ratio of the contents of component (C) and component (D3) can be expressed as the ratio (C / D3 ratio) of the fluorine ion amount (ppm) of component (C) to the content (mass%) of component (D3). The C / D3 ratio is preferably 500 or more, more preferably 2000 or more, and even more preferably 3000 or more. The upper limit is preferably 150,000 or less, more preferably 50,000 or less, and even more preferably 30,000 or less. Therefore, the range is preferably 500 to 150,000, more preferably 2,000 to 50,000, and even more preferably 3,000 to 30,000. By keeping the C / D3 ratio within the above range, the effects of the present invention can be more efficiently exhibited.

[0047] -(D4) Chelating agent- Component (D4) is a chelating agent. By including component (D4), the dentifrice composition can be provided with a refreshing feeling during and after brushing, stain dissolution, a gum astringent feeling during and after brushing, pH stability, enhanced bactericidal activity, and retention of the cationic bactericide in the oral cavity.

[0048] Examples of chelating agents include condensed phosphoric acid and organic acids. Examples of condensed phosphoric acid include linear polyphosphoric acids such as pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, and polyphosphoric acids with higher polymerization degrees, as well as their salts; and cyclic polyphosphoric acids such as trimetaphosphoric acid, tetrametaphosphoric acid, and hexametaphosphoric acid. Examples of organic acids include oxalic acid, malonic acid, maleic acid, fumaric acid, lactic acid, malic acid, tartaric acid, citric acid, pyruvic acid, oxaloacetic acid, aspartic acid, succinic acid, glucuronic acid, adipic acid, phytic acid, phthalic acid, and acetic acid. Among these, pyrophosphoric acid, polyphosphoric acid, phytic acid, hexametaphosphoric acid, malic acid, citric acid, and their salts are preferred. Examples of salts include alkali metal salts such as sodium salts and potassium salts, and alkaline earth metal salts such as calcium salts. The (D4) component may be one of the chelating agents or a combination of two or more of them. The condensed phosphoric acid and organic acid may be in the form of a salt. When two or more types are combined, the blending ratio can be appropriately selected.

[0049] The content of component (D4) is preferably 0.1% by mass or more, more preferably 0.3% by mass or more, and even more preferably 0.5% by mass or more. The upper limit is preferably 5% by mass or less, more preferably 3% by mass or less, and even more preferably 2% by mass or less. Therefore, it is preferably 0.1 to 5% by mass, more preferably 0.3 to 3% by mass, and even more preferably 0.5 to 2% by mass. By keeping it within the above range, the effects of containing component (D4) can be more efficiently exerted.

[0050] The ratio of the contents of component (C) and component (D4) can be expressed as the ratio (C / D4 ratio) of the amount of fluorine ions (ppm) in component (C) to the amount (mass%) of component (D4). The C / D4 ratio is preferably 1,000 or more, more preferably 2,000 or more, and even more preferably 2,500 or more. The upper limit is preferably 150,000 or less, more preferably 20,000 or less, and even more preferably 12,000 or less. Therefore, the range is preferably 1,000 to 150,000, more preferably 2,000 to 20,000, and even more preferably 2,500 to 12,000. By keeping the C / D4 ratio within the above range, the effects of the present invention can be more efficiently exhibited.

[0051] -(D5) Water-soluble calcium compounds- Component (D5) is a water-soluble calcium compound. By including component (D5), the dentifrice composition can be provided with the effects of fluoride adsorption to teeth and the effect of imparting a moderate astringent taste during brushing.

[0052] As used herein, a water-soluble calcium compound is a compound that is water-soluble and contains calcium. As used herein, water-soluble means having a solubility of at least 0.1 g per 100 g of water at pH 7 at 25°C. Examples include calcium salts of inorganic acids such as calcium chloride, calcium nitrate, calcium sulfate, and monocalcium phosphate; and calcium salts of organic acids such as calcium lactate, calcium gluconate, calcium acetate, calcium pantothenate, calcium propionate, calcium formate, and calcium glycerophosphate. Calcium glycerophosphate, calcium chloride, and calcium lactate are preferred. The (D5) component may be one water-soluble calcium compound or a combination of two or more of them. When two or more water-soluble calcium compounds are used in combination, the blending ratio can be appropriately selected.

[0053] The content of component (D5) is preferably 0.1% by mass or more, more preferably 0.3% by mass or more, and even more preferably 0.5% by mass or more. The upper limit is preferably 5% by mass or less, more preferably 3% by mass or less, and even more preferably 2% by mass or less. Therefore, it is preferably 0.1 to 5% by mass, more preferably 0.3 to 3% by mass, and even more preferably 0.5 to 2% by mass. By keeping it within the above range, the effects of containing component (D5) can be more efficiently exerted.

[0054] The ratio of the contents of component (C) and component (D5) can be expressed as the ratio (mass %) of the fluorine ion amount (ppm) of component (C) to the content (mass %) of component (D5) (C / D5 ratio). The C / D5 ratio is preferably 1,000 or more, more preferably 1,500 or more, even more preferably 2,000 or more, and even more preferably 2,500 or more. The upper limit is preferably 150,000 or less, more preferably 50,000 or less, even more preferably 20,000 or less, and even more preferably 12,000 or less. Therefore, the range is preferably 1,000 to 150,000, more preferably 1,500 to 50,000, even more preferably 2,000 to 20,000, and even more preferably 2,500 to 12,000. By keeping the C / D5 ratio within the above range, the effects of the present invention can be more efficiently exhibited.

[0055] [2.Optional ingredients] The dentifrice composition contains optional ingredients other than (A), (B), (C), and (D1) to (D5). Examples of optional ingredients include abrasives, binders, surfactants, humectants, sweeteners, flavorings, cooling agents, pH adjusters, preservatives, medicinal ingredients, colorants, water, emulsifying oily ingredients, etc., and these can be selected as needed within a range that does not impair the effects of the present invention. The optional ingredients can be used alone or in combination of two or more.

[0056] [2.1 Abrasives] Abrasives are components other than components (A) to (D5), and examples include calcium phosphate compounds such as dibasic calcium phosphate dihydrate or anhydrate, monobasic calcium phosphate, tribasic calcium phosphate, and calcium pyrophosphate; calcium carbonate (light and heavy), calcium sulfate, calcium hydroxide, and other calcium-based abrasives; sodium bicarbonate; aluminum-based materials other than aluminum oxide, such as aluminum hydroxide and alumina; silicate-based materials such as zeolite and zirconium silicate; magnesium-based materials such as magnesium carbonate and tribasic magnesium phosphate; apatite-based materials such as fluoroapatite and calcium-deficient apatite; titanium-based materials such as titanium dioxide and titanium mica; and minerals such as bentonite. Examples of organic abrasives include polymethyl methacrylate and synthetic resin-based abrasives. Abrasives may be used alone or in combination.

[0057] When an abrasive is contained, the content thereof is usually 5 to 70 mass %, and preferably 10 to 50 mass %, based on the total amount of the composition.

[0058] [2.2 Binder] The binder is a component other than components (A) to (D5), and examples thereof include cellulose-based binders (e.g., hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropylmethyl cellulose, methyl cellulose, cationized cellulose, etc.), polysaccharide-based thickeners (e.g., guar gum, gellan gum, tragacanth gum, karaya gum, gum arabic, locust bean gum, carrageenan), and synthetic water-soluble polymers (e.g., sodium polyacrylate, carboxyvinyl polymer, carbopol, polyvinylpyrrolidone, polyvinyl alcohol, propylene glycol alginate, methyl vinyl ether / maleic anhydride copolymer). Also included are inorganic binders such as Veegum. One type of binder may be used alone, or two or more types may be used in combination.

[0059] When a binder is contained, the content thereof is usually 10% by mass or less, preferably 0.1 to 10% by mass, and more preferably 1 to 8% by mass, based on the total amount of the composition.

[0060] [2.3 Surfactants] The surfactant is a component other than the components (A) to (D5), and examples thereof include anionic surfactants other than amino acid-based surfactants, nonionic surfactants other than sugar-based surfactants, and amphoteric surfactants. One or more of these surfactants can be used.

[0061] -Anionic surfactants- Examples of anionic surfactants include alkyl sulfates, α-olefin sulfonates, hydrogenated coconut fatty acid monoglyceride monosulfates, and lauryl sulfoacetates. The alkyl and acyl groups may be linear or branched, saturated or unsaturated, and typically contain 10 to 20 carbon atoms, preferably 12 to 18, and more preferably 12 to 14. The salts may be selected from pharmacologically acceptable salts. Examples of pharmacologically acceptable salts include base addition salts and amino acid salts. Specific examples include inorganic base salts such as sodium salts, potassium salts, calcium salts, magnesium salts, and ammonium salts; organic base salts such as triethylammonium salts, triethanolammonium salts, pyridinium salts, and diisopropylammonium salts; and basic amino acid salts such as arginine salts. Among these, inorganic base salts are preferred, with alkali metal salts (e.g., sodium salts and potassium salts) and ammonium salts being more preferred, and sodium salts being even more preferred.

[0062] Examples of alkyl sulfates include lauryl sulfate (sodium lauryl sulfate) and myristoyl sulfate. Examples of α-olefin sulfonates include α-olefin sulfonates having 12 to 18 carbon atoms, such as tetradecene sulfonate. Other examples of anionic surfactants include hydrogenated coconut fatty acid monoglyceride sodium monosulfate and sodium lauryl sulfoacetate.

[0063] The anionic surfactant preferably contains a sulfonic acid group, and more preferably an alkyl sulfate, from the viewpoint of foaming ability and foam quality. When an anionic surfactant is contained, its content is usually 0.4 to 2 mass %, preferably 0.8 to 1.8 mass %, based on the total amount of the composition.

[0064] -Nonionic surfactants- Examples of nonionic surfactants include polyoxyethylene alkyl ethers (e.g., polyoxyethylene stearyl ether), polyoxyethylene hydrogenated castor oil, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters (e.g., polyoxyethylene sorbitan monostearate), alkylolamides, polyoxyethylene fatty acid esters, polyoxyethylene alkenyl ethers, (poly)glycerin fatty acid esters (e.g., polyglyceryl monolaurate), sugar alcohol fatty acid esters (e.g., maltitol fatty acid esters, lactitol fatty acid esters), fatty acid diethanolamides (e.g., lauric acid mono- or diethanolamide), polyoxyethylene polyoxypropylene copolymers, and polyoxyethylene polyoxypropylene fatty acid esters. The number of carbon atoms in the alkyl chain of the polyoxyethylene alkyl ether is typically 14 to 18, and the average number of moles of ethylene oxide added is typically 5 to 30. The average number of moles of ethylene oxide added in polyoxyethylene hydrogenated castor oil is typically 20 to 100 moles, preferably 20 to 60 moles, and more preferably 10 to 60. The number of carbon atoms in the fatty acid of the sorbitan fatty acid ester is usually 12 to 18. The number of carbon atoms in the fatty acid of the polyoxyethylene sorbitan fatty acid ester is usually 16 to 18, and the average number of moles of ethylene oxide added is usually 10 to 40. The number of carbon atoms in the alkyl chain of the alkylolamide is usually 12 to 14. As the nonionic surfactant, polyoxyethylene hydrogenated castor oil is preferred.

[0065] When a nonionic surfactant is contained, its content is generally 0.05% by mass or more, or 0.1% by mass or more, preferably 0.3% by mass or more, based on the total amount of the composition, and the upper limit is generally 3% by mass or less, or 2% by mass or less, preferably 1.5% by mass or less.

[0066] -Amphoteric surfactant- Examples of amphoteric surfactants include amidopropyl betaine amphoteric surfactants, acetic acid betaine amphoteric surfactants, imidazoline amphoteric surfactants, amine oxide amphoteric surfactants, etc. When an amphoteric surfactant is contained, the content thereof is usually 0.1 to 5% by mass, and preferably 0.3 to 1% by mass, relative to the total amount of the composition.

[0067] When a surfactant is contained, the content thereof (total amount when multiple surfactants are contained) is usually preferably 0.001 to 10% by mass relative to the total amount of the composition.

[0068] 2.4 Wetting Agents The humectant is a component other than the components (A) to (D5), and examples thereof include sugar alcohols such as xylitol and erythritol, and polyhydric alcohols such as propylene glycol, ethylene glycol, 1,3-butylene glycol, and polyethylene glycol (PEG). Examples of polyethylene glycol include polyethylene glycols having an average molecular weight of 150 to 6,000, preferably 190 to 630. Specific examples include PEG200, PEG300, PEG400, and PEG600. The average molecular weight is the average molecular weight described in the Quasi-drug Raw Materials Standards 2021. When a humectant is included, its content is typically 1 to 70% by mass, preferably 1 to 50% by mass, more preferably 1 to 40% by mass, 3 to 40% by mass, or 3 to 30% by mass, based on the total amount of the composition.

[0069] [2.5 Sweeteners] Examples of sweeteners include saccharin, saccharin sodium, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, perlartine, glycyrrhizin, thaumatin, aspartyl phenylalanine methyl ester, and aspartame.

[0070] [2.6 Fragrances and cooling agents] The fragrance may be any known fragrance, such as peppermint oil, refined peppermint oil, spearmint oil, refined spearmint oil, Japanese peppermint oil, refined Japanese peppermint oil, anise oil, cassia oil, eucalyptus oil, wintergreen oil, mastic oil, neroli oil (orange flower oil), lemongrass oil, jasmine oil, rose oil, iris oil, clove oil, thyme oil, sage oil, cardamom oil, rosemary oil, laurel oil, chamomile oil, caraway oil, basil oil, marjoram oil, lemon oil, refined lemon oil, orange oil, refined orange oil, lime oil, grapefruit oil, mandarin oil, yuzu oil, nutmeg oil, lavender oil, paraben, etc. Natural essential oils such as cress oil, vanilla oil, cinnamon oil, pimento oil, cinnamon leaf oil, perilla oil, wintergreen oil, and coriander oil; fragrance components contained in the above natural essential oils such as menthol, carvone, cinnamic aldehyde, p-methoxycinnamic aldehyde, anethole, 1,8-cineole, methyl salicylate, eugenol, thymol, linalool, limonene, menthone, menthyl acetate, citral, decanal, camphor, borneol, pinene, spilanthol, n-decyl alcohol, citronellol, α-terpineol, citronellyl acetate, ethyl linalool, and vanillin;Ethyl acetate, ethyl butyrate, isoamyl acetate, hexanal, hexenal, cis-3-hexenol, trans-2-hexenol, trans-2-hexenal, methyl anthranilate, ethyl methylphenylglycidate, benzaldehyde, ethyl vanillin, furaneol, menthofuran, undecalactone, decalactone, linalool oxide, vanillyl butyl ether, hexyl acetate, ethyl 2-methylbutyrate, benzyl alcohol, linalyl acetate, phenylethyl glycidate, phenylethyl alcohol, allyl hexanoate, octanol, methyl cinnamate, methylheptyne carbonate, ionone, ethyl-β-methylthiopropionate, cinnamal Examples of suitable fragrance ingredients include 6-nonenol, calone, methyl jasmonate, maltol, ethyl maltol, furaneol, ethyl cyclopentenolone, 3-hydroxy-4,5-dimethylfuran-2-one, cyclotene, 2-methylbutyric acid, acetic acid, propionic acid, and 7-methyl-2H-1,5-benzodioxepin-3(4H)-one; plant extracts such as chili pepper extract, ginger extract, pepper extract, and Japanese pepper extract; various blended flavors such as mint, fruit, and herb flavors, which are combinations of fragrance ingredients and natural essential oils; and fragrance solvents such as ethyl alcohol, propylene glycol, triacetin, and glycerin fatty acid esters. The above-listed fragrances may be used alone or in combination of two or more. When a fragrance is included, the content thereof is typically 0.000001 to 1% by mass, preferably 0.01 to 1% by mass, based on the total amount of the composition. ;

[0071] Examples of cooling agents include N-ethyl-p-menthane-3-carboxamide (WS-3), ethyl-3-(p-menthane-carboxamide) acetate (WS-5), N-(4-cyanomethylphenyl)-p-menthanecarboxamide (EVERCOOL180), N-(2-(pyridin-2-yl)-3-p-menthanecarboxamide) (EVERCOOL190), 2-isopropyl-N,2,3-trimethylbutyramide (WS-23), menthone glycerol acetal (MGA), N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide, N-[(ethoxycarbonyl)methyl] ... Examples of the cooling agent include [2-(4-methylphenoxy)-N-(1H-pyrazol-yl)-N-(thiophen-2-ylmethyl)acetamide, 3-l-menthoxypropane-1,2-diol, menthyl lactate, menthyl succinate (menthyl succinate), menthyl glyceryl ether, and isopulegol. When a cooling agent is contained, the content thereof is preferably 0.00001 to 0.01% by mass relative to the total amount of the composition.

[0072] [2.7 pH adjuster] The pH adjuster is a component other than the components (A) to (D5), and examples thereof include inorganic compounds such as hydrochloric acid, sodium hydroxide, potassium hydroxide, disodium hydrogen phosphate, and sodium dihydrogen phosphate.

[0073] [2.8 Preservatives] Examples of preservatives include parahydroxybenzoates and sodium benzoate.

[0074] [2.9 Medicinal ingredients] The medicinal ingredient (medicinal ingredient) is a component other than the components (A) to (D5), and examples thereof include enzymes such as dextranase, amylase, protease, and mutanase; anti-inflammatory agents such as tranexamic acid, ε-aminocaproic acid, allantoin, aluminum chlorohydrate allantoin, azulene, and glycyrrhizinic acid or a salt thereof (e.g., dipotassium glycyrrhizinate); cell activators such as sodium chloride and vitamins; isopropylmethylphenol, cetylpyridinium chloride, benzalkonium chloride, benzethonium chloride, hinokitiol, thymol, lysozyme chloride, chlorhexidine, triclosan, and hypoglycerin. Examples of suitable antiseptic or antibacterial agents include lead, zinc citrate, and the like; water-soluble copper compounds such as copper chlorophyll, copper gluconate, and the like; anti-tartar agents such as zeolite, ethanehydroxydiphosphonate, and polyphosphates; blood circulation promoters such as vitamin E; vitamins such as vitamin C (e.g., ascorbic acid), vitamin E (e.g., tocopherol acetate, tocopherol nicotinate, and tocopherol), and pyridoxine, astringents such as sodium chloride, alum, and lysozyme chloride, hypersensitivity inhibitors such as potassium nitrate, aluminum lactate, and strontium chloride, amino acids such as alanine, glycine, and proline, and peptides such as callopeptides. When a medicinal ingredient is contained, the content thereof can be an effective amount within a range that does not interfere with the effects of the present invention (a pharmaceutically acceptable range).

[0075] [2.10 Oil-based ingredients for emulsification] Examples of oily emulsifying components include light liquid paraffin, liquid paraffin, stearyl alcohol, stearic acid, and cetanol.

[0076] 2.11 Colorants The colorant is a component other than components (A) to (D5), and examples thereof include natural pigments such as safflower red pigment, gardenia yellow pigment, gardenia blue pigment, perilla pigment, monascus koji pigment, red cabbage pigment, carrot pigment, hibiscus pigment, cacao pigment, spirulina blue pigment, and tamarind pigment, as well as legally designated pigments such as Red No. 2, Red No. 3, Red No. 104, Red No. 105, Red No. 106, Red No. 227, Yellow No. 4, Yellow No. 5, Green No. 3, and Blue No. 1, riboflavin, sodium copper chlorophyll, and titanium dioxide. When a colorant is contained, the content thereof is typically 0.00001 to 3% by mass of the total amount of the composition.

[0077] 2.11 Other optional ingredients Optional components other than those mentioned above include, for example, inorganic compounds such as mica titanium, titanium oxide, zinc oxide, magnesium oxide, and zirconium oxide; natural polymer compounds such as agar, gelatin, starch, and glucomannan; synthetic polymer compounds or copolymers thereof such as polyvinyl acetate, acrylic resin, polyurethane, polyester, polyvinyl chloride, nylon powder, and polyethylene powder; waxes such as carnauba wax, rosin, rice wax, microcrystalline wax, beeswax, and paraffin wax; higher alcohols such as cetanol and stearyl alcohol; polyisobutylene, polybutadiene, urethane, silicone, and natural rubber.

[0078] [3. Formulation, manufacturing method, and physical properties of dentifrice composition] The dentifrice composition of the present invention can be prepared in the form of a paste, gel, or the like, and can be prepared as a toothpaste, liquid toothpaste, or the like, especially as a toothpaste. There are no particular restrictions on the production method, and conventional methods can be used depending on the dosage form.

[0079] The pH (25°C) of the dentifrice composition is preferably 5.0 to 9.0. The pH can be adjusted by adding a pH adjuster, adjusting the component composition, etc. In this specification, the pH value generally refers to the value measured at 25°C, 3 minutes after the start of measurement. The pH value can be measured, for example, using a pH meter (model number Hm-30S) manufactured by Toa Denpa Kogyo Co., Ltd.

[0080] The viscosity of the dentifrice composition can be adjusted appropriately depending on the dosage form, etc. For example, the viscosity of a paste or gel dentifrice composition is preferably 30 to 150 Pa s. In this specification, viscosity refers to the viscosity at 25°C measured using a BH viscometer (B-type viscometer). [Example]

[0081] The present invention will be described in detail below with reference to examples and comparative examples, but the present invention is not limited to the following examples. In the following examples, unless otherwise specified, "%" in the composition indicates % by mass, and the ratio indicates the mass ratio.

[0082] Examples 1 to 23 and Comparative Examples 1 to 6 Test products (toothpastes) were manufactured by blending the raw materials listed in Tables 1 to 3 and subjected to testing. [Raw materials used] Sorbitol: D-sorbitol solution / Mitsubishi Corporation Life Sciences Co., Ltd. Glycerin: Cosmetic glycerin / Sakamoto Pharmaceutical Industry Co., Ltd. Xanthan gum: Monart Gum DA / CP manufactured by Kelco Co., Ltd. Sodium carboxymethylcellulose: CMC1260 / manufactured by Daicel Millize Co., Ltd. (Etherification degree: 0.94) Sodium alginate: Kimica Algin / Kimica Co., Ltd. Sodium fluoride: Sodium fluoride / Stella Chemifa Corporation Sodium Monofluorophosphate: Sodium Monofluorophosphate / Taihei Chemical Industry Co., Ltd. Stannous fluoride: Tin(II) fluoride / Fujifilm Wako Pure Chemical Industries, Ltd. Fragrance Fragrance A (Table 4)

[0083] (1) Manufacturing method The test samples were prepared by a conventional method and filled into laminated tubes with a diameter of 23 mm for testing.

[0084] (2) Threadability (ease of application to toothbrush) The test product filled into a 23 mm diameter laminated tube was extruded onto straw paper, and the tube was slowly lifted up to evaluate its spinnability. Evaluation was based on the following criteria. The evaluation was carried out three times, and an average of less than 20 mm was considered to be acceptable.

[0085] Evaluation criteria 4 points: Stringiness is 0-5mm 3 points: Stringiness 5-10mm 2 points: Threadability 10-20mm 1 point: Stringiness is 20mm or more

[0086] ·Judgment criteria A (Excellent): Average value is less than 10 mm B (Good): Average value is less than 10-20mm C (unacceptable): average value is 20 mm or more

[0087] (3) Usability (no stickiness in the mouth after rinsing) The test product was placed in a 23mm diameter laminated tube, and approximately 15mm of it was placed on a toothbrush. The patient brushed their teeth in the usual way for two minutes, then rinsed their mouth twice with 20mL of water, after which the feeling of the stickiness in the mouth was evaluated. The evaluation was carried out by 10 people, who evaluated it according to the following evaluation criteria, and the average score of the 10 people was used to judge. A score of 4.0 or above was considered a pass.

[0088] Evaluation criteria 5 points: No stickiness felt in the mouth after rinsing 4 points: After rinsing, the mouth felt slightly sticky 3 points: After rinsing, I felt a sticky feeling in my mouth. 2 points: After rinsing, the mouth felt slightly sticky 1 point: After rinsing, the mouth felt very sticky

[0089] ·Judgment criteria A: The average score of 10 people is 4.5 points or more B: The average value of 10 people is less than 4.0 to 4.5 points C: The average value of 10 people is less than 3.0 to 4.0 points D: The average value of 10 people is less than 3.0 points

[0090] (4) Storage stability (dryness of the tube opening) The test product was filled into a 23 mm diameter laminated tube, and the cap was left half-open. After two weeks of storage at 40°C and 75% RH, the condition of the opening was observed, and the condition (extrusion property) when extruded onto straw paper was evaluated according to the following criteria. The evaluation was carried out three times, and an average score of 3.0 or higher was considered to be acceptable.

[0091] Evaluation criteria 5 points: No solidification was observed at the mouth, and there were no problems with extrusion 4 points: Some solidification was observed around the mouth, but there was no problem with extrusion 3 points: Some solidification was observed around the mouth, making it difficult to extrude 2 points: Solidification was observed around the mouth, making it difficult to extrude 1 point: Solidification was observed at the mouth and it was not possible to extrude

[0092] ·Judgment criteria A: Average score is 4.0 or above B: Average score is 3.0 or more and less than 4.0 C: Average score is 2.0 or more and less than 3.0 D: Average score is less than 2.0 points

[0093] [Table 1]

[0094] [Table 2]

[0095] [Table 3]

[0096] [Table 4]

[0097] [Table 5]

[0098] [Table 6]

[0099] [Table 7]

[0100] [Table 8]

[0101] The test products of the comparative examples were rated low in either spinnability, storage stability, or usability, while all three test products of the examples were rated high. Furthermore, test products prepared in the same manner as the above examples, except that flavors B to P (Tables 4 to 5) were used instead of flavor A, also received ratings similar to those of the examples shown in Tables 1 to 3. These results demonstrate that the dentifrice composition of the present invention has both usability and storage stability.

[0102] Examples 24 to 74 Test products (toothpastes) were manufactured and subjected to the tests by blending the raw materials shown in Tables 9 to 14. The raw materials used other than those shown below were the same as those used in Tables 1 to 4.

[0103] [Raw materials used] Silica anhydride-1 (abrasive): Zeodent 124 (Evonik Japan Co., Ltd.) Silica anhydride-2 (abrasive): NIPGEL AY (Tosoh Silica Corporation) Sodium lauroyl methyl taurate: NIKKOL LMT-P (Nippon Chemicals Co., Ltd.) Sodium lauroyl sarcosinate: NIKKOL Sarcosinate LN (Nikko Chemicals Co., Ltd.) Sodium lauroyl glutamate: Sodium lauroyl glutamate (Asahi Kasei Chemicals Corporation) Sucrose laurate: Sucrose fatty acid ester C-1216 (Mitsubishi Chemical Foods Corporation) Alkyl glucoside: Plantacare® 1200UP, (BASF, C12-16) Isopropylmethylphenol: 3-methyl-4-isopropylphenol (Osaka Chemical Industry Co., Ltd.) Vitamin E: dl-α-tocopherol acetate (DSM Nutrition Japan Co., Ltd.) Sodium polyphosphate: Sodium polyphosphate (Taihei Chemical Industry Co., Ltd.) Sodium hexametaphosphate: Sodium hexametaphosphate (Taihei Chemical Industry Co., Ltd.) Malic acid: DL-malic acid (Fujifilm Wako Pure Chemical Industries, Ltd.) Sodium pyrophosphate: Sodium pyrophosphate (Taihei Chemical Industry Co., Ltd.) Calcium lactate: Calcium lactate (Taihei Chemical Industry Co., Ltd.) Calcium glycerophosphate: Calcium glycerophosphate (Iwaki Pharmaceutical Co., Ltd.)

[0104] (5) Manufacturing method The test samples were prepared by a conventional method. The prepared test samples were filled into laminated tubes with an opening diameter of 8 mm and subjected to the test.

[0105] Of the following tests, all tests except for isopropylmethylphenol stability and vitamin E stability were conducted as sensory tests using a panel of 10 experts.

[0106] (6) Brushing sensation Approximately 1g of the test product, packed in an 8mm diameter laminated tube, was placed on a toothbrush (Clinica Advantage toothbrush, 4-row compact normal, manufactured by Lion Corporation), and brushed for 3 minutes, after which the brushing sensation in the oral cavity during use was evaluated. The evaluation was carried out by 10 people, who evaluated using the following evaluation criteria, and judged the average of the 10 people, with an average score of 3.0 points or more (criteria A and B) being considered a pass.

[0107] Evaluation criteria 4 points: Strong feeling of brushing 3 points: Feels like you are brushing 2 points: Somewhat felt like brushing 1 point: Almost no brushing sensation

[0108] ·Judgment criteria A: Average score is between 3.5 and 4.0 points B: Average score is between 3.0 and 3.5 C: Average score is between 2.0 and 3.0 points D: Average score is less than 2.0 points

[0109] (7) Ease of rinsing Approximately 1 g of the test product (toothpaste) packed in an 8 mm diameter laminated tube was placed on a toothbrush (Clinica Advantage Toothbrush, 4-row compact normal, manufactured by Lion Corporation), brushed for 3 minutes, and then rinsed twice with approximately 20 mL of water, after which the ease of rinsing (how little toothpaste remained in the mouth) was evaluated. The evaluation was carried out by 10 people, who evaluated using the following evaluation criteria, and the average of the 10 people was judged. An average score of 2.0 points or more (criteria A and B) was considered a pass.

[0110] Evaluation criteria 3 points: It felt like there was no toothpaste left in the mouth 2 points: Some toothpaste felt left in the mouth 1 point: Feeling that toothpaste remains in the mouth

[0111] ·Judgment criteria A: Average score is between 2.5 and 3.0 points B: Average score is between 2.0 and 2.5 points C: Average score is less than 2.0 points

[0112] (8) Softness of foam when brushing teeth The test product (toothpaste) was filled in an 8 mm diameter laminate tube, and about 1 g of the dentifrice composition was taken from the tube onto a toothbrush (Clinica Advantage Toothbrush, 4-row compact normal, manufactured by Lion Corporation), and brushed for 3 minutes, and the softness of the toothpaste foam in the oral cavity during use was evaluated. The evaluation was carried out by 10 people, and evaluation was carried out according to the following evaluation criteria, and the average of the 10 people was judged, with an average score of 3.0 points or more (criteria A and B) being considered pass.

[0113] Evaluation criteria 4 points: The foam feels very soft 3 points: Feel the softness of the foam 2 points: The foam feels a little soft 1 point: The foam is barely soft

[0114] ·Judgment criteria A: Average score is between 3.5 and 4.0 points B: Average score is between 3.0 and 3.5 C: Average score is between 2.0 and 3.0 points D: Average score is less than 2.0 points

[0115] (9) Long-lasting foam when brushing teeth Approximately 1 g of the test product (toothpaste) packed in an 8 mm diameter laminated tube was placed on a toothbrush (Clinica Advantage Toothbrush, 4-row compact normal, manufactured by Lion Corporation), and brushed for 3 minutes, and the toothpaste's foam retention in the mouth during use was evaluated. The evaluation was carried out by 10 people, who evaluated it according to the following evaluation criteria, and judged it based on the average of the 10 people, with an average score of 3.0 points or more (criteria A and B) being considered a pass.

[0116] Evaluation criteria 4 points: The foam lasts long enough 3 points: Moderate foam retention 2 points: Low foam retention 1 point: Almost no foam retention

[0117] ·Judgment criteria A: Average score is between 3.5 and 4.0 points B: Average score is between 3.0 and 3.5 C: Average score is between 2.0 and 3.0 points D: Average score is less than 2.0 points

[0118] (10) Stability of isopropylmethylphenol The test samples were filled into 8mm diameter laminated tubes and stored at 60°C or -5°C for one month. After allowing them to cool to room temperature, 10g of each sample was taken and extracted with methanol. The amount of isopropyl methylphenol was then measured using HPLC (high performance liquid chromatography) under the following test conditions. The quantitative value of isopropyl methylphenol in the test sample after one month of storage at -5°C was designated the initial value, and the quantitative value of isopropyl methylphenol in the test sample after one month of storage at 60°C was designated the evaluation sample value. The residual rate of isopropyl methylphenol was calculated using the following formula to evaluate the stability of isopropyl methylphenol over time. Residual rate of isopropyl methylphenol (%) = {Evaluation sample value / Initial value} x 100 Regarding the stability of isopropylmethylphenol, the residual rate of isopropylmethylphenol calculated by the above formula is preferably 90% or more, and particularly preferably 95% or more.

[0119] Test conditions Detector: ultraviolet absorption photometer (measurement wavelength: 285 nm) Column: YMC-Pack ODS-A A-303 (4.6 mm diameter x 250 mm) Column temperature: 45℃ Mobile phase: Acetonitrile / water / acetic acid mixture (60:40:1)

[0120] ·Equipment used Pump: JASCO Corporation, PU-980 Sample introduction unit: JASCO Corporation, AS-950 Detector: JASCO Corporation, UV-970 Column thermostat: JASCO Corporation, CO-960 Flow rate: 1mL / min

[0121] (11) Vitamin E stability The test samples were filled into 8mm diameter laminated tubes and stored at 60°C or -5°C for one month. After allowing them to cool to room temperature, 10g portions were taken and extracted with methanol. Vitamin E was then quantified using the absolute calibration curve method by HPLC (high performance liquid chromatography) under the following test conditions. The quantified value of vitamin E in the test sample after one month of storage at -5°C was designated the initial value, and the quantified value of vitamin E in the test sample after one month of storage at 60°C was designated the evaluation sample value. The residual vitamin E rate was calculated using the following formula to evaluate the stability of vitamin E over time. Vitamin E Residual Rate (%) = {Evaluation sample value / Initial value} x 100 The stability of vitamin E is such that the residual rate of vitamin E calculated by the above formula is preferably 90% or more, and particularly preferably 95% or more.

[0122] Test conditions Detector: ultraviolet absorption photometer (measurement wavelength: 273 nm) Column: COSMOSIL 5C18-MS-II Column temperature: 40℃ Eluent: methanol

[0123] (12) Refreshing feeling after brushing your teeth Approximately 1 g of the test product packed in an 8 mm diameter laminated tube was placed on a toothbrush (Clinica Advantage toothbrush, 4-row compact normal, manufactured by Lion Corporation), brushed for 3 minutes, and then rinsed twice with approximately 20 mL of water, after which the feeling of freshness in the oral cavity was evaluated. The evaluation was carried out by 10 people, who evaluated using the following evaluation criteria, and judged the average of the 10 people. An average of 3.0 points or more (criteria A and B) was considered a pass.

[0124] Evaluation criteria 4 points: I felt a strong sense of freshness 3 points: I felt refreshed 2 points: I felt a slight sense of freshness 1 point: I didn't feel refreshed

[0125] ·Judgment criteria A: Average score is between 3.5 and 4.0 points B: Average score is between 3.0 and 3.5 C: Average score is between 2.0 and 3.0 points D: Average score is less than 2.0 points

[0126] (13) Astringent feeling on gums after brushing teeth Approximately 1 g of the test product, packed in an 8 mm diameter laminated tube, was placed on a toothbrush (Clinica Advantage toothbrush, 4-row compact regular, manufactured by Lion Corporation), and brushed for 3 minutes. After rinsing twice with approximately 20 mL of water, the astringent feeling on the gums was evaluated. The evaluation was carried out by 10 people, who evaluated using the following evaluation criteria. The average score of the 10 people was judged, and an average score of 3.0 points or more (criteria A and B) was considered to be acceptable.

[0127] Evaluation criteria 4 points: I felt a strong sense of astringency 3 points: I felt a sense of astringency 2 points: I felt a slight sense of astringency. 1 point: No astringency felt

[0128] ·Judgment criteria A: Average score is between 3.5 and 4.0 points B: Average score is between 3.0 and 3.5 C: Average score is between 2.0 and 3.0 points D: Average score is less than 2.0 points

[0129] (14) Astringency when brushing teeth Approximately 1 g of the test product (toothpaste) packed in an 8 mm diameter laminated tube was placed on a toothbrush (Clinica Advantage Toothbrush, 4-row compact normal, manufactured by Lion Corporation), and brushed for 3 minutes, and the astringency of the toothpaste in the oral cavity during use was evaluated. The evaluation was carried out by 10 people, who evaluated using the following evaluation criteria and judged the average of the 10 people, with an average score of 2.0 points or more but less than 3.0 points (criterion A) being considered pass.

[0130] Evaluation criteria 4 points: Strong astringency 3 points: Astringent 2 points: Slightly bitter 1 point: No bitterness felt

[0131] ·Judgment criteria A: 2.0 points or more and less than 3.0 points B: 1.5 points or more but less than 2.0 points, or 3.0 points or more but less than 3.5 points C: Less than 1.5 points, or 3.5 points to 4.0 points

[0132] [Table 9]

[0133] [Table 10]

[0134] [Table 11]

[0135] [Table 12]

[0136] [Table 13]

[0137] [Table 14]

[0138] [Table 15]

[0139] In addition to the three effects of stringiness, storage stability, and usability, the test products of Examples 24 to 74 were highly rated in terms of brushing feel during toothbrushing, ease of rinsing, foam softness during toothbrushing, foam retention during toothbrushing, stability of isopropyl methylphenol and vitamin E, refreshing feeling after toothbrushing, gum astringency after toothbrushing, and moderate astringency during toothbrushing. Furthermore, test products prepared in the same manner except for using flavors B to P (Tables 4 to 5) instead of flavor A also received evaluations similar to those of the Examples shown in Tables 9 to 14. These results demonstrate that the dentifrice composition of the present invention can exhibit the effects attributable to components (D1) to (D5) in addition to the three effects of stringiness, storage stability, and usability.

Claims

1. (A) at least one of sorbitol and glycerin, (B) at least one selected from the group consisting of xanthan gum, sodium carboxymethylcellulose, and sodium alginate; and (C) Fluorine-containing compound Contains The content of component (A) is 15 to 47 mass %, The content of the (B) component is 0.7 to 4 mass %, and The content of component (C) is 3,500 to 20,000 ppm when converted into a fluorine ion concentration. A dentifrice composition comprising:

2. 2. The dentifrice composition according to claim 1, wherein the content of component (C) is 4,500 to 15,000 ppm when converted into a fluoride ion concentration.

3. 3. The dentifrice composition according to claim 1, wherein the ratio (C / B) of the content (ppm) of component (C) converted into fluoride ion concentration to the content (mass%) of component (B) is 1,500 to 14,000.

4. (D1) At least one selected from the group consisting of silicic anhydride, hydroxyapatite, cellulose powder, and granules 3. The dentifrice composition of claim 1 or 2, further comprising:

5. (D2) Amino acid-based anionic surfactant 3. The dentifrice composition of claim 1 or 2, further comprising:

6. (D3) Sugar-based nonionic surfactant 3. The dentifrice composition of claim 1 or 2, further comprising:

7. (D4) Chelating agent 3. The dentifrice composition of claim 1 or 2, further comprising:

8. (D5) Water-soluble calcium compound 3. The dentifrice composition of claim 1 or 2, further comprising: