Toothpaste composition

Abstract

To provide a toothpaste composition that has a high whitening effect and maintains that whitening effect even after long-term storage. [Solution] A toothpaste composition containing (A) component: glucose oxidase and (B) component: polyethylene glycol, wherein the glucose oxidase activity per 1 g of the toothpaste composition is 20 to 200 U / g, the average molecular weight of component (B) is 150 to 600, and the content of component (B) is 0.2 to 3% by mass relative to the total mass of the toothpaste composition.

Description

Technical Field

[0001] The present invention relates to a dentifrice composition.

Background Art

[0002] One of the important functions of a dentifrice composition is a whitening effect that whitens teeth. In Patent Document 1, it is disclosed that a whitening effect can be obtained by blending an alkyl sulfate and a water-soluble polyphosphate into a dentifrice composition. In Patent Document 2, a method for whitening teeth is disclosed by alternately applying a composition (A) containing phytic acid and a cellulose-based binder and not containing a polyvalent metal cation, and a composition (B) containing a peroxide to teeth.

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Patent Document 2

Summary of the Invention

Problems to be Solved by the Invention

[0004] For dentifrice compositions, further improvement of the whitening effect is desired. Compositions containing peroxides as in Patent Document 2 are unstable to light and heat, so they are likely to decompose during storage, and it is difficult to ensure long-term product stability. Therefore, the development of a dentifrice composition with a long-term stable whitening effect is desired. An object of the present invention is to provide a dentifrice composition having a high whitening effect and maintaining a high whitening effect even after long-term storage. [[ID=4,3]]

Means for Solving the Problems

[0005] The present invention has the following aspects. [1] Component (A): glucose oxidase, and (B) Component: A toothpaste composition containing polyethylene glycol, The glucose oxidase activity per gram of the toothpaste composition is 20 to 200 U / g. The average molecular weight of component (B) is 150 to 650. The content of component (B) is 0.2 to 3% by mass relative to the total mass of the toothpaste composition. Toothpaste composition. [2] The content of component (B) is 1 to 2.5% by mass relative to the total mass of the toothpaste composition. The toothpaste composition described in [1]. [3] The ratio of the glucose oxidase activity (U / g) to the content (mass%) of component (B), as shown by component (A) / component (B), is 3 to 250. The toothpaste composition described in [1] or [2]. [4] The ratio of the glucose oxidase activity (U / g) to the content (mass%) of component (B), represented by component (A) / component (B), is 5 to 120. The toothpaste composition described in [1] or [2]. [5] The ratio of the glucose oxidase activity (U / g) to the content (mass%) of component (B), as shown by component (A) / component (B), is 7 to 90. The toothpaste composition described in [1] or [2]. [6](C) component: further comprising at least one selected from the group consisting of polyoxyethylene hydrogenated castor oil and fatty acid amidopropyl betaine, The aforementioned polyoxyethylene hydrogenated castor oil has an average number of repeating oxyethylene groups of 10 to 40. A toothpaste composition described in any one of [1] to [5]. [7] The content of component (C) is 0.1 to 1% by mass relative to the total mass of the toothpaste composition. The toothpaste composition described in [6]. [8] The content of component (C) is 0.3 to 0.8% by mass relative to the total mass of the toothpaste composition. The toothpaste composition described in [6]. [9] The content of component (C) is 0.3 to 0.7% by mass relative to the total mass of the toothpaste composition. The toothpaste composition described in [6].

[10] The ratio of the mass of component (B) to the mass of component (C), as shown by component (B) / component (C), is 0.4 to 8. A toothpaste composition as described in any one of [6] to [9].

[11] The ratio of the mass of component (B) to the mass of component (C), represented by component (B) / component (C), is between 1 and 8. A toothpaste composition as described in any one of [6] to [9].

[12] The ratio of the mass of component (B) to the mass of component (C), represented by component (B) / component (C), is 2 to 5. A toothpaste composition as described in any one of [6] to [9].

[13] The toothpaste composition according to any one of [1] to

[12] , wherein the average molecular weight of component (B) is 280 to 630.

[14] The toothpaste composition according to any one of [1] to

[13] , wherein the average molecular weight of component (B) is 380 to 630. [Effects of the Invention]

[0006] According to the present invention, it is possible to provide a toothpaste composition that has a high whitening effect and maintains that whitening effect even after long-term storage. [Modes for carrying out the invention]

[0007] The embodiments of the present invention will be described in detail below, but the present invention is not limited to the embodiments described below and can be implemented with various modifications within the scope of its gist.

[0008] In this specification and in the claims, a numerical range represented by "~" means a numerical range that includes the numbers before and after "~" as the lower and upper limits, respectively. For example, A~B is synonymous with A or greater and B or less.

[0009] In this specification, excellent long-term stability means that the dentifrice composition has a good whitening effect even when stored for a long time after production.

[0010] <Dentifrice composition> The dentifrice composition of this aspect contains the following component (A) and component (B).

[0011] [Component (A)] Component (A) is glucose oxidase. By including component (A) in the dentifrice composition, the whitening effect of the dentifrice composition can be further enhanced.

[0012] The content of component (A) is determined in consideration of the activity amount of glucose oxidase, which is component (A) (hereinafter, may be referred to as the glucose oxidase activity amount). That is, component (A) is formulated so that the glucose oxidase activity amount of the dentifrice composition falls within a desired range. The glucose oxidase activity amount per 1 g of the dentifrice composition is 20 to 200 U / g, preferably 30 to 150 U / g, and more preferably 50 to 100 U / g. When the glucose oxidase activity amount per 1 g of the dentifrice composition is at least the above lower limit value, the whitening effect of the dentifrice composition can be further enhanced. When the glucose oxidase activity amount per 1 g of the dentifrice composition is at most the above upper limit value, coloring (yellowing) when the dentifrice composition is stored can be suppressed. The glucose oxidase activity amount represented by the unit of "U (unit)" uses o-phenylenediamine as an indicator substance, and indicates the activity amount that generates 1 μmol of hydrogen peroxide when the composition containing component (A) is reacted at 30°C for 3 minutes.

[0013] Component (A) may be formulated as glucose oxidase alone, or a preparation containing glucose oxidase may be formulated. Examples of the preparation containing glucose oxidase include a solution and powder containing glucose oxidase and a solvent. Examples of preparations containing glucose oxidase include Glucose Oxidase (manufactured by Zhongnuo), Gluzyme® Fortis (manufactured by Novonesis), Glucose Oxidase ”Amano®” AM (manufactured by Amano Enzyme), Hyderase 15 (manufactured by Amano Enzyme), and the like.

[0014] The amount of glucose oxidase activity as a raw material of component (A) incorporated into the dentifrice composition is not particularly limited. When component (A) is a preparation containing glucose oxidase, the amount of glucose oxidase activity (raw material activity) per 1 g of the preparation is preferably 8,000 to 15,000 U / g, more preferably 9,000 to 12,000 U / g, and even more preferably 10,000 to 12,000 U / g. When the raw material activity is at least the above lower limit value, the whitening effect of the dentifrice composition can be further enhanced. When the raw material activity is at most the above upper limit value, coloring (yellowing) upon storage of the dentifrice composition can be suppressed. The raw material activity is indicated by the amount of activity that generates 1 μmol of hydrogen peroxide when the preparation containing component (A) is reacted for 3 minutes under the condition of 30°C, using o-phenylenediamine as an indicator substance.

[0015] [Component (B)] Component (B) is polyethylene glycol (PEG). By including component (B) in the dentifrice composition, the whitening effect of the dentifrice composition can be further enhanced.

[0016] The average molecular weight of component (B) is preferably 150 to 650, and more preferably 280 to 630. If the average molecular weight of component (B) is above the lower limit, it has excellent viscosity and retention properties, and tends to stay in the oral cavity longer. If the average molecular weight of component (B) is below the upper limit, the penetration rate of component (B) into stains, which are discolored deposits on the tooth surface, increases, and the stains swell more. As a result, the glucose contained in the stains and glucose oxidase, which is component (A) contained in the toothpaste composition, come into contact more easily, and the whitening effect can be further enhanced. The average molecular weight of component (B) is a value measured by gel permeation chromatography (GPC).

[0017] (B) Examples of component (B) include polyethylene glycol 200 (average molecular weight 190-210), polyethylene glycol 300 (average molecular weight 280-320), polyethylene glycol 400 (average molecular weight 380-420), and polyethylene glycol 600 (average molecular weight 570-630). The polyethylene glycol may be prepared or a commercially available product may be used.

[0018] The content of component (B) in the toothpaste composition is 0.2 to 3% by mass, preferably 0.2 to 2.5% by mass, and more preferably 1 to 2.5% by mass, based on the total mass of the toothpaste composition. If the content of component (B) in the toothpaste composition is above the lower limit, the whitening effect of the toothpaste composition can be further enhanced. If the content of component (B) in the toothpaste composition is below the upper limit, the bitterness when using the toothpaste composition can be suppressed, and the user experience can be improved.

[0019] [(C) component] The toothpaste composition may further contain component (C). Component (C) is at least one selected from the group consisting of polyoxyethylene hydrogenated castor oil and fatty acid amidopropyl betaine.

[0020] In polyoxyethylene hydrogenated castor oil, the average number of repeating oxyethylene groups is preferably 10 to 60, more preferably 15 to 40, and even more preferably 18 to 25. When the average number of repeating oxyethylene groups is above the lower limit, the hydrophilicity of the polyoxyethylene hydrogenated castor oil is increased, structural modification due to hydrophobic interaction with component (A) is suppressed, and the stability of the three-dimensional structure of component (A) is increased. When the average number of repeating oxyethylene groups is below the upper limit, a balance with hydrophobic groups is maintained, and appropriate adsorption to the interface is maintained, thereby keeping the surrounding environment of component (A) stable. Commercially available polyoxyethylene hydrogenated castor oil may be used, for example, NIKKOL® HCO-20, 40, 60 (manufactured by Nikko Chemicals Co., Ltd.) can be used. The average number of repeating oxyethylene groups can be measured by gel filtration chromatography.

[0021] The number of carbon atoms in fatty acid amidopropyl betaine is preferably 10 to 16, more preferably 12 to 14, and even more preferably 12 to 13. When the number of carbon atoms in fatty acid amidopropyl betaine is above the lower limit, the hydrophobicity of fatty acid amidopropyl betaine increases, suppressing excessive interaction with the surface of component (A) and increasing the stability of the three-dimensional structure of component (A). When the number of carbon atoms in fatty acid amidopropyl betaine is below the upper limit, the hydrophilicity of fatty acid amidopropyl betaine increases, improving its dispersibility with saliva and stains in the formulation. Furthermore, when the number of carbon atoms in fatty acid amidopropyl betaine is below the upper limit, the dispersibility of component (A) with saliva and stains in the formulation increases, and the stability of the activity of component (A) increases.

[0022] Fatty acid amidopropyl betaine is preferably one having an alkyl group with 10 to 16 carbon atoms. Examples of such fatty acid amidopropyl betaine include coconut oil fatty acid amidopropyl betaine and lauric acid amidopropyl betaine. Of these, coconut oil fatty acid amidopropyl betaine is preferred. Commercially available fatty acid amidopropyl betaine can be used, for example, Energikol® C-30B manufactured by Lion Specialty Chemicals Co., Ltd. and NIKKOL® AM-3130N manufactured by Nikko Chemicals Co., Ltd.

[0023] The content of component (C) in the toothpaste composition is preferably 0.1 to 1% by mass, more preferably 0.3 to 0.8% by mass, and even more preferably 0.3 to 0.7% by mass, relative to the total mass of the toothpaste composition. When the content of component (C) in the toothpaste composition is above the lower limit, the long-term stability of the whitening effect is further enhanced, and the immediate effect of the whitening effect is further enhanced. Here, an immediate effect of the whitening effect means that the whitening effect of the toothpaste composition can be obtained even with shorter usage times. When the content of component (C) in the toothpaste composition is below the upper limit, the bitterness when using the toothpaste composition can be suppressed, and the user experience can be improved.

[0024] When a toothpaste composition contains anionic surfactants, the immediate whitening effect may be reduced. However, by including component (C) in the toothpaste composition, the reduction in immediate effect caused by anionic surfactants is suppressed, and a whitening effect can be obtained with shorter usage time.

[0025] [Mixing ratio] The ratio of glucose oxidase activity (U / g) to the content (mass%) of component (B) in the toothpaste composition (A / B ratio) is preferably 3 to 250, more preferably 5 to 120, and even more preferably 7 to 90. If the A / B ratio is above the lower limit, the whitening effect can be further enhanced. If the A / B ratio is below the upper limit, an efficient whitening effect can be achieved while maintaining the storage stability against discoloration of the toothpaste composition. Here, the glucose oxidase activity (U / g) in the A / B ratio represents the amount of glucose oxidase activity (U) per gram of toothpaste composition. The content of component (B) in the A / B ratio represents the mass of component (B) relative to the total mass of the toothpaste composition.

[0026] The ratio of the mass of component (B) to the mass of component (C) in the toothpaste composition (B / C ratio) is preferably 0.4 to 8, more preferably 1 to 8, and even more preferably 2 to 5. If the B / C ratio is above the lower limit, the bitterness when using the toothpaste composition can be suppressed and the user experience can be improved. If the B / C ratio is below the upper limit, the long-term stability of the whitening effect can be further enhanced.

[0027] [Optional ingredients] The toothpaste composition may further contain components other than those described above (A), (B), and (C) (hereinafter sometimes referred to as "optional components"). The optional components can be appropriately selected from known components, taking into consideration the form and method of use of the toothpaste composition. Examples of optional components include abrasives, binders, surfactants other than component (C) (hereinafter sometimes referred to as "optional surfactants"), humectants other than component (B) (hereinafter sometimes referred to as "optional humectants"), sweeteners, oily components, fragrances, cooling agents, pH adjusters, preservatives, and medicinal components. The total amount of component (A), component (B), component (C), and optional components mentioned above shall not exceed 100% by mass.

[0028] (Abrasive) Examples of abrasives include calcium phosphate compounds such as dicalcium phosphate dihydrate and anhydrous, monocalcium phosphate, tricalcium phosphate, and calcium pyrophosphate; silica-based abrasives such as precipitated silica, aluminosilicate, zirconosilicate, and titanium-bonded silica; calcium carbonate, calcium hydroxide, aluminum hydroxide, trimagnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, and hydroxyapatite. Of these abrasives, compounds mainly composed of silicates, such as precipitated silica, aluminosilicate, zirconosilicate, and titanium-bonded silica, and calcium carbonate are preferred. These abrasives may be included individually or in combination of two or more.

[0029] Examples of precipitated 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. The precipitated silica may be commercially available, such as Zeodent® 124, Zeodent® 113, Zeodent® 103, Sident® 3, Sident® 9, and Sident® 20 from EVONIK, TIXOSIL® 73 and TIXOSIL® 63 from Rhodia, and zirconosilicate and aluminosilicate from Taki Chemical Co., Ltd.

[0030] The total amount of abrasives contained in the toothpaste composition is not particularly limited, but is preferably 5 to 70% by mass relative to the total mass of the toothpaste composition.

[0031] As an abrasive, a granular preparation containing an abrasive can be used. In this specification, a granular preparation is a granulated particle formed from a water-insoluble powder. A binder may or may not be used in the production of the granular preparation, but it is preferable that no binder is used. Examples of water-insoluble powders include inorganic powders such as dicalcium phosphate, tricalcium phosphate, water-insoluble calcium metaphosphate, silica, aluminum hydroxide, magnesium phosphate, iron oxide, calcium carbonate, calcium pyrophosphate, zeolite, aluminosilicate, magnesium carbonate, zirconosilicate, and calcium sulfate, as well as mixtures thereof. As abrasive-containing granular preparations, silica granules and zeolite granules are preferred.

[0032] The method for preparing silica granules is not particularly limited. For example, one method involves forming a mass of silica gel with a grown primary particle size by the gel method, washing and drying the silica gel mass, and then grinding it. Another method involves spraying silica hydrosol into the air and allowing it to gel. Yet another known method involves agglomerating the silica while suppressing the growth of primary particles using the sedimentation method, and then allowing the primary particle size to grow. Of these preparation methods, the gel method is preferred because it is simple to manufacture and allows for easy control of the average particle size through classification. These preparation methods allow for the preparation of silica granules with a more appropriate average collapse strength.

[0033] The primary particle size in the above-described preparation method is not particularly limited, but is preferably 3 to 15 nm, and more preferably 4 to 10 nm.

[0034] The volume-average particle size (median diameter d50) of the granules is preferably 50 to 500 μm. The volume-average particle size is measured using a particle size distribution analyzer (Microtrac particle size distribution analyzer, manufactured by Nikkiso Co., Ltd., dispersion medium: water).

[0035] The average disintegration strength of the granules is preferably 10 to 200 g / granule. In this specification, the average disintegration strength is calculated as the average of the automatic breaking strength measurements of 30 granules using a rheometer (Sun Rheometer CR-200D, manufactured by Sun Science Co., Ltd.). The breaking strength measurement is the value obtained by measuring the load at which a granule disintegrates when it is compressed at a speed of 10 mm / min.

[0036] Commercially available silica granules can be used as silica granules having the above-mentioned preferred average particle size and average collapse strength. Examples of such silica granules include SORBOSIL® BFG10 and SORBOSIL® BFG50 from PQ Corporation, NIPGEL® AY and NIPGEL® BY-001 from Tosoh Silica Co., Ltd., and SYLOPURE® 30, SYLOPURE® 39, SYLOPURE® 40, SYLOPURE® 50, and SYLOPURE® 60 from Fuji Silicia Chemical Co., Ltd. Examples of zeolite granules include COLITE TG from Cosmo Co., Ltd.

[0037] Granular formulations can also be colored, such as SORBOSIL® BFG51, SORBOSIL® BFG52, and SORBOSIL® BFG54, manufactured by PQ Corporation.

[0038] When the abrasive is in granular form, the amount to be included is not particularly limited, but the total mass of the granules relative to the total mass of the toothpaste composition is preferably 0.1 to 20% by mass.

[0039] (Binding agent) As binders, inorganic binders such as thickening silica and aluminum silicate, and organic binders such as sodium carboxymethylcellulose, xanthan gum, polyvinylpyrrolidone, carrageenan, methylcellulose, sodium hydroxyethylcellulose, sodium alginate, tragacanth gum, karaya gum, arabia gum, locust bean gum, polyvinyl alcohol, sodium polyacrylate, cross-linked sodium polyacrylate, carboxyvinyl polymer, Carbopol, bee gum, propylene glycol alginate, and methyl vinyl ether / maleic anhydride copolymer may be included.

[0040] As the thickening silica, silica obtained by known manufacturing methods with an absorption capacity in the range of 2 to 5 ml / g can be used. Here, the absorption capacity is the value measured by the following procedure. 1.0 g of silica is weighed onto a clean glass plate, and using a microburette, 42.5% by mass glycerin is added dropwise in small amounts while mixing the silica and glycerin with a stainless steel spatula until the liquid is uniform. The endpoint is reached when the sample forms a single mass and can be cleanly peeled off the glass plate with the spatula, and the amount of glycerin added dropwise up to the endpoint (ml) is defined as the absorption capacity.

[0041] Examples of thickening silica include SORBOSIL® TC15 from PQ Corporation, TIXOSIL® 43 from Rhodia, Zeodent® 153 from EVONIK, Carplex® #67Q from DSL Japan, and Silopure® 25 from Fuji Silicia Chemical Co., Ltd.

[0042] The average degree of substitution (DS) of carboxymethyl groups in sodium carboxymethylcellulose is preferably 0.5 to 1.5. The viscosity of sodium carboxymethylcellulose is preferably 15 to 3,000 mPa·s. Here, the above viscosity is the value measured at 20°C in a 2% aqueous solution. The above viscosity is the value measured using a B8H type viscometer (e.g., manufactured by Tokyo Keiki Co., Ltd.) with rotors 1 to 4 according to the viscosity range. For example, when the viscosity is less than 100 mPa·s, the viscosity is measured after 3 minutes at 50 rpm using rotor 1. When the viscosity is 100 mPa·s or more, the viscosity can be measured after 3 minutes at 20 rpm using rotors 1 to 4.

[0043] As the carboxymethylcellulose sodium having the above-mentioned preferred degree of DS conversion and viscosity, commercially available products can be used. Examples of such carboxymethylcellulose sodium include CMC Daicel® sold by Daicel Mirise, Selogen® manufactured by Daiichi Kogyo Seiyaku Co., Ltd., and Sunrose® manufactured by Nippon Paper Industries Co., Ltd.

[0044] The total amount of binders contained in the toothpaste composition is not particularly limited, but is preferably 0.1 to 10% by mass relative to the total mass of the toothpaste composition.

[0045] (Optional surfactant) In this specification, "optional surfactant" refers to a surfactant other than component (C). Various known surfactants can be used as optional surfactants, for example, anionic surfactants, nonionic surfactants, and amphoteric surfactants. These optional surfactants may be included individually or in combination of two or more.

[0046] Examples of anionic surfactants as optional surfactants include alkyl sulfates, dodecylbenzenesulfonates, hydrogenated coconut fatty acid monoglyceride monosulfates, lauryl sulfoacetates, α-olefin sulfonates, N-acyl taurates such as N-methyl-N-acyl taurate, acyl sarcosine salts, and N-acyl-L-glutamates. Examples of the salts include sodium salts, potassium salts, and ammonium salts, with sodium salts being preferred.

[0047] Examples of nonionic surfactants used as optional surfactants include polyoxyethylene fatty acid esters other than polyoxyethylene hydrogenated castor oil, polyglycerin fatty acid esters, sucrose fatty acid esters, maltitol fatty acid esters, lactitol fatty acid esters and other sugar alcohol fatty acid esters, alkylolamides, polyoxyethylene sorbitan fatty acid esters such as polyoxyethylene sorbitan monostearate, fatty acid diethanolamides such as lauryl acid diethanolamide, sorbitan fatty acid esters, polyoxyethylene higher alcohol ethers, alkyl glucosides, polyoxyethylene polyoxypropylene copolymers, and polyoxyethylene polyoxypropylene fatty acid esters.

[0048] As an optional surfactant, any known amphoteric surfactant other than fatty acid amidopropyl betaine, which is component (C), can be included. Examples of such amphoteric surfactants include alkyl betaines such as lauryldimethylaminoacetic acid betaine, and imidazoline-type amphoteric surfactants such as coconut oil fatty acid imidazolium betaine.

[0049] The total amount of optional surfactants contained in the toothpaste composition is not particularly limited, but is preferably 0.001 to 10% by mass relative to the total mass of the toothpaste composition.

[0050] (Optional Wetting Agent) In this specification, "optional wetting agent" refers to a wetting agent other than polyethylene glycol, which is component (B). Various known wetting agents can be used as optional wetting agents, for example, sugar alcohols such as sorbitol, xylitol, and erythritol, and polyhydric alcohols such as glycerin and propylene glycol. These optional wetting agents may be included individually or in combination of two or more.

[0051] The total amount of optional wetting agents contained in the toothpaste composition is not particularly limited, but is preferably 2 to 70% by mass relative to the total mass of the toothpaste composition.

[0052] (Sweetener) Examples of sweeteners include sodium saccharin, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, perlarthin, glycyrrhizin, thaumatin, and aspartylphenylalanine methyl ester. These sweeteners may be included individually or in combination of two or more.

[0053] (Oily components) Examples of oily components include light liquid paraffin, liquid paraffin, stearyl alcohol, stearic acid, and cetanol. These oily components may be included individually or in combination of two or more.

[0054] (fragrance) Examples of fragrances include menthol, anethole, carvone, eugenol, limonene, n-decyl alcohol, citronellol, α-terpineol, citronellyl acetate, cineole, linalool, ethyl linalool, vanillin, thymol, spearmint oil, peppermint oil, lemon oil, orange oil, sage oil, rosemary oil, cinnamon oil, pimento oil, cinnamon leaf oil, perilla oil, wintergreen oil, clove oil, and eucalyptus oil. These fragrances may be included individually or in combination of two or more.

[0055] The total amount of fragrance contained in the toothpaste composition is not particularly limited, but is preferably 0.01 to 1% by mass relative to the total mass of the toothpaste composition. If the fragrance is menthol and the amount of fragrance is above the lower limit mentioned above, the refreshing feeling when using the toothpaste composition can be further enhanced.

[0056] (Cooling agent) 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 (EVERCOOL® 180), N-(2-(pyridine-2-yl)-3-p-menthanecarboxamide) (EVERCOOL® 190), 2-isopropyl-N,2,3-trimethylbutylamide (WS-23), menthongglycerol acetal (MGA), menthoxypropane-1,2-diol, menthyl lactate, menthyl succinate, and isopulegol. These cooling agents may be included individually or in combination of two or more.

[0057] The total amount of cooling agents included in the toothpaste composition is not particularly limited, but is preferably 0.00001 to 0.01% by mass relative to the total mass of the toothpaste composition. If the amount of cooling agents is above the lower limit mentioned above, the refreshing feeling when using the toothpaste composition can be further enhanced.

[0058] (pH adjuster) Examples of pH adjusting agents include organic acids such as citric acid, lactic acid, and fumaric acid, and their salts; and inorganic compounds such as hydrochloric acid, sodium hydroxide, potassium hydroxide, disodium hydrogen phosphate, and sodium dihydrogen phosphate. These pH adjusting agents may be included individually or in combination of two or more.

[0059] (Preservative) Examples of preservatives include parahydroxybenzoic acid esters, sodium benzoate, and triclosan. These preservatives may be included individually or in combination of two or more.

[0060] (Medicinal ingredients) Examples of active pharmaceutical ingredients include fluorides such as sodium fluoride, sodium monofluorophosphate, and tin fluoride; enzymes other than glucose oxidase (component A), such as dextranase, amylase, protease, and mutanase; anti-inflammatory agents such as tranexamic acid, epsilon-aminocaproic acid, allantoin, aluminum chlorohydroxyallantoin, panthenol, azulene, glycyrrhizinate, glycyrrhetinate, and Phellodendron amurense; cell activators such as sodium chloride and vitamins; antibacterial agents such as isopropylmethylphenol, copper chlorophyll, copper gluconate, cetylpyridinium chloride, benzalkonium chloride, hinokitiol, and lysozyme chloride; tartar preventatives such as pyrophosphates, polyphosphates, and zeolites; blood circulation promoters such as vitamin E; and amino acids such as alanine, glycine, and proline. These active pharmaceutical ingredients may be included individually or in combination of two or more. The amount of active pharmaceutical ingredient is not particularly limited and can be set as appropriate within a range that does not hinder the effects of the present invention.

[0061] (Other optional components) Other optional components besides those mentioned above (hereinafter sometimes referred to as "other optional components") include, for example, inorganic compounds such as titanium mica, titanium dioxide, zinc oxide, magnesium oxide, zirconium oxide, and bentonite; cellulosic organic powders such as crystalline cellulose; natural polymer compounds such as agar, gelatin, starch, and glucomannan; synthetic polymer compounds and copolymers thereof such as polyvinyl acetate, polyacrylic, 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. The content of other optional components is not particularly limited and can be set appropriately within a range that does not hinder the effects of the present invention.

[0062] The viscosity of the toothpaste composition at 25°C is not particularly limited, and an appropriate viscosity can be selected depending on the form and dosage form. The viscosity of the toothpaste composition at 25°C is preferably 40 to 150 Pa·s, and more preferably 80 to 120 Pa·s. If the viscosity of the toothpaste composition is above the lower limit, the shape retention and feel can be further improved. If the viscosity of the toothpaste composition is below the upper limit, the shape retention and feel can be further improved. The viscosity of the toothpaste composition is measured using a BH viscometer.

[0063] The pH of the toothpaste composition at 25°C is preferably 5.0 to 9.0, and more preferably 6.0 to 8.0. If the pH of the toothpaste composition is above the lower limit, the activity of component (A) may decrease. If the pH of the toothpaste composition is below the upper limit, the activity of component (A) may decrease.

[0064] [Form, dosage form] The form of the toothpaste composition is not particularly limited and can be prepared in various forms, such as paste or gel. The dosage form of the toothpaste composition is not particularly limited and examples include toothpaste paste, liquid toothpaste, moistened toothpaste, etc. The dosage form of the toothpaste composition is preferably toothpaste paste.

[0065] [Manufacturing method] The toothpaste composition of this disclosure can be manufactured by known methods. For example, it can be manufactured by mixing the above-mentioned components (A), (B), (C) and optional components by conventional methods.

[0066] As described above, the toothpaste composition of this embodiment contains component (A) and component (B), thereby enhancing the whitening effect and long-term stability. [Examples]

[0067] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to the following description. In these examples, "%" refers to "mass%" unless otherwise specified.

[0068] <Raw materials used> [(A) component] Glucose oxidase (manufactured by Zhongnuo, product name: Glucose Oxidase, raw material activity: 10986 U / g)

[0069] [(B) Component] Polyethylene glycol 400 (manufactured by LiaoNing Oxiranpharm, product name: PEG-400) Polyethylene glycol 600 (manufactured by LiaoNing Oxiranpharm, product name: PEG-600)

[0070] [(C) component] Polyoxyethylene hydrogenated castor oil (manufactured by AOKI OIL INDUSTRIAL, product name: BLAUNON® RCW-20, average number of oxyethylene groups: 10-40) Fatty acid amidopropyl betaine (manufactured by Evonik, trade name: Tego® Betaine CK OK MB)

[0071] [Optional ingredients] Sodium pyrophosphate (manufactured by Hubei Xingfa Chemicals Group, product name: Food additive tetrasodium pyrophosphate) Sodium saccharin (manufactured by Henan Kaifeng Pingmei Shenma Xinhua Fine Chemical Co., Ltd., trade name: Sodium Saccharin) Sodium lauryl sulfate (manufactured by Dongming Jujin Chemical Industry, product name: K12) Thickening silica (manufactured by Evonik, product code: Zeodent® 165) Abrasive silica (manufactured by Evonik, product name: Zeodent® 103) Sodium Fluoride (manufactured by Shandong Huafufuloro-chemical, trade name: Sodium Fluoride) Fragrances A-S: The composition of each fragrance composition is shown in Tables 4 and 5 below, and the compositions of flavors 1-7 and solvents listed in Tables 4-5 are shown in Tables 6-13 below.

[0072] <Examples 1-17 and Comparative Examples 1-4> Toothpaste compositions were prepared by conventional methods according to the compositions shown in Tables 1-3 to obtain the toothpaste compositions of Examples 1-17 and Comparative Examples 1-4. In Tables 1-3, the values ​​listed for component (A) indicate the glucose oxidase activity (U / g) per gram of toothpaste composition. Here, the glucose oxidase activity per gram of toothpaste composition was measured according to the following procedure.

[0073] A toothpaste composition containing GB-T(A) was appropriately dispersed in a pH 6.0 phosphate buffer solution. This was then mixed with a reaction solution prepared beforehand by mixing β-D-glucose, horseradish peroxidase, and o-phenylenediamine to initiate the reaction. After the reaction began, β-D-glucose was oxidized by the action of glucose oxidase (component A), generating hydrogen peroxide. The resulting peroxide then formed a color-developing product. After a 3-minute reaction, the reaction was stopped by adding 2M sulfuric acid to create acidic conditions. After stopping the reaction, the absorbance of the colored product at 540 nm was measured. Based on this absorbance, the glucose oxidase activity was calculated as the amount of enzyme activity (U / g) that produces 1 μmol of hydrogen peroxide per 1 g of the toothpaste composition. This measurement was conducted based on a method compliant with the Chinese national standard GB / T 4484-2024, with some conditions adjusted according to the purpose of the measurement.

[0074] In Tables 1-3, the values ​​for components other than component (A) represent the content (mass%) of each component relative to the total mass of the toothpaste composition in each example. In Tables 1-3, unless otherwise specified, mass% indicates the purity, and if a component is marked with "-", that component is not included. The "residue" listed under the water column indicates the amount that makes the total volume of the toothpaste composition in each example equal to 100% by mass. In Tables 1 and 2, the "A / B ratio" indicates the ratio of the glucose oxidase activity per gram of toothpaste composition (U / g) to the content (mass) of component (B) in the toothpaste composition. In Tables 1 and 2, the "B / C ratio" indicates the ratio of the content (mass) of component (B) to the content (mass) of component (C) in the toothpaste composition.

[0075] [Whitening effect] The whitening effect of the toothpaste compositions of Examples 1-17 and Comparative Examples 1-4 was evaluated according to the following evaluation method. The whitening effect was evaluated for each toothpaste composition, both immediately after manufacture and after being stored for 3 months under a temperature of 40°C.

[0076] The attached gingiva, cementum, and root were removed from bovine mandibular incisors, leaving only the enamel. The enamel was cut into 1cm x 1cm x 1cm pieces to create enamel blocks, which were then embedded in acrylic resin (UNIFAST® III, manufactured by GC Corporation). The enamel blocks were polished with waterproof abrasive paper (#800, #2000, #4000) to create a uniform surface. To secure a test area of ​​approximately 6mm x 6mm, nail polish was applied to the polished enamel blocks for masking. Four test areas of the enamel blocks were fixed with nail polish.

[0077] The stain was applied to the test area by alternating between procedures A and B below. Procedures A and B were performed three times each per day for two days. In other words, procedures A and B were performed a total of six times each over the two days. <Procedure A> 300 μL of saliva (Medix Biochemica USA Inc., catalog number: 991-05-P) was dropped onto four test areas, sealed, and incubated at 37°C for 2 hours. <Procedure B> After performing procedure A above, 300 μL of black tea extract (extracted from Brisk Tea Bags (manufactured by Unilever Japan Co., Ltd.) according to the conditions described on the package) was added to the test area and incubated at 37°C for 1 hour.

[0078] A mixture was prepared by mixing a toothpaste composition with glucose. The toothpaste composition used included both a composition immediately after manufacturing and a composition stored for 3 months at 40°C. The amount of glucose in the mixture was 5% by mass relative to the total mass of the mixture.

[0079] The stained enamel blocks were treated by immersing them in the aforementioned mixture at 37°C for 4 hours. Images of the enamel blocks were taken before and after the treatment, and the E-values ​​were measured for each. The change in E-value (ΔE) was calculated by subtracting the E-value after treatment from the E-value before treatment, and the stain removal effect was evaluated according to the evaluation criteria below. A result of D or higher was considered a pass. The evaluation results are shown in Tables 1 to 3.

[0080] [Evaluation Criteria] • ΔE is 4.0 or higher: A • ΔE is 3.5 or greater and less than 4.0: B • ΔE is 3.0 or greater and less than 3.5: C • ΔE is between 2.0 and 3.0: D • ΔE is between 1.0 and 2.0: E • ΔE is less than 1.0: F

[0081] [Table 1]

[0082] [Table 2]

[0083] [Table 3]

[0084] Tables 1 and 2 show that all toothpaste compositions in the examples exhibited high whitening effects. Furthermore, the excellent whitening effect was maintained even after the toothpaste compositions were stored for three months, indicating that the whitening effect remains high even after long-term storage.

[0085] Table 3 shows that the toothpaste composition of Comparative Example 1, which has a low enzyme activity level of glucose oxidase (component A), has a lower whitening effect. Comparative Example 2, which does not contain polyoxyethylene glycol, component (B), was shown to have a lower whitening effect. Comparative Example 3, a toothpaste composition with a high average molecular weight of polyethylene glycol (component B), was shown to have a lower whitening effect.

[0086] Furthermore, when toothpaste compositions with the same composition as in Example 1 were prepared, except that fragrance compositions B to S listed in Tables 4 and 5 below were used instead of fragrance composition A, it was shown that all of them had a high whitening effect and high long-term stability of the whitening effect. The compositions of flavors 1-7 and solvents listed in Tables 4 and 5 below are shown in Tables 6-13 below. In the table, "a% cut from the forward distillation portion" means that the initial a% is removed during the fractional distillation of the essential oil, and "b% cut from the forward and backward distillation portions" means that the initial b% and the final b% are removed during the fractional distillation of the essential oil.

[0087] [Table 4]

[0088] [Table 5]

[0089] [Table 6]

[0090] [Table 7]

[0091] [Table 8]

[0092] [Table 9]

[0093] Table 10

[0094] Table 11

[0095] Table 12

[0096] Table 13

Claims

1. (A) Components: glucose oxidase and (B) Component: A toothpaste composition containing polyethylene glycol, The glucose oxidase activity per gram of the toothpaste composition is 20 to 200 U / g. The average molecular weight of component (B) is 150 to 650. The content of component (B) is 0.2 to 3% by mass relative to the total mass of the toothpaste composition. (C) Component: further comprising at least one selected from the group consisting of polyoxyethylene hydrogenated castor oil and fatty acid amidopropyl betaine, Toothpaste composition.

2. The content of component (B) is 1 to 2.5% by mass relative to the total mass of the toothpaste composition. The toothpaste composition according to claim 1.

3. The ratio of the glucose oxidase activity (U / g) to the content (mass%) of component (B), as shown by component (A) / component (B), is 3 to 250. The toothpaste composition according to claim 1.

4. The ratio of the glucose oxidase activity (U / g) to the content (mass%) of component (B), as shown by component (A) / component (B), is 5 to 120. The toothpaste composition according to claim 1.

5. The ratio of the glucose oxidase activity (U / g) to the content (mass%) of component (B), as shown by component (A) / component (B), is 7 to 90. The toothpaste composition according to claim 1.

6. The polyoxyethylene hydrogenated castor oil has an average number of repeating oxyethylene groups of 10 to 40. The toothpaste composition according to claim 1.

7. The content of component (C) is 0.1 to 1% by mass relative to the total mass of the toothpaste composition. The toothpaste composition according to claim 6.

8. The content of component (C) is 0.3 to 0.8% by mass relative to the total mass of the toothpaste composition. The toothpaste composition according to claim 6.

9. The content of component (C) is 0.3 to 0.7% by mass relative to the total mass of the toothpaste composition. The toothpaste composition according to claim 6.

10. The ratio of the mass of component (B) to the mass of component (C), as shown by component (B) / component (C), is between 0.4 and 8. The toothpaste composition according to claim 6.

11. The ratio of the mass of component (B) to the mass of component (C), as shown by component (B) / component (C), is between 1 and 8. The toothpaste composition according to claim 6.

12. The ratio of the mass of component (B) to the mass of component (C), as shown by component (B) / component (C), is between 2 and 5. The toothpaste composition according to claim 6.

13. The toothpaste composition according to claim 1, wherein the average molecular weight of component (B) is 280 to 630.

14. The toothpaste composition according to claim 1, wherein the average molecular weight of component (B) is 380 to 630.

Images