Oral composition

Abstract

Provided is an oral composition having good fluorine ion retention properties and good low-temperature storage stability. An oral composition containing: (A) sodium fluoride; (B) one or more substances selected from the group consisting of calcium lactate, calcium gluconate, calcium chloride, and calcium pantothenate; (C) one or more substances selected from condensed phosphoric acid and alkali metal salts thereof; and (D) isopropyl methyl phenol.

Description

TECHNICAL FIELD

[0001] The present application relates to an oral composition. BACKGROUND

[0002] Fluorides such as sodium fluoride are widely used as a medicinal ingredient for oral compositions such as dentifrices because of their caries-preventive effect. In order to make the fluorides effectively function, it is effective to make the fluoride ions stay in the mucous membranes and tooth surfaces in the oral cavity for a long time, and it is desirable that the fluoride ions remain in the oral cavity in a large amount even after rinsing the oral cavity with water or the like after use.

[0003] In Patent Literature 1, as an oral composition having high fluoride ion retention in the oral cavity, an oral composition containing a complex formed in an aqueous solution containing a polyphosphate, a calcium salt, and a fluoride salt is disclosed.

[0004] PRIOR ART DOCUMENTS PATENT LITERATURE Patent Literature 1: Japanese Patent Application Laid-Open No. 2009-137863 SUMMARY

[0005] PROBLEMS TO BE SOLVED BY THE INVENTION However, according to the research by the present inventors, the oral composition containing the above complex can be impaired in uniformity when stored at low temperature. For example, in the case where the oral composition is a toothpaste, wrinkles and particles can appear on the surface of the paste after storage at low temperature.

[0006] An object of the present application is to provide an oral composition having good fluoride ion retention and good low-temperature storage stability.

[0007] MEANS FOR SOLVING THE PROBLEMS The present application has the following modes.

[0008] [1] An oral composition containing: (A) sodium fluoride; (B) one or more selected from the group consisting of calcium lactate, calcium gluconate, calcium chloride, and calcium pantothenate; (C) one or more selected from the group consisting of condensed phosphoric acid and alkali metal salts thereof; and (D) isopropyl methyl phenol.

[0009] [2] The oral composition according to [1], wherein the (C) component contains one or more selected from the group consisting of pyrophosphoric acid and alkali metal salts of pyrophosphoric acid.

[0010] [3] The oral composition according to [1] or [2], wherein (D) / (A+B+C) representing the molar ratio of the (D) component to the total of the (A) component, the (B) component, and the (C) component is 0.001 to 0.5.

[0011] [4] The oral composition according to any one of [1] to [3], wherein the oral composition is a dentifrice.

[0012] Effects of the Invention According to the present application, an oral composition having good fluoride ion retention and good low-temperature storage stability is obtained. DETAILED DESCRIPTION

[0013] In the present specification, the "oral composition" means a composition whose main purpose is use in the oral cavity.

[0014] In the present specification, the "water-soluble" means a solubility of 1 g / 100 g or more in water at 20°C.

[0015] In the present specification, the "~" indicating a numerical range means that the numerical values recited before and after it are included as lower limit values and upper limit values.

[0016] [Oral Composition] The oral composition of the present application contains a (A) component, a (B) component, a (C) component, and a (D) component.

[0017] <(A) Component> The (A) component is sodium fluoride (NaF). The (A) component is a supply source of fluoride ions having a caries-preventive effect, and contributes to fluoride ion retention. The (A) component can be used as a commercially available product.

[0018] <(B) Component> The (B) component is a water-soluble calcium salt selected from one or more of calcium lactate, calcium gluconate, calcium chloride, and calcium pantothenate. Two or more (B) components can be combined.

[0019] The (B) component contributes to improvement in fluoride ion retention. In addition, it contributes to reduction in odor from the (D) component. The (B) component can be used as a commercially available product.

[0020] <(C) Component> The (C) component is at least one selected from condensed phosphoric acids and alkali metal salts thereof. Two or more (C) components can be combined.

[0021] The (C) component contributes to improvement in fluoride ion retention.

[0022] As the condensed phosphoric acid or alkali metal salt thereof, a water-soluble condensed phosphoric acid or salt thereof can be preferably used.

[0023] As the condensed phosphoric acid, for example, linear polyphosphoric acids such as pyrophosphoric acid, tripolyphosphoric acid, and tetrapolyphosphoric acid; and cyclic polyphosphoric acids such as trimetaphosphoric acid, tetrametaphosphoric acid, and hexametaphosphoric acid can be mentioned.

[0024] Examples of alkali metal salts that can be used for condensed phosphoric acid include sodium and potassium salts.

[0025] As component (C), alkali metal pyrophosphate, alkali metal tripolyphosphate, alkali metal hexametaphosphate, etc. are preferred. Alkali metal pyrophosphate is particularly preferred, and potassium pyrophosphate or sodium pyrophosphate is more preferred.

[0026] (C) The ingredients can be used in commercially available products.

[0027] (C) Component is preferably composed of one or more (C1) components selected from pyrophosphate and alkali metal pyrophosphate salts. The (C1) component has a particularly excellent effect on improving the fluoride ion retention performance.

[0028] The proportion of component (C1) relative to the total mass of component (C) can be, for example, 90% or more by mass, 95% or more by mass, 96% or more by mass, 97% or more by mass, 98% or more by mass, or 99% or more by mass, or it can be 100% by mass.

[0029] <(D) component> (D) is isopropyl methylphenol. Due to the presence of component (D), it exhibits excellent stability at low temperatures.

[0030] <Content of each component> The content of component (A) relative to the total mass of the oral composition is preferably 0.09% to 1.3% by mass, more preferably 0.10% to 1.1% by mass. If the content of component (A) is above the lower limit above, the fluoride ion retention is better. If the content of component (A) is below the upper limit above, the low-temperature storage stability is better.

[0031] The content of component (B) relative to the total mass of the oral composition is preferably 0.02% to 5.0% by mass, more preferably 0.03% to 3.0% by mass. If the content of component (B) is above the lower limit mentioned above, the fluoride ion retention is even better. If the content of component (B) is below the upper limit mentioned above, the fluoride ion retention is even better.

[0032] Furthermore, by combining component (B), the odor from component (D) can be reduced. If the content of component (B) is within the above range, the degree of elimination of the odor unique to component (D) is better, and the fragrance of the oral composition is better.

[0033] The content of component (C) relative to the total mass of the oral composition is preferably 0.02% to 3.0% by mass, more preferably 0.03% to 1.3% by mass. If the content of component (C) is above the lower limit above, the fluoride ion retention is better. If the content of component (C) is below the upper limit above, the low-temperature storage stability is better.

[0034] The content of the component (D) is preferably 0.01 to 0.2 mass%, more preferably 0.02 to 0.1 mass%, relative to the total mass of the oral composition. If the content of the component (D) is equal to or more than the lower limit of the above range, the low-temperature storage stability is more excellent. If the content of the component (D) is equal to or less than the upper limit of the above range, the peculiar odor of the component (D) is reduced, and the flavor of the oral composition is more excellent.

[0035] The molar ratio of the component (D) relative to the total of the components (A), (B), and (C), represented by (D) / (A+B+C), is preferably 0.001 to 0.5, preferably 0.008 to 0.25, more preferably 0.02 to 0.22. If (D) / (A+B+C) is equal to or more than the lower limit of the above range, the low-temperature storage stability is more excellent. If (D) / (A+B+C) is equal to or less than the upper limit of the above range, the fluoride ion retention property is more excellent.

[0036] < Water > The oral composition typically further contains water. As the water, purified water, sterilized purified water, water for injection, and the like can be given.

[0037] The content of water in the oral composition can be appropriately set depending on the product form and the method of use of the oral composition.

[0038] For example, in the case where the oral composition is a toothpaste, the content of water relative to the total mass of the oral composition is preferably 5 to 90 mass%, more preferably 10 to 60 mass%, further preferably 20 to 50 mass%.

[0039] < Other Components > The oral composition can further contain other components than the components (A), (B), (C), (D), and water.

[0040] The other components can be appropriately selected from publicly known components in consideration of the form and the method of use of the oral composition, and the like. As examples of the other components, abrasives, binders, thickening agents, surfactants, colorants, sweeteners, preservatives, flavorings, effective components other than isopropylmethylphenol, pH adjustors, and the like can be given.

[0041] As the surfactant, publicly known surfactants in oral compositions can be used. For example, nonionic surfactants, amphoteric surfactants, anionic surfactants, and the like can be given.

[0042] As the nonionic surfactant, for example, polyoxyethylene alkyl ether, polyoxyethylene hydrogenated castor oil, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester (for example, polyoxyethylene sorbitan monostearate), alkanolamide, polyoxyethylene fatty acid ester, polyoxyethylene alkenyl ether, glycerin fatty acid ester, sucrose fatty acid ester (for example, maltose fatty acid ester), sugar alcohol fatty acid ester (for example, maltitol fatty acid ester, lactitol fatty acid ester), fatty acid diethanolamide (for example, lauric acid monoethanolamide or lauric acid diethanolamide), polyoxyethylene polyoxypropylene copolymer, polyoxyethylene polyoxypropylene fatty acid ester, polyoxyethylene polyoxypropylene (EOPO) copolymer, alkyl glucoside, polyglycerin fatty acid ester can be mentioned.

[0043] The number of carbon atoms of the alkyl group of the polyoxyethylene alkyl ether is usually 12 to 18, preferably 14 to 18 (for example, lauryl group, stearyl group), and the average addition mole number of ethylene oxide is usually 5 moles to 30 moles, preferably 15 moles to 30 moles.

[0044] The average addition mole number of ethylene oxide of the polyoxyethylene hydrogenated castor oil is usually 5 moles to 100 moles, preferably 20 moles to 100 moles, more preferably 20 moles to 60 moles.

[0045] The number of carbon atoms of the fatty acid of the sorbitan fatty acid ester is usually 12 to 18. The number of carbon atoms of the fatty acid of the polyoxyethylene sorbitan fatty acid ester is usually 16 to 18, and the average addition mole number of ethylene oxide is usually 10 moles to 40 moles.

[0046] The number of carbon atoms of the alkyl chain of the alkanolamide is usually 12 to 14.

[0047] The polyoxyethylene polyoxypropylene (EOPO) copolymer is preferably a block copolymer or a random copolymer in which the average addition mole number of ethylene oxide is 20 to 210 and the average addition mole number of propylene oxide is 15 to 60.

[0048] As the amphoteric surfactant, for example, betaine type amphoteric surfactants and amino acid type amphoteric surfactants can be given. As the betaine type amphoteric surfactant, for example, fatty acid amide propyl betaine (e.g., coco fatty acid amide propyl betaine), alkyl betaine (e.g., lauryl dimethylamino acetic acid betaine and the like alkyl amino acetic acid betaine), alkyl imidazoline betaine (e.g., alkyl carboxymethyl hydroxyethyl imidazoline betaine) can be given. Among them, fatty acid amide propyl betaine, alkyl betaine are preferred, and coco fatty acid amide propyl betaine is more preferred. In the case where the amphoteric surfactant has an alkyl group or an acyl group, they can be either of a straight chain and a branched chain, and either of an alkyl group or an acyl group, saturated and unsaturated. The number of carbon atoms of the alkyl group or the acyl group is preferably 10 to 20, more preferably 12 to 18, and further preferably 14 to 16.

[0049] As the anionic surfactant, for example, alkyl sulfate salts (e.g., sodium dodecyl sulfate (SDS)), alkyl arylsulfonate salts (e.g., sodium dodecylbenzenesulfonate), fatty acid salts (e.g., sodium stearate), alkenyl sulfonate salts (AOS), lauroyl methyl taurine (LMT), sulfosuccinic acid, GluNa, alanine salts, and the like can be given. The alkyl group, the acyl group can be either of a straight chain and a branched chain, and either of saturated and unsaturated. The number of carbon atoms of the alkyl group or the acyl group is preferably, for example, 10 to 20, more preferably 12 to 18, and further preferably 14 to 16. α

[0050] The salt is selected from pharmacologically allowable salts. As the pharmacologically allowable salts, for example, base addition salts and amino acid salts can be given. As the salt, inorganic base salts such as sodium salt, potassium salt, calcium salt, magnesium salt, ammonium salt; organic base salts such as triethylammonium salt, triethanolammonium salt, pyridinium salt, diisopropylammonium salt; basic amino acid salts such as arginine salt can be given. Among them, inorganic base salts are preferred, and alkali metal salts (e.g., sodium salt, potassium salt) or ammonium salts are more preferred, and sodium salt is further preferred.

[0051] The content of the surfactant in the case where the oral composition contains the surfactant is preferably 0.05% by mass to 10.0% by mass, and more preferably 0.1% by mass to 8.0% by mass, relative to the total mass of the oral composition.

[0052] As the abrasive, for example, silica-based abrasives such as anhydrous silicic acid, precipitated silica, silica gel, aluminum silicate, zirconium silicate; calcium hydrogen phosphate dihydrate or anhydride, calcium dihydrogen phosphate, tricalcium phosphate, tetracalcium phosphate (Japanese original: "4th calcium phosphate"), calcium carbonate, calcium hydroxide, aluminum hydroxide, insoluble sodium metaphosphate, trimagnesium phosphate, magnesium carbonate can be given. Silica-based abrasives are particularly preferred.

[0053] ​The content of the abrasive is preferably 0 to 60 mass%, more preferably 0 to 30 mass%, and can also be 25 mass% or less, for example, relative to the total mass of the oral composition. A content of 0 mass% means that no abrasive is contained.

[0054] As the binder, for example, organic binders selected from carboxymethylcellulose sodium, methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, and the like cellulose derivatives; xanthan gum, gum tragacanth, gum karaya, gum arabic, and the like gums; sodium polyacrylate and the like polyacrylic acid salts; water-soluble high molecular substances, thickening silica, thickening aluminum silicate, propolis, montmorillonite, and the like inorganic binders can be mentioned.

[0055] The content of the binder is preferably 0.05 to 13.0 mass%, for example, relative to the total mass of the oral composition.

[0056] In the case where the binder contains an organic binder, the content of the organic binder is more preferably 0.1 to 3 mass%, and more preferably 0.5 to 2.5 mass%, relative to the total mass of the oral composition.

[0057] In the case where the binder contains an inorganic binder, the content of the inorganic binder is more preferably 0 to 10.0 mass%, and further preferably 0 to 8.0 mass%, relative to the total mass of the oral composition, from the viewpoint of the adsorptivity of fluoride ions to the tooth surface.

[0058] As the thickening agent, for example, sugar alcohols such as sorbitol, xylitol, erythritol, maltitol, and the like, glycerol, propylene glycol, polyhydric alcohols such as polyethylene glycol having an average molecular weight of 160 to 400 (average molecular weight described in Yakuhinbu-gaihyou Specified Values 2006), and the like can be mentioned.

[0059] The content of the thickening agent is preferably 20 to 70 mass%, and more preferably 25 to 65 mass%, for example, relative to the total mass of the oral composition.

[0060] As the coloring agent, for example, Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green No. 3, mica titanium, titanium oxide, and the like can be mentioned.

[0061] As the sweetening agent, for example, sodium saccharin, aspartame, stevioside, stevia extract, p-methoxy cinnamyl aldehyde, neohesperidin dihydrochalcone, perillartine, and the like can be mentioned.

[0062] As the preservative, for example, p-hydroxybenzoic acid esters such as methyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, butyl p-hydroxybenzoate, and the like; benzoic acid and its salts such as sodium benzoate can be mentioned.

[0063] As the flavor, for example, menthol, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cinnamon oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, Asian mint oil, cardamom oil, coriander oil, mandarin oil, raspberry oil, lavender oil, rosemary oil, bay oil, chamomile oil, cumin oil, marjoram oil, lilac oil, jasmine oil, grapefruit oil, white gold grapefruit oil, yuzu oil, iris extract, natural flavors such as peppermint essence, rose essence, and orange flower; flavors obtained by processing (front fraction removal, rear fraction removal, fractionation, liquid-liquid extraction, concentration, powdering, and the like) of these natural flavors; menthol, carvone, anethole, eucalyptol, methyl salicylate, cinnamic aldehyde, eugenol, 3-L-menthoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone, menthyl acetate, N-substituted-p-menthane-3-carboxamide, pinene, octanal, citral, pulegone, carvacryl acetate, anisic aldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexylpropionate, methyl anthranilate, ethyl methylphenylglycidate, vanillin, undecanolide, hexanal, butanol, isopentanol, hexenol, dimethyl sulfide, cyclic glycoside, furfural, trimethylpyrazine, ethyl lactate, ethyl thioacetate, and other single flavor materials; blended flavors such as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mixed flavor, and tropical fruit flavor, which can be used in combination as a known flavor raw material for oral compositions.

[0064] The content of the flavor is not particularly limited, and the content of the above-mentioned flavor raw material is preferably 0.000001 to 1% by mass relative to the total mass of the oral composition. The content of the flavoring flavor using the above-mentioned flavor raw material is preferably 0.05 to 2% by mass relative to the total mass of the oral composition.

[0065] As the active ingredient, for example, bactericides such as cetylpyridinium chloride, water-soluble phosphoric acid compounds (except for the (C) component) such as potassium salt and sodium salt of orthophosphoric acid, enzymes such as glucanase, mutanase, amylase, and protease, tranexamic acid, e - aminohexanoic acid, triclosan, lysozyme chloride, chlorohydroxyl aluminum allantoinate, hinokitiol, ascorbic acid, tocopherol acetate, dihydrocholesterol, α - bisabolol, chlorhexidine salts, azulene, copper sodium chlorophyllin, chlorophyll, water-soluble copper compounds such as copper gluconate, aluminum lactate, strontium chloride, potassium nitrate, berberine, hydroxamic acid or its derivative, glycyrrhizic acid or its salt, glycyrrhetic acid or its derivative, tartar-preventing agent. The above-mentioned active ingredients can be combined in an effective amount within a range not impairing the effects of the present application.

[0066] As the pH adjusting agent, for example, sodium hydroxide can be mentioned.

[0067] <Shape, dosage form> The oral composition can be prepared, for example, in various shapes such as a liquid, a paste, a gel, a solid, and the like.

[0068] The dosage form of the oral composition is not particularly limited. The dosage form of the oral composition is typically an oral preparation which is discharged from the oral cavity after use. As the oral preparation, for example, dentifrices (liquid dentifrices, liquid dentifrices, toothpastes, wet dentifrices, powder dentifrices, and the like), mouthwashes, gargles, coating agents, oral sprays, adhesion agents, tablets, intraoral sustained-release agents, chewable agents, intraoral dissolving agents, intraoral disintegrating agents, tongue care agents, mouth fresheners, denture care agents, and the like can be mentioned.

[0069] The oral composition of the present embodiment is suitable as a dentifrice, particularly as a toothpaste, among the above.

[0070] The oral composition of the present embodiment can be prepared by a publicly known method. For example, it can be prepared by mixing the components (A), (B), (C), and (D), and other components as necessary, using a general method.

[0071] In the oral composition, the fluoride ion retention is improved by forming a complex of the fluoride ion, the calcium ion, and the phosphorus ion. On the other hand, the complex has an anionic charge and is easily gelled at a low temperature, and it is considered that this is a cause of the decrease in the low-temperature storage stability.

[0072] The formation of the above complex can be confirmed by observing the crystallite diameter by X-ray crystal structure analysis and the exothermic peak at the time of the departure of the crystal water near the phosphate group near 450°C by thermal gravimetric analysis (TG-DTA measurement). That is, if the complex is formed, the crystallite diameter calculated from the diffraction peak attributed to CaF2 is less than 10 nm by the complexation with the phosphate group. In addition, the generation of the peak of the crystal water indicates that the CaF2 found in the X-ray crystal structure analysis is not a crystal composed of calcium and fluoride ions, but a complex formed after the interaction of the phosphate group.

[0073] Specifically, the formation of the complex is confirmed by confirming that the crystallite diameter is less than 10 nm in the following method (1) and the exothermic peak at 450°C is present in the following method (2).

[0074] (1) Crystallite diameter An X-ray structure diffractometer (light source Cu: K α , 40 kV, 20 mA, divergence slit 1 / 2 deg, scattering slit 1 / 2 deg, light receiving slit 0.15 mm, scanning speed 4.000 ° / min, 2theta = 2.000° ~ 80.000°) and the crystal diameter was calculated by the following formula (Scherrer formula) to evaluate the presence or absence of complex formation.

[0075] L = K lambda / ( β cos theta ) L: crystallite diameter, K: coefficient 0.9, β : half-value width, lambda : 1.54056 A, theta : diffraction angle (2) TG-DTA measurement (exothermic peak) Rising rate: 5°C / min, measurement range: 25°C ~ 600°C As the method of forming the above complex, there is no particular limitation, and in the preparation of the oral composition, for example, either of the procedures of combining the (A) component and the (C) component after combining the (B) component, or combining the (B) component and the (C) component after combining the (A) component is preferably employed. Note that if the (A) component and the (B) component are combined at the same time, calcium fluoride is generated in part, and the efficiency of complex formation can possibly become poor.

[0076] Since the above-described oral composition contains the (A) component, the (B) component, the (C) component, and the (D) component, the fluoride ion retention is excellent, and the low-temperature storage stability is also excellent. For example, when the oral composition is a toothpaste, the paste surface after low-temperature storage is excellent.

[0077] Examples Hereinafter, the present application will be described in detail using experimental examples, but the present application is not limited to the following description.

[0078] Note that in the following examples, "%" as the unit of content means "mass %" unless otherwise specified.

[0079] <Usage of Raw Materials> [(A) Component] Sodium fluoride: manufactured by Stella Chemifa Corporation. Hereinafter, also referred to as "NaF".

[0080] [(B) Component] Calcium lactate hydrate: manufactured by Taihei Chemical Industrial Co., Ltd., trade name "Calcium Lactate". Hereinafter, also referred to as "lactic acid Ca".

[0081] Calcium gluconate: manufactured by Fusosan Chemical Industry Co., Ltd.. Hereinafter, also referred to as "gluconic acid Ca".

[0082] Calcium chloride: Manufactured by Tomita Pharmaceutical Co., Ltd. Hereinafter also referred to as "Ca chloride".

[0083] Calcium pantothenate: Manufactured by BASF. Also referred to below as "Pamoate (Ca)".

[0084] [(C) Component] Tetrapotassium pyrophosphate: Manufactured by Taihei Chemical Industry Co., Ltd. Hereinafter also referred to as "K pyrophosphate".

[0085] Sodium pyrophosphate: Manufactured by Taihei Chemical Industry Co., Ltd., product name "Sodium pyrophosphate (anhydrous)". Hereinafter also referred to as "Na pyrophosphate".

[0086] Sodium tripolyphosphate: Manufactured by Taihei Chemical Industry Co., Ltd. Hereinafter also referred to as "Na tripolyphosphate".

[0087] [(D) component] Isopropylmethylphenol: 4-Isopropyl-3-methylphenol, manufactured by Osaka Chemical Co., Ltd., product name "BIOSOL". Also referred to below as "IPMP".

[0088] [spices] The fragrance composition A is described in Table 5 below.

[0089] [water] Purified water.

[0090] [Common components (any components)] Anhydrous silica (abrasive silica) 10%, sorbitol liquid (70% concentration, thickener) 40%, propylene glycol (thickener) 3%, xanthan gum (binder) 0.5%, sodium polyacrylate (binder) 0.5%, sodium lauryl sulfate 0.5%, and sodium saccharin (sweetener) 0.2%. Total 44.7%.

[0091] <Examples 1-21, Comparative Examples 1-4> The oral composition (toothpaste) with the compositions shown in Tables 1-4 was prepared using conventional methods. The components were mixed in the following order: aqueous solution of component (C), aqueous solution of component (B), and aqueous solution of component (A) to prepare a premix. The amount of water was set to the amount required to achieve the compositions shown in the table. Phase A was prepared by adding water-soluble components (sorbitol solution, sodium saccharin) to this premix and dissolving them. Meanwhile, Phase B was prepared by dissolving sodium polyacrylate, xanthan gum, and sodium lauryl sulfate in propylene glycol at room temperature and dispersing them. Next, Phase B was added to Phase A while stirring to prepare Phase C. Furthermore, Phase D was prepared by dissolving isopropyl methylphenol in fragrance at room temperature and dispersing it. Phase D and anhydrous silica were added to Phase C, and the mixture was mixed at room temperature using a 1.5L kneader (manufactured by Ishiyama Works), and degassed under reduced pressure to 4 kPa to obtain 1.0 kg of toothpaste.

[0092] In each of the toothpastes, it was confirmed that the fluoride ions, calcium ions, and phosphorus ions were formed into complexes by the above method.

[0093] The blank in the table indicates that the ingredient was not blended. The "remainder" of purified water indicates an amount of 100% of the total amount of the oral composition.

[0094] The obtained oral compositions (toothpastes) were subjected to the following evaluations. The results are collectively shown in the table.

[0095] < Evaluation Method > [Fluoride ion retention] The retention of fluoride ions in enamel was evaluated by the following method.

[0096] A liquid in which the oral composition was diluted 4 times with purified water was applied to a 6 mm x 6 mm square section made of bovine enamel for 3 minutes, and immediately washed 3 times with purified water. After drying the section, 120 mu L artificial saliva for 3 minutes, the concentration (unit: ppm (mass standard)) of the extracted fluoride ions was measured using an ion meter (product name: Orion 1115000 4-Star, manufactured by Thermo Fisher Scientific, Inc.), the average value for N = 3 was calculated, and evaluated according to the following criteria.

[0097] (Evaluation Criteria) ◎: 0.3 ppm or more.

[0098] O: 0.2 ppm or more and less than 0.3 ppm.

[0099] Δ: 0.1 ppm or more and less than 0.2 ppm.

[0100] X: Less than 0.1 ppm.

[0101] [Low-temperature storage stability (appearance stability of the paste surface)] Each 50 g of the oral composition was filled into 3 tube containers (raw material: laminated tube (manufactured by Dainippon Printing Co., Ltd.) with a diameter of 26 mm containing straight-chain low-density polyethylene, the innermost layer), and stored in an atmosphere of -5°C for 1 month.

[0102] At -5°C, the composition was taken out from the tube onto a paper for evaluation as 15 cm x 3 strips, and the composition was slightly flattened in a manner that the paper for evaluation was bent, and the paper was unfolded to the original state, and the paste surface of the composition at that time was evaluated according to the following scoring criteria. The amount of 3 tubes was evaluated in the same manner, and the average was evaluated according to the following evaluation criteria.

[0103] (score criteria) 5 points: no wrinkles, no particles, and the surface is glossy.

[0104] 4 points: several wrinkles, and no gloss.

[0105] 3 points: several wrinkles, and particles.

[0106] 2 points: wrinkles and particles can be confirmed.

[0107] 1 point: a large amount of wrinkles and particles can be confirmed, and the composition is not uniform.

[0108] (evaluation criteria) ◎: average score is 4.6 or more.

[0109] O: average score is 4.3 or more and less than 4.6.

[0110] △: average score is 4.0 or more and less than 4.3.

[0111] X: average score is less than 4.0.

[0112] [Odor (degree of elimination of odor)] As a subject, evaluation was performed by using a sensory test based on 10 panelists. 1 g of the oral composition was extruded from a tube container in which the oral composition was housed, placed on a toothbrush (manufactured by Lion Corporation, Clinica Toothbrush 4-row brush head, medium size), and brushing was performed for 3 minutes. The degree of elimination of odor felt during use was determined according to the following score criteria.

[0113] The average of the scores of 10 people was calculated, and the odor (degree of elimination of odor) was evaluated according to the following evaluation criteria.

[0114] (score criteria) 4 points: no odor at all.

[0115] 3 points: almost no odor.

[0116] 2 points: slightly odor.

[0117] 1 point: odor.

[0118] (evaluation criteria) ◎: average score is 3.5 or more.

[0119] O: average score is 3.0 or more and less than 3.5.

[0120] △: average score is 2.0 or more and less than 3.0.

[0121] X: average score is less than 2.0.

[0122] [Table 1]

[0123] [Table 2]

[0124] [Table 3]

[0125] [Table 4]

[0126] As shown in the above results, the fluoride ion retention of the oral compositions of Examples 1 to 21 is excellent, and the low-temperature storage stability is excellent. Furthermore, there is no peculiar odor of isopropyl methyl phenol, and the fragrance is excellent.

[0127] On the other hand, Comparative Example 1 not containing the (A) component, Comparative Example 2 not containing the (B) component, and Comparative Example 3 not containing the (C) component have good low-temperature storage stability, but poor fluoride ion retention. The fragrance of Comparative Example 2 is also poor.

[0128] Comparative Example 4 not containing the (D) isopropyl methyl phenol has good fragrance, but poor low-temperature storage stability.

[0129] <Formula Examples> In any of the following formula examples, the fluoride ion retention, the low-temperature storage stability, and the fragrance (degree of elimination of peculiar odor) are excellent.

[0130] <Formula Example 1 Toothpaste> Sodium fluoride 0.32% Calcium lactate 0.2% Sodium pyrophosphate 0.1% Isopropyl methyl phenol 0.05% Anhydrous silicic acid 10% Sorbitol solution (70%) 40% Propylene glycol 3% Xanthan gum 0.3% Cocofatty acid amide propyl betaine 0.5% Sodium saccharin 0.2% Fragrance composition A 1% Purified water remainder <Formula Example 2 Toothpaste> Sodium fluoride 0.32% Calcium lactate 0.2% Sodium pyrophosphate 0.1% Isopropyl methyl phenol 0.05% Anhydrous silicic acid 10% Sorbitol solution (70% concentration) 40% Propylene glycol 3% Xanthan gum 0.5% Sodium polyacrylate 0.5% Polyoxyethylene hydrogenated castor oil 0.5% Saccharin sodium 0.2% Flavor composition A 1% Purified water remainder <Formula Example 3 Toothpaste> Sodium fluoride 0.32% Calcium lactate 0.2% Potassium pyrophosphate 0.1% Isopropyl methyl phenol 0.05% Anhydrous silicic acid 10% Sorbitol solution (70% concentration) 40% Propylene glycol 3% Xanthan gum 0.5% Sodium polyacrylate 0.5% Polyoxyethylene hydrogenated castor oil 0.5% Saccharin sodium 0.2% Flavor composition A 1% Purified water remainder <Formula Example 4 Liquid dentifrice> Sodium fluoride 0.32% Calcium lactate 0.2% Sodium pyrophosphate 0.1% Glycerin 7.5% Propylene glycol 3% Sorbitol solution (70%) 5% Cocofatty acid amide propyl betaine 0.3% Isopropyl methyl phenol 0.05% Flavor composition A 0.2% Purified water remainder <Formula Example 5 Mouthwash> Sodium fluoride 0.1% Calcium lactate 0.2% Sodium pyrophosphate 0.1% Isopropyl methyl phenol 0.05% Propylene glycol 2% Sorbitol solution (70%) 3% Isopropyl methyl phenol 0.05% Flavor composition A 0.2% Purified water remainder Also, in the above Examples 1 to 21 and the above Formulation Examples 1 to 5, instead of the perfume composition A, the same composition was prepared except that the perfume compositions B to P described in Tables 5 and 6 below were used, respectively, and as a result, both the fluoride ion retention and the low-temperature storage stability were good, there was no peculiar odor of isopropyl methyl phenol, and the fragrance was also good.

[0131] The compositions of the essential oils 1 to 7 and the solvents described in Tables 5 and 6 are shown in Tables 7 to 14.

[0132] Note that "a% of the front fraction removed" in the table means the first a% removed when the essential oil is fractionated, and "b% of the front fraction and the back fraction removed" means the first b% and the last b% removed when the essential oil is fractionated.

[0133] [Table 5]

[0134] [Table 6]

[0135] [Table 7]

[0136] [Table 8]

[0137] [Table 9]

[0138] [Table 10]

[0139] [Table 11]

[0140] [Table 12]

[0141] [Table 13]

[0142] [Table 14]

Claims

1. An oral composition characterized in that, contains: (A) sodium fluoride; (B) one or more selected from the group consisting of calcium lactate, calcium gluconate, calcium chloride, and calcium pantothenate; (C) one or more selected from the group consisting of condensed phosphoric acids and alkali metal salts thereof; and (D) isopropylmethylphenol.

2. The oral composition of claim 1, wherein, The condensed phosphoric acid is selected from one or more of pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, trimetaphosphoric acid, tetrametaphosphoric acid, and hexametaphosphoric acid.

3. The oral composition of claim 1, wherein, The (C) component contains one or more selected from the group consisting of pyrophosphoric acid and alkali metal salts of pyrophosphoric acid.

4. The oral composition of claim 1, wherein, (D) / (A+B+C) representing the molar ratio of the (D) component with respect to the total of the (A) component, the (B) component, and the (C) component is 0.001 to 0.

5.

5. The oral composition of claim 1, wherein, The content of the (A) component is 0.09 mass% to 1.3 mass% with respect to the total mass of the oral composition. The content of the (B) component is 0.02 mass% to 5.0 mass% with respect to the total mass of the oral composition.

6. The oral composition of claim 1, wherein, The content of the (C) component is 0.02 mass% to 3.0 mass% with respect to the total mass of the oral composition.

7. The oral composition of claim 1, wherein, The content of the (D) component is 0.01 mass% to 0.2 mass% with respect to the total mass of the oral composition.

8. The oral composition of claim 1, wherein, The oral composition is a toothpaste.

9. The oral composition according to any one of claims 1 to 8, wherein, ​

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