Oral care composition

Abstract

An oral care composition according to the present invention contains a surface-treated calcium carbonate (A) component and a fluidity-imparting material (B) component. Here, the surface-treated calcium carbonate (A) component is a particle that has a BET specific surface area of 3 to 50 m2 / g and is provided with a coating layer containing a surface treatment agent on the surface thereof. Furthermore, the pH of a test solution obtained by adding 10 parts by mass of purified water to 100 parts by mass of the oral care composition is in the range of 8-12.

Description

Oral care composition

[0001] The present invention relates to oral care compositions.

[0002] Brushing your teeth has long been a method of preventing caries, periodontitis, and pigmentation. Originally, tooth brushing involved brushing with a toothpaste primarily composed of abrasives and surfactants to remove various deposits and food debris that cause caries and periodontitis. However, there are subtle recesses on the tooth surface that cannot be reached by abrasive particles or toothbrush bristles, making it difficult to remove deposits and plaque that have accumulated in these areas with abrasives.

[0003] Furthermore, conventional techniques for preventing dental caries have focused on preventing the elution of minerals from teeth by microorganisms, such as preventing the adhesion of plaque to the tooth surface, removing plaque that has adhered to the tooth surface (brushing), killing microorganisms in plaque with disinfectants or antibacterial agents, or regulating the intake of sugar or consuming sugar substitutes.

[0004] Despite the wide range of preventive methods available as described above, it is difficult to completely prevent various dental conditions such as caries, periodontitis, and pigmentation, and many people currently suffer from these conditions.

[0005] The pellicle (organic film / acquired film) that covers the tooth surface is considered to be the biggest factor. Pellicle, a colorless and transparent protein derived from saliva, protects teeth from physical stimuli, inhibits acid dissolution of tooth tissue, and promotes remineralization. However, it also easily adsorbs bacteria and pigments that cause caries, periodontitis, and pigmentation. Bacteria adsorbed to the pellicle settle and multiply, forming plaque, which, if further progressed, can cause caries and periodontitis.

[0006] Plaque can be removed by careful brushing, but the pellicle is difficult to remove, raising concerns that stubborn bacterial flora that cannot be removed may develop into disease.

[0007] Pellicle removal is difficult with brushing alone, so it must be done periodically with a specialized tool. Pellicle removal is essential for preventing dental caries and periodontal disease and for removing stains, so there is a strong demand for a method for easily removing pellicles on a daily basis.

[0008] The present invention aims to solve the above problems, and its purpose is to provide an oral care composition that can effectively remove the pellicle from the oral cavity, which is the basis for bacterial adhesion that causes caries and pigment adsorption that causes tooth discoloration.

[0009] The present invention provides an oral care composition comprising a surface-treated calcium carbonate (A) component and a fluidity-imparting material (B) component, wherein the surface-treated calcium carbonate (A) component has a viscosity of 3 to 50 m / s. ２ The oral care composition is a particle having a BET specific surface area of ​​1 / g and having a coating layer on the surface thereof containing a surface treatment agent, and the pH of a test solution obtained by adding 10 parts by mass of purified water to 100 parts by mass of the oral care composition is 8 to 12.

[0010] In one embodiment, the surface treatment agent is at least one selected from the group consisting of anionic surfactants and polysaccharides.

[0011] In a further embodiment, the surface treatment agent is at least one selected from the group consisting of sodium polyacrylate, sodium lauryl sulfate, gum arabic, and sodium carboxymethylcellulose.

[0012] In one embodiment, the component (A) satisfies the following formulas (a), (b), and (c): (a) 0.1≦As≦5 (mg / m ２ ) (b) 0.05≦Dx50≦5 (μm) (c) 0.1≦Dx100≦100 (μm) As is the thermal loss (mg / g) of the component (A) at 200 to 500°C (N １ ) and BET specific surface area (m ２ / g) (B １ ) and the ratio (N １ / B １) Dx50 is the median diameter (μm) of the component (A) measured with a laser diffraction particle size distribution analyzer; and Dx100 is the maximum diameter (μm) of the component (A) measured with a laser diffraction particle size distribution analyzer.

[0013] In one embodiment, the component (B) is at least one selected from the group consisting of water, a wetting agent, a thickening agent, and a binder.

[0014] In one embodiment, the content of the component (A) is 20 to 70 mass % based on the total mass of the composition.

[0015] In one embodiment, the mass ratio of the component (A) to the component (B) (component (A) / component (B)) is 0.3 to 2.0.

[0016] In one embodiment, the oral care composition of the present invention further comprises a cleaning agent (C) component.

[0017] In a further embodiment, the component (C) is at least one selected from the group consisting of ground calcium carbonate, light calcium carbonate, and silica.

[0018] In a further embodiment, the component (C) satisfies the following formulas (d) and (e): (d) 0.5≦Dx50≦50 (μm) (e) 5≦Dx100≦500 (μm), where Dx50 is the median diameter (μm) of the component (C) measured with a laser diffraction particle size distribution analyzer; and Dx100 is the maximum diameter (μm) of the component (C) measured with a laser diffraction particle size distribution analyzer.

[0019] In a further embodiment, the total content of the component (A) and the component (C) is 20 to 70 mass % based on the total mass of the composition, the content of the component (A) is 5 to 60 mass % based on the total mass of the composition, and the content of the component (C) is 10 to 65 mass % based on the total mass of the composition.

[0020] In one embodiment, the oral care compositions of the present invention are used to remove the pellicle in the oral cavity and on the teeth.

[0021] According to the present invention, pellicles present in the oral cavity and between teeth can be easily removed. For example, the oral care composition of the present invention can remove pellicles simply by application, without necessarily requiring special brushing. Therefore, tooth wear can be suppressed, and the composition is also useful for oral care after implants, dentures, and other prosthetic replacements.

[0022] The present invention will be described in detail below.

[0023] 1. Oral Care Composition The oral care composition of the present invention can be provided for the purpose of removing, for example, the pellicle, which serves as the basis for bacterial adhesion that causes dental caries and pigment adsorption that causes tooth discoloration, and contains, as constituents, a surface-treated calcium carbonate component (A) and a fluidity-imparting material component (B).

[0024] (Surface-treated calcium carbonate (A) component) The surface-treated calcium carbonate (A) component in the present invention is 3 to 50 m ２ The powder has a BET specific surface area of ​​1 / g and has a particle form having a coating layer containing a surface treatment agent on the surface.

[0025] The surface-treated calcium carbonate (A) is used to polish the tooth surface or to remove the pellicle by applying it to the tooth surface. ２ If the BET specific surface area of ​​component (A) is less than 50 m / g, the resulting surface-treated calcium carbonate particles will be too large, and even if the pellicle covering the tooth surface can be partially removed, it will be difficult to completely remove the pellicle from subtle recesses and gaps in the teeth, as well as scratches and irregularities on the tooth surface. ２ If the BET specific surface area of ​​the surface-treated calcium carbonate (A) component in the present invention is more preferably 10 to 40 m / g, the resulting surface-treated calcium carbonate is too small and tends to aggregate, resulting in a lack of dispersion stability. ２ / g, and even more preferably 20 to 35 m ２ / g.

[0026] The BET specific surface area can be measured using, for example, a BET specific surface area measuring device (fully automatic specific surface area measuring device Macsorb; manufactured by Mountec Co., Ltd.) under the following conditions.

[0027] <Conditions for measuring BET specific surface area (Sw)> 0.2 to 0.3 g of the surface-treated calcium carbonate to be measured is placed in a measuring device, and a pretreatment is carried out, in which the calcium carbonate is heated at 200°C for 5 minutes in a mixed gas atmosphere of nitrogen and helium, followed by low-temperature, low-humidity physical adsorption in a liquid nitrogen environment, after which the specific surface area is measured using the measuring device.

[0028] The calcium carbonate material constituting the surface-treated calcium carbonate (A) component is not particularly limited, and examples thereof include heavy calcium carbonate obtained by a physical production method, light calcium carbonate obtained by chemical synthesis, and combinations thereof. For production reasons such as ease of adjusting the particle size distribution, the calcium carbonate material used is preferably light calcium carbonate obtained by chemical synthesis.

[0029] Among light calcium carbonate, finer particles are called colloidal calcium carbonate, etc., and are synthesized in the same manner as light calcium carbonate, but are useful in that they have a colloidal shape, whereas general light calcium carbonate has a spindle shape.

[0030] In applications such as the present invention, where the purpose is to apply the composition to tooth surfaces, colloidal calcium carbonate is more preferred because it is finer and has excellent particle uniformity.

[0031] In the present invention, a coating layer made of a surface treatment agent is formed on the surface of the calcium carbonate in order to maintain the dispersion stability of the calcium carbonate and its stability as an oral care composition. For example, when a coating layer made of a hydrophilic surface treatment agent is formed on the surface of calcium carbonate, the dispersion stability of the obtained surface-treated calcium carbonate and its stability as an oral care composition can be maintained. Furthermore, since the coating layer quickly penetrates not only the tooth surface but also fine details such as periodontal pockets and fine scratches on the tooth surface, it can be removed more effectively than a pellicle.

[0032] The surface treatment agent contained in the coating layer may be, for example, a polysaccharide, a surfactant, or a combination thereof, because they have dispersion stability and good compatibility with calcium carbonate. Examples of the surfactant include anionic surfactants, amphoteric surfactants, nonionic surfactants, cationic surfactants, and combinations thereof.

[0033] Examples of polysaccharides include tamarind seed gum, guar gum, locust bean gum, gum arabic, karaya gum, pectin, cellulose, sodium carboxymethylcellulose, soybean polysaccharides, carrageenan, alginate esters, xanthan gum, and gellan gum, and combinations thereof. Among these, gum arabic and sodium carboxymethylcellulose are preferred.

[0034] Examples of anionic surfactants include polyacrylates (e.g., sodium polyacrylate), alkyl sulfates (e.g., sodium lauryl sulfate), acylamino acid salts (e.g., sodium lauroyl methyl taurate), hydrogenated coconut fatty acid monoglyceride monosulfate (e.g., sodium hydrogenated coconut fatty acid monoglyceride monosulfate), and lauryl sulfoacetate (e.g., sodium lauryl sulfoacetate), as well as combinations thereof. Examples of salts that can constitute the anionic surfactant include inorganic salts such as sodium salts, potassium salts, magnesium salts, and ammonium salts; organic base salts such as triethylammonium salts, triethanolammonium salts, pyridinium salts, and diisopropylammonium salts; and amino acid salts such as arginine salts, lysine salts, and histidine salts. Among these, sodium polyacrylate and alkyl sulfates (e.g., sodium lauryl sulfate) are preferred.

[0035] Examples of amphoteric surfactants include betaine-type amphoteric surfactants such as alkyl dimethylamino acetate salts (e.g., lauryl dimethylamino acetate betaine) and fatty acid amidopropyl dimethylamino acetate betaine (e.g., cocamidopropyl betaine); imidazoline-type amphoteric surfactants such as N-fatty acid acyl-N-carboxymethyl-N-hydroxyethyl ethylenediamine salts (e.g., N-coconut oil fatty acid acyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine), coconut oil fatty acid imidazolinium betaine, and 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine; alkyl betaines such as lauryl dimethylamino acetate betaine; and natural lecithin, as well as combinations thereof.

[0036] Examples of nonionic surfactants include polyoxyethylene alkyl ethers, 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, glycerin fatty acid esters, sucrose fatty acid esters (e.g., maltose fatty acid esters), sugar alcohol fatty acid esters (e.g., maltitol fatty acid esters, lactitol fatty acid esters), fatty acid diethanolamides (e.g., lauric acid mono- and diethanolamides), polyoxyethylene polyoxypropylene copolymers, polyoxyethylene polyoxypropylene fatty acid esters, and natural saponins, as well as combinations thereof.

[0037] Cationic surfactants include, for example, alkylammonium salts and alkylbenzylammonium salts, and combinations thereof.

[0038] For the purpose of maintaining the dispersion stability of the obtained surface-treated calcium carbonate and the stability as an oral care composition, the surface treatment agent is preferably a polysaccharide, an anionic surfactant, or a combination thereof, and more preferably sodium polyacrylate, sodium lauryl sulfate, gum arabic, sodium carboxymethylcellulose, or a combination thereof.

[0039] The surface-treated calcium carbonate (A) component is preferably obtained by adding the above-mentioned surface treatment agent and water to a powder when heavy calcium carbonate is used as the calcium carbonate material; or to a calcium carbonate slurry, a water-containing cake obtained by dehydrating the slurry, or a powder obtained by drying and powdering the slurry or dehydrated cake when synthetic calcium carbonate is used as the calcium carbonate material, appropriately adjusting the concentration of calcium carbonate solids, further improving the dispersibility of the particles using a grinder such as a bead mill or a homogenizer, and then drying the mixture.

[0040] The content (amount used) of the surface treatment agent relative to the calcium carbonate is not necessarily limited, as it varies depending on the BET specific surface area of ​​the calcium carbonate and the surfactant used. For example, it is preferably 0.3 to 30 parts by mass, more preferably 0.5 to 15 parts by mass, relative to 100 parts by mass of calcium carbonate. If the content of the surface treatment agent is less than 0.3 parts by mass, the dispersibility of the resulting surface-treated calcium carbonate particles may be insufficient, making it difficult to completely remove pellicles adhering to subtle recesses and gaps in teeth, or scratches and irregularities on the tooth surface. If the content of the surface treatment agent exceeds 30 parts by mass, the resulting surface-treated calcium carbonate particles will have sufficient dispersibility, but excess surface treatment agent may reduce the fluidity of the fluidity-imparting material (B) component, etc., as described below, potentially adversely affecting stability over time. Furthermore, excess surface treatment agent may be disadvantageous in terms of production costs.

[0041] In the present invention, the surface-treated calcium carbonate (A) preferably satisfies the following formula (a): (a) 0.1≦As≦5 (mg / m ２) (where As is the amount of heat source (mg / g) of the component (A) at 200 to 500°C (N １ ) and BET specific surface area (m ２ / g) (B １ ) and the ratio (N １ / B １ )).

[0042] In formula (a), As is 0.1 mg / m ２ If As is less than 5 mg / m, it may be difficult to form a sufficient coating film that covers the entire surface of the calcium carbonate particles. ２ If the amount of the surface treatment agent exceeds this range, it is possible to form a sufficient coating film that covers the entire surface of the calcium carbonate particles, but the excess surface treatment agent may not only deteriorate the stability and stability over time of the resulting oral care composition, but may also be disadvantageous in terms of production costs.

[0043] In formula (a), As is more preferably 0.2 to 3.5 mg / m ２ and even more preferably 0.3 to 2.0 mg / m ２ is.

[0044] The above As can be measured, for example, using a thermogravimetric and differential thermal analysis (TG-DTA) device (DTG-60A; manufactured by Shimadzu Corporation) under the following conditions, and calculated together with the value of the BET specific surface area.

[0045] <Measurement method> Using a simultaneous differential thermal and thermogravimetric (TG-DTA) device (DTG-60A; manufactured by Shimadzu Corporation), approximately 30 mg of a sample (surface-treated calcium carbonate particles; component (A)) was placed in a platinum cell, and the heat loss was measured from 200 to 500°C at a temperature increase rate of 15°C / min to determine the heat loss (mg / g; TG) of the surface-treated calcium carbonate particles. This value was used as the BET specific surface area (m ２ / g), As can be calculated.

[0046] In the present invention, the surface-treated calcium carbonate component (A) preferably also independently satisfies the following formula (b) and formula (c): (b) 0.05≦Dx50≦5 (μm) (c) 0.1≦Dx100≦100 (μm) (where Dx50 is the median diameter (μm) of the component (A) measured with a laser diffraction particle size analyzer, and Dx100 is the maximum diameter (μm) of the component (A) measured with a laser diffraction particle size analyzer).

[0047] In formula (b), the median diameter (Dx50) is an index for determining the dispersion state of the surface-treated calcium carbonate (A) component, and is an actual value measured by laser diffraction particle size distribution. If Dx50 is less than 0.05 μm, the dispersion stability, stability over time, or dispersibility of the surface-treated calcium carbonate may be insufficient, and additional procedures (e.g., the use of a large amount of surface treatment agent) may be required to improve these properties, which may increase the production cost of the resulting preparation. If Dx50 is more than 5 μm, the surface-treated calcium carbonate particles may be too large, making it difficult to completely remove the pellicle covering the tooth surface, even if it can be partially removed.

[0048] In formula (b), Dx50 is more preferably 0.07 to 3 μm, and even more preferably 0.10 to 2 μm.

[0049] In formula (c), the maximum particle size (Dx100) is an index for determining the state of coarse particle size of the surface-treated calcium carbonate (A) component, and is an actual measured value by laser diffraction particle size distribution. If Dx100 is less than 0.1 μm, it may be difficult to maintain the stability over time and dispersion stability of the surface-treated calcium carbonate. If Dx100 is more than 100 μm, the particles of the surface-treated calcium carbonate may be too large, and even if the pellicle covering the tooth surface can be partially removed, it may be difficult to completely remove it.

[0050] In formula (c), Dx100 is more preferably 1 to 50 μm, and even more preferably 2 to 25 μm.

[0051] The Dx50 and Dx100 can be obtained by measuring the laser diffraction particle size distribution under the following conditions using, for example, a laser diffraction particle size distribution analyzer (Microtrac MT-3300EXII; manufactured by Microtrac Bell Co., Ltd.).

[0052] <Measurement conditions for laser diffraction particle size distribution> As a pretreatment for measurement, approximately 0.3 g of a sample (surface-treated calcium carbonate particles) is suspended in 50 ml of water in a beaker (100 ml), and ultrasonic waves are applied for 1 minute at 300 μA using, for example, a tip-type ultrasonic disperser (Ultrasonic Homogenizer US-300T; manufactured by Nippon Seiki Seisakusho Co., Ltd.), and the sample is then measured using a laser diffraction particle size distribution analyzer (Microtrac MT-3300EXII; manufactured by Microtrac-Bell Co., Ltd.), thereby obtaining a laser diffraction particle size distribution. The Dx50 and Dx100 can then be calculated from the obtained distribution curve.

[0053] The content of the surface-treated calcium carbonate (A) component in the oral care composition of the present invention is preferably 20 to 70% by mass, more preferably 35 to 65% by mass, and even more preferably 40 to 60% by mass, based on the total mass of the composition. If the content of component (A) is less than 20% by mass, the amount of component (A) in the composition will be too small, making it difficult to fully exert the pellicle-removing effect in the oral cavity. The greater the content of component (A), the greater the pellicle-removing effect of the resulting composition in the oral cavity. However, if the content exceeds 70% by mass, the amount of component (A) will be too high, making it difficult to maintain the stability of the resulting composition, and the uniform polishing of the tooth surface or the ease of application to the tooth surface may be impaired.

[0054] (Fluidity-imparting material (B) component) The fluidity-imparting material (B) component can function, for example, to provide appropriate fluidity to the oral care composition of the present invention and to improve the dispersibility of the surface-treated calcium carbonate (A) component in the composition. The fluidity-imparting material (B) component also preferably contains an aqueous material, because it can improve the powdery feeling and astringency after tooth brushing and / or improve the mouthfeel (e.g., the dispersibility of the formulation during brushing) and prevent deterioration in the appearance of the resulting oral care composition.

[0055] From this viewpoint, examples of the fluidity-imparting material (B) component include water, wetting agents, thickening agents, binders, and other solvents (other than water), as well as combinations thereof.

[0056] The water that can be used as the fluidity-imparting material (B) component may be any of purified water, pure water, ion-exchanged water, distilled water, RO water, and tap water.

[0057] The humectant and thickener may be the same or different, and each may be composed of at least two materials. Specific examples of humectants and thickeners include sugar alcohols such as sorbitol, maltitol, lactitol, xylitol, and reduced starch saccharification products, glycerin, diglycerin, polyglycerin, 1,3-butylene glycol, polyethylene glycol, 1,2-pentanediol, 1,3-hexanediol, propylene glycol, dipropylene glycol, isopropylene glycol, polypropylene glycol, ethylene glycol, diethylene glycol, and triethylene glycol, and combinations thereof.

[0058] Examples of the binder include carrageenan (ι, λ, κ), alginic acid, sodium alginate, propylene glycol alginate, calcium-containing sodium alginate, potassium alginate, calcium alginate, ammonium alginate, and other alginates and their derivatives, xanthan gum, guar gum, agar, sodium carboxymethylcellulose, hydroxyethylcellulose, and sodium polyacrylate, as well as combinations thereof. The binder may be composed of at least two materials.

[0059] Examples of the other solvent include organic solvents such as ethanol, propyl alcohol, isopropyl alcohol, etc. The other solvent may be composed of at least two materials.

[0060] The content of the fluidity-imparting material (B) component is not particularly limited, but is preferably 30% to 80% by mass, more preferably 35% to 65% by mass, and even more preferably 40% to 60% by mass, relative to the total mass of the oral care composition, in order to maintain the pH of the entire oral care composition within a predetermined range, as described below. If the water content in the oral care composition is less than 30% by mass, the fluidity of the resulting composition may decrease. If the water content exceeds 80% by mass, the fluidity of the resulting composition may become too high, resulting in reduced adhesion of the composition to teeth and reduced pellicle removal effectiveness.

[0061] In the oral care composition of the present invention, the mass ratio of the surface-treated calcium carbonate component (A) to the fluidity-imparting material component (B) (component (A) / component (B)) is preferably 0.3 to 2.0, more preferably 0.5 to 1.8, and even more preferably 0.6 to 1.5. If the mass ratio of component (A) to component (B) is less than 0.3, the relative content of component (A) will be low, and the resulting composition may have difficulty in satisfactorily exhibiting its pellicle-removing effect in the oral cavity. If the mass ratio of component (A) to component (B) is greater than 2.0, the relative content of component (A) or component (A) to component (C) will be high, and the resulting composition may be difficult to maintain stability, and the uniform polishing of tooth surfaces or the ease of application to tooth surfaces may be impaired.

[0062] (pH of Oral Care Composition) In the present invention, the pH of the test solution obtained by adding 10 parts by mass of purified water to 100 parts by mass of the oral care composition is 8 to 12, preferably 8.5 to 11.5, more preferably 9.0 to 11.2, and even more preferably 9.5 to 11.0. If the pH of the test solution is below 8, the resulting oral care composition will not be effective in removing pellicle. Furthermore, if the pH of the test solution is above 12, alkaline components such as calcium hydroxide may remain in the oral care composition, which may impair the stability over time and the flavor of the composition.

[0063] (Cleaning agent (C) component) When the tooth surface is heavily soiled, it may be difficult to obtain a sufficient pellicle removal effect. This is because plaque forms on the pellicle attached to the tooth surface, making it difficult for the composition to act directly on the pellicle. To remove such plaque, for example, a method of brushing it off by brushing the teeth using physical means such as a toothbrush is used.

[0064] However, if a larger amount of plaque has formed, brushing the teeth using the above physical means may not be sufficient to remove the plaque itself, and it may also be difficult to remove the pellicle that exists underneath the plaque.

[0065] The oral care composition of the present invention may further contain a cleaning agent (C) component, for example, in consideration of the presence of plaque. The cleaning agent (C) component can enhance the plaque removal effect of the oral care composition of the present invention, thereby effectively maintaining the pellicle removal effect of the component (A) in the composition. Furthermore, by including the cleaning agent (C) component in the oral care composition of the present invention, it is possible to predictably reduce the content of the component (A) in the composition, and the oral care composition of the present invention can be produced more efficiently overall, for example, in terms of production costs.

[0066] In the present invention, examples of the cleaning agent (C) component include cleaning agents known in the art. The manufacturer, product type, and grade of the cleaning agent (C) component are not particularly limited. In particular, the cleaning agent (C) component is preferably heavy calcium carbonate, light calcium carbonate, silica, or a combination thereof, because the resulting oral care composition can provide an appropriate pH that is gentle on the user and can prevent wear on the user's teeth during brushing.

[0067] In the present invention, it is preferable that the cleaning agent component (C) also independently satisfy the following formula (d) and formula (e): (d) 0.5≦Dx50≦20 (μm) (e) 5≦Dx100≦100 (μm) (where Dx50 is the median diameter (μm) of the component (C) measured with a laser diffraction particle size analyzer, and Dx100 is the maximum diameter (μm) of the component (C) measured with a laser diffraction particle size analyzer).

[0068] In formula (d), the median diameter (Dx50) is an index for grasping the dispersion state of the cleaning agent (C) component, and is an actual measurement value by laser diffraction particle size distribution. If Dx50 is less than 0.5 μm, it may be difficult to obtain cleaning effect. If Dx50 is more than 20 μm, the particles may be too large, making them feel rough and resulting in a poor mouthfeel.

[0069] Here, to explain in detail the range that can be included in the above formula (d), Dx50 of the cleaning agent component (C) is preferably 0.5 to 20 μm, more preferably 1.0 to 10 μm.

[0070] In formula (e), the maximum particle size (Dx100) is an index for grasping the state of the coarse particle size of the cleaning agent (C) component, and is an actual measurement value by laser diffraction particle size distribution. If Dx100 is less than 1 μm, it may be difficult to obtain the above-mentioned effects of the cleaning agent. If Dx100 is more than 500 μm, the particles of the cleaning agent may be too large, making the particles feel rough and resulting in a poor mouthfeel.

[0071] Here, to explain in detail the range that can be included in the above formula (e), Dx100 of the cleaning agent component (C) is preferably 5 to 100 μm, more preferably 10 to 50 μm.

[0072] The Dx50 and Dx100 can be obtained by measuring the laser diffraction particle size distribution under the following conditions using, for example, a laser diffraction particle size distribution analyzer (Microtrac MT-3300EXII; manufactured by Microtrac Bell Co., Ltd.).

[0073] <Measurement conditions for laser diffraction particle size distribution> As a pretreatment for measurement, about 0.3 g of a sample (cleaning agent component (C)) is added to 50 ml of water and suspended in a beaker (100 ml), and ultrasonic waves are irradiated at 300 μA for 1 minute using, for example, a tip-type ultrasonic disperser (Ultrasonic Homogenizer US-300T; manufactured by Nippon Seiki Seisakusho Co., Ltd.), and the sample is then measured using a laser diffraction particle size distribution analyzer (Microtrac MT-3300EXII; manufactured by Microtrac-Bell Co., Ltd.), thereby obtaining a laser diffraction particle size distribution. Then, the Dx50 and Dx100 can be calculated from the obtained distribution curve.

[0074] When the oral care composition of the present invention contains a cleaning agent (C), the total content of the surface-treated calcium carbonate (A) and the cleaning agent (C) is preferably 20% to 70% by mass, more preferably 30% to 60% by mass, based on the total mass of the composition. If the total content of the (A) and (C) components in the oral care composition is less than 20% by mass, the relative amounts of the (A) and (C) components in the composition will be too small, making it difficult to achieve both pellicle and plaque removal effects in the oral cavity using the resulting composition. If the total content of the (A) and (C) components in the oral care composition is more than 70% by mass, the relative amounts of the (A) and (C) components in the composition will be too large, making it difficult to maintain the stability of the resulting composition, and the uniform polishing of tooth surfaces or the ease of application to the tooth surfaces may be impaired.

[0075] When the oral care composition of the present invention contains a cleaning agent (C), the content of the surface-treated calcium carbonate (A) contained in the oral care composition is preferably 5% by mass to 60% by mass, and more preferably 20% by mass to 50% by mass, based on the total mass of the composition. When the cleaning agent (C) is contained, if the content of the (A) component is less than 5% by mass, the amount of the (A) component in the composition will be too small, and it may be difficult to fully exert the pellicle-removing effect in the oral cavity. When the cleaning agent (C) is contained, the greater the content of the (A) component, the greater the pellicle-removing effect of the resulting composition in the oral cavity. However, when the content of the (A) component in the cleaning agent (C) is contained, if the content of the (A) component exceeds 60% by mass, the content of the (A) component will be too high, and the relative amount of the (C) component in the composition will be small, and it may be difficult to fully exert the cleaning effect in the oral cavity.

[0076] When the oral care composition of the present invention contains a cleaning agent (C), the content of the component (C) is preferably 10% by mass to 65% by mass, and more preferably 20% by mass to 50% by mass, based on the total mass of the composition. If the content of the component (C) is less than 10% by mass, the content of the component (C) in the composition will be too low, and it may be difficult to fully exert its cleaning effect in the oral cavity. The higher the content of the component (C), the greater the cleaning effect of the resulting composition. However, if the content of the component (C) exceeds 60% by mass, the content of the component (C) will be too high, and the relative amount of the component (A) in the composition will be low, and it may be difficult to fully exert its pellicle removal effect in the oral cavity.

[0077] (Optional Components) The oral care composition of the present invention may also contain optional components other than the above-mentioned components, provided that the effects of the present invention are not impaired.

[0078] Optional ingredients include, for example, abrasives, medicinal ingredients, flavorings, sweeteners, foaming agents, preservatives, pH adjusters, coloring agents (pigments), and resins, and combinations thereof.

[0079] Examples of abrasives include calcium carbonate (e.g., heavy calcium carbonate and light calcium carbonate), sodium bicarbonate, calcium phosphate, dibasic calcium phosphate, calcium pyrophosphate, insoluble calcium metaphosphate, silica, hydrous silicic acid, anhydrous silicic acid, titanium dioxide, amorphous silica, crystalline silica, aluminosilicate, aluminum oxide, aluminum hydroxide, and resin, as well as combinations thereof. The content of the abrasive can be appropriately determined to an effective amount according to conventional methods.

[0080] Examples of medicinal ingredients include bactericidal or antibacterial agents such as cetylpyridinium chloride, benzalkonium chloride, benzethonium chloride, isopropylmethylphenol, polyethylene glycol, zinc gluconate, zinc citrate, triclosan, thymol, hinokitiol, and lysozyme chloride; enzymes such as dextranase, mutanase, amylase, protease, and Liteque Enzyme; fluorides such as sodium fluoride, sodium monofluorophosphate, and stannous fluoride; ε-aminocaproic acid, allantoin, tranexamic acid, glycyrrhizinate (e.g., dipotassium glycyrrhizinate), glycyrrhetinic acid, glycyrrhetinate (e.g., stearyl glycyrrhetinate), azulene, allantoin chlorohydroxyaluminum, and dihydrocholesterol. Examples of suitable medicinal ingredients include anti-inflammatory agents such as sterols, metal salts such as zinc, copper salts, and tin salts, anti-tartar agents such as condensed phosphates and ethanehydroxydiphosphonate, blood flow promoters such as vitamin E (e.g., tocopherol acetate), anti-dentin hypersensitivity agents such as potassium nitrate, aluminum lactate, and strontium chloride, coating agents such as hydroxyethylcellulose dimethyldiallylammonium chloride, astringents such as vitamin C (e.g., ascorbic acid or its salts), and lysozyme chloride, water-soluble copper compounds such as copper chlorophyll and copper gluconate, anti-tartar agents, amino acids such as alanine, glycine, proline, and pyrrolidonecarboxylic acid (salts), plant extracts such as Phellodendron bark, thyme, Scutellaria root, clove, and witch hazel, callopeptide, and polyvinylpyrrolidone. The content of the medicinal ingredients can be appropriately determined to an effective amount according to conventional methods.

[0081] Examples of fragrances include peppermint oil, spearmint oil, 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, orange oil, lime oil, yuzu oil, nutmeg oil, lavender oil, paracles oil, vanilla oil, cinnamon oil, pimento oil, Natural essential oils such as cinnamon leaf oil, perilla oil, and wintergreen oil; fragrance components contained in the above natural essential oils such as menthol, carvone, cinnamic 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, cineole, ethyl linalool, and vanillin; ethyl a Fragrance ingredients such as acetate, ethyl butyrate, isoamyl acetate, hexanal, hexenal, methyl anthranilate, ethyl methylphenyl glycidate, benzaldehyde, vanillin, ethyl vanillin, and furaneol; N-ethyl-p-menthane-3-carboxamide, menthyl lactate, menthyl monosuccinate, isopulegol, menthone glycerol ketal, N-(4-cyanomethylphenyl)-p-menthanecarboxamide, and 3-l-menthoxypropane-1,2-diol , 5-methyl-2-propan-2-yl-N-(2-pyridin-2-ylethyl)cyclohexane-1-carboxamide, ethyl 3-(p-menthane-3carboxamide)acetate, 2-isopropyl-N,2,3-trimethylbutyramide, (1R,2S,5R)-N-(4-(cyanomethyl)phenyl)menthylcarboxamide, and other cooling sensation agents, as well as various blended flavors such as mint, fruit, and herb flavors that are obtained by combining several flavoring ingredients and natural essential oils, and combinations thereof. The content of the flavoring can be appropriately determined to an effective amount according to conventional methods.

[0082] Examples of sweeteners include saccharin, saccharin sodium, aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidin dihydrochalcone, perillartine, glycyrrhizin, thaumatin, and aspartylphenylalanine methyl ester, and combinations thereof. The content of the sweetener can be appropriately determined to an effective amount according to conventional methods.

[0083] Examples of foaming agents include hydrocarbons such as squalane, liquid paraffin, petrolatum, and microcrystalline wax, higher alcohols (e.g., alcohols having 8 to 22 carbon atoms such as lauryl alcohol, cetyl alcohol, cetostearyl alcohol, oleyl alcohol, and isostearyl alcohol), higher fatty acids (e.g., fatty acids having 8 to 22 carbon atoms such as lauric acid, myristic acid, oleic acid, and isostearic acid), vegetable oils such as olive oil, castor oil, and coconut oil, and fatty acid esters such as isopropyl myristate, as well as combinations thereof. The content of the oily component can be appropriately determined to an effective amount according to conventional methods.

[0084] Examples of preservatives include parahydroxybenzoates (e.g., methyl parahydroxybenzoate, ethyl parahydroxybenzoate, butyl parahydroxybenzoate), benzoates (e.g., sodium benzoate), and combinations thereof. The content of the preservatives can be appropriately determined to an effective amount according to conventional methods.

[0085] Examples of pH adjusters include organic acids such as phthalic acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid, and lactic acid, or their salts (sodium citrate), inorganic acids such as phosphoric acid (orthophosphoric acid), or their salts (e.g., potassium salts, sodium salts, and ammonium salts), and hydroxides such as sodium hydroxide and potassium hydroxide, as well as combinations thereof. The content of the pH adjuster can be appropriately determined to an effective amount according to conventional methods.

[0086] Examples of coloring agents include natural dyes such as safflower red, gardenia yellow, gardenia blue, perilla color, red koji color, red cabbage color, carrot color, hibiscus color, cacao color, spirulina blue, and tamarind color, legally designated dyes 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, titanium dioxide, and combinations thereof. The content of the coloring agent can be appropriately determined to an effective amount according to conventional methods.

[0087] Examples of resins include polyisobutylene, polybutadiene, urethane, silicone, and natural rubber, and combinations thereof. The content of the resin can be appropriately determined to an effective amount according to a conventional method.

[0088] (Dosage form of oral care composition) The oral care composition of the present invention can be appropriately selected depending on the form of use and is not particularly limited. The dosage form can be, for example, a paste, a liquid, or the like, and specifically can be an oral preparation such as a dentifrice, a mouthwash, a liniment, or an oral dissolving agent. Dentifrices (e.g., toothpaste, liquid dentifrice, liquid dentifrice, lubricant toothpaste) and mouthwashes are preferred because of their versatility.

[0089] 2. Method for Producing Oral Care Composition The oral care composition of the present invention can be prepared using any means known in the art depending on the formulation.

[0090] For example, when producing toothpaste, the water-soluble components constituting the fluidity-imparting material (B) are first added and dissolved, and then the other water-insoluble components are mixed in, followed by degassing (e.g., by reducing pressure) as necessary. The resulting toothpaste can be placed in a predetermined container to produce a finished product. The shape and material of the container are not particularly limited, and containers commonly used for ordinary toothpaste compositions can be used, including, for example, laminated tubes made of plastics such as polyethylene, polypropylene, polyethylene terephthalate, and nylon.

[0091] 3. Method for Removing Pellicle in the Oral Cavity Using the oral care composition of the present invention, pellicle in the oral cavity can be removed as follows.

[0092] For example, the oral care composition of the present invention processed into the form of the oral preparation described above is applied to the oral cavity (including, for example, the oral cavity, tooth surfaces, and between teeth) of a human and / or non-human mammal. Such application can be carried out, for example, by brushing, spraying, applying, rinsing, or a combination thereof. The oral care composition applied in this manner can remove pellicles that have adhered to and formed on tooth surfaces and between teeth, and / or can effectively remove pellicles from the oral cavity.

[0093] The oral care composition of the present invention can be used at the same frequency as normal tooth brushing. The oral care composition of the present invention can be used, for example, three times a day, at intervals of, for example, 3 hours or more, preferably 5 hours or more, more preferably 8 hours or more. For example, when the oral care composition of the present invention is used before going to bed, the pellicle removal effect can be maintained throughout the sleep period (for example, 8 hours or more).

[0094] It should be noted that pellicle removal using the oral care composition of the present invention can also be applied to pellicles formed in vitro.

[0095] The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples. In the following description, % means % by mass and parts means parts by mass unless otherwise specified.

[0096] The oral care compositions obtained in Examples 1 to 23 and Comparative Examples 1 to 6 described below were evaluated in the following (1) to (5).

[0097] (1) Measurement of characteristic values ​​The BET specific surface area, thermal loss (TG), and As (thermal loss (mg / g) (N) of the prepared surface-treated calcium carbonate particles (A) components-1 to 16) were measured. １ ) and BET specific surface area (m ２ / g) (B １ ) and the ratio (N １ / B １)), median diameter (Dx50), and maximum diameter (Dx100) were measured or calculated using the above-mentioned measuring device and measuring method.

[0098] (2) Evaluation of pellicle removal effect A pellicle-like composition (nitrogen compound) was artificially prepared according to the following procedure, and the presence or absence of nitrogen (N) contained in the protein, which is its main component, was used as an indicator element by X-ray photoelectron spectroscopy (XPS).

[0099] (2-1) Preparation of "pellicle-like composition (nitrogen compound)" 0.125 g of mucin, a glycoprotein that is the main component of salivary mucus, and 0.125 g of proline (L-proline), an amino acid that is the main component of pellicle, were added to 100 mL of ultrapure water to prepare an aqueous solution of "pellicle-like composition (nitrogen compound)" as a test liquid.

[0100] (2-2) Preparation of "Test Tooth Specimens (Nitrogen Compound (Protein)-Removed Tooth Specimens)" The tooth specimens were polished with prophy paste (four types: blue, green, pink, and yellow) and thoroughly rinsed with water until the paste was removed. The polished tooth specimens were then immersed in an aqueous NaOH solution (concentration: 1.0% by mass) and ultrasonically cleaned for 30 minutes. Furthermore, instead of the aqueous NaOH solution, they were ultrasonically cleaned in tap water for 30 minutes. They were then dried in a constant temperature bath at 37°C for 24 hours and cut to lengths of 5 mm or less using a diamond cutting system to prepare test tooth specimens.

[0101] (2-3) Confirmation of removal of "pellicle-like composition (nitrogen compound)" The aqueous solution of "pellicle-like composition (nitrogen compound)" prepared in (2-1) above was heated to a temperature of 37°C, and the test tooth specimen prepared in (2-2) above was immersed in this for 90 minutes, allowing the pellicle-like composition (nitrogen compound) to adhere sufficiently to the tooth specimen. An appropriate amount of the oral care composition prepared in the following Examples or Comparative Examples was then applied to the tooth specimen, allowed to stand for 5 minutes, and then rinsed with purified water until the paste on the surface was removed (approximately 3 seconds). Test specimens were then obtained by drying in a constant temperature dryer at 50°C for 60 minutes. Five such test specimens were prepared for each Example and Comparative Example.

[0102] (2-4) Evaluation of Test Specimens The test specimens obtained in (2-3) above were measured for the presence (intensity) of nitrogen (N) remaining in the test specimens using an X-ray photoelectron spectrometer (PHI X-tool manufactured by ULVAC-PHI, Inc.) (XPS device). The obtained nitrogen (N) intensities were classified into the scores shown in Table 1, the average score of the obtained test specimens was calculated, and the results were further classified according to the following evaluation criteria.

[0103]

[0104] (Evaluation criteria for pellicle removal) A: Average value of 4.5 points or more and 5.0 points or less B: Average value of 3.0 points or more and less than 4.5 points C: Average value of 1.5 points or more and less than 3.0 points D: Average value less than 1.5 points

[0105] (3) Evaluation of Appearance and Workability of Preparations The appearance of each of the oral care compositions (number of samples: 5) obtained in the Examples and Comparative Examples was visually observed and evaluated according to the criteria shown in Table 2. The average score obtained was calculated, and the results were further classified according to the following evaluation criteria.

[0106]

[0107] (Evaluation criteria for appearance and workability of formulations) A: Average value of 3.5 points or more and 4.0 points or less B: Average value of 2.5 points or more and less than 3.5 points C: Average value of 1.5 points or more and less than 2.5 points D: Average value of 1.0 points or more and less than 1.5 points

[0108] (4) Formulation Stability Five samples were prepared by filling 20 g of the prepared oral care composition into laminated tubes and storing them for one month at 40° C. Thereafter, the oral care composition in the tube was returned to room temperature and placed on a toothbrush, and its appearance was observed and evaluated according to the criteria shown in Table 3. The obtained scores were averaged and the results were further classified according to the following evaluation criteria.

[0109]

[0110] (Evaluation criteria for formulation stability) A: Average value of 3.5 to 4.0 points B: Average value of 2.5 to less than 3.5 points C: Average value of 1.5 to less than 2.5 points D: Average value of 1.0 to less than 1.5 points

[0111] (5) Experience of using oral care compositions Five subjects used the oral care compositions obtained in the Examples and Comparative Examples for tooth brushing, and evaluated the experience of using them according to the criteria shown in Table 4. The average score obtained was calculated, and the results were further classified according to the following evaluation criteria.

[0112] Each subject brushed their teeth by applying approximately 1 g of the oral care composition to a toothbrush and brushing for 3 minutes.

[0113]

[0114] (Evaluation criteria for usability) A: Average value of 3.5 points or more and 4.0 points or less B: Average value of 2.5 points or more and less than 3.5 C: Average value of 1.5 points or more and less than 2.5 D: Average value of 1.0 points or more and less than 1.5

[0115] Reference Example 1: Preparation of surface-treated calcium carbonate particles (Component (A)-1) White crystalline limestone was coarsely and mediumly pulverized to prepare a finely pulverized raw material, which was then finely pulverized using a Super Hybrid Mill (manufactured by Ishikawajima-Harima Heavy Industries Co., Ltd.). This finely pulverized material was classified, and the resulting product was classified several times to obtain heavy calcium carbonate. Five parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) was added as a surface treatment agent to 100 parts by mass of the resulting heavy calcium carbonate. Water was then added to the mixture to prepare a calcium carbonate solution with a 40% solids content, which was then mixed and stirred. The resulting solution was then wet-pulverized using a wet mill (DYNO-MILL KD model; manufactured by Weily & Bachofen GmbH (WAB)) and dried using a spray dryer (manufactured by Okawara Kakoki Co., Ltd.) to obtain a calcium carbonate solution with a BET specific surface area of ​​3.5 m. ２ / g of component (A)-1 was obtained. The powder values ​​of the obtained component (A)-1 are shown in Table 5.

[0116] Reference Example 2: Preparation of surface-treated calcium carbonate particles (component (A)-2) Gray dense limestone was fired in a fluidized-tank kiln using kerosene as a heat source, and the resulting quicklime was dissolved to form slaked lime slurry, which was then reacted with carbon dioxide to synthesize calcium carbonate. This calcium carbonate was suspended in water to obtain a suspension, and after removing foreign matter and coarse particles using a sieve (400 mesh), the calcium carbonate aqueous suspension was subjected to particle growth by Ostwald aging for 60 hours, followed by dehydration using a filter press, drying, and crushing to obtain calcium carbonate particles.

[0117] Next, 5 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) was added as a surface treatment agent to 100 parts by mass of the calcium carbonate particles, and water was added to prepare a calcium carbonate solution with a solid content of 40%, which was then mixed and stirred. Thereafter, the solution was wet-pulverized using a wet pulverizer (DYNO-MILL KD type; manufactured by Weily & Bachofen GmbH (WAB GmbH)) and dried using a spray dryer (manufactured by Okawara Kakoki Co., Ltd.) to obtain a solution with a BET specific surface area of ​​7.0 m. ２ / g of component (A)-2 was obtained. The powder values ​​of the obtained component (A)-2 are shown in Table 5.

[0118] Reference Example 3: Preparation of surface-treated calcium carbonate particles (component (A)-3) The Ostwald ripening time was shortened to 12 hours to allow the particles to grow, and the particles were dehydrated using a filter press. The resulting calcium carbonate dehydrated cake with a solid content of 65% by mass was used. The same procedure as in Reference Example 2 was repeated to prepare surface-treated calcium carbonate particles having a BET specific surface area of ​​15.0 m. ２ / g of component (A)-3 was obtained. The powder values ​​of the obtained component (A)-3 are shown in Table 5.

[0119] Reference Example 4: Preparation of surface-treated calcium carbonate particles (component (A)-4) A surface-treated calcium carbonate particle having a BET specific surface area of ​​24.0 m was prepared in the same manner as in Reference Example 2, except that the Ostwald ripening time was shortened to 3 hours. ２ The powder values ​​of the obtained component (A)-4 are shown in Table 5.

[0120] Reference Example 5: Preparation of surface-treated calcium carbonate particles (component (A)-5) When calcium carbonate was synthesized by reacting slaked lime slurry with carbon dioxide gas by the method described in Reference Example 2, calcium carbonate was synthesized by adding citric acid in an amount of 1.0% relative to calcium hydroxide, and then the resulting mixture was concentrated using a rotary filter to obtain a calcium carbonate slurry.

[0121] Next, a calcium carbonate slurry having a BET specific surface area of ​​41.0 m was prepared in the same manner as in Reference Example 2, except that 5 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) was added as a surface treatment agent relative to 100 parts by mass of the calcium carbonate solid content contained in the calcium carbonate slurry. ２ / g of component (A)-5 was obtained. The powder values ​​of the obtained component (A)-5 are shown in Table 5.

[0122] Reference Example 6: Preparation of surface-treated calcium carbonate particles (component (A)-6)) A calcium carbonate slurry was obtained in the same manner as in Reference Example 4, and a calcium carbonate slurry having a BET specific surface area of ​​24.0 m was prepared in the same manner as in Reference Example 4, except that the surface treatment agent was changed to sodium lauryl sulfate (manufactured by Kao Corporation). ２ / g of component (A)-6 was obtained. The powder values ​​of the obtained component (A)-6 are shown in Table 6.

[0123] Reference Example 7: Preparation of surface-treated calcium carbonate particles (component (A)-7)) Calcium carbonate was obtained in the same manner as in Reference Example 7, and a BET specific surface area of ​​27.0 m was obtained in the same manner as in Reference Example 4, except that the surface treatment agent was changed to a sucrose fatty acid ester (manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.). ２ / g of component (A)-7 was obtained. The powder values ​​of the obtained component (A)-7 are shown in Table 6.

[0124] Reference Example 8: Preparation of surface-treated calcium carbonate particles (component (A)-8)) Calcium carbonate was obtained in the same manner as in Reference Example 4, and a BET specific surface area of ​​27.0 m was obtained in the same manner as in Reference Example 4, except that the surface treatment agent was changed to sodium carboxymethyl cellulose (manufactured by Nippon Paper Industries Co., Ltd.). ２ / g of component (A)-8 was obtained. The powder values ​​of the obtained component (A)-8 are shown in Table 6.

[0125] Reference Example 9: Preparation of surface-treated calcium carbonate particles (Component (A)-9)) Calcium carbonate was obtained in the same manner as in Reference Example 4, and a BET specific surface area of ​​26.0 m was obtained in the same manner as in Reference Example 4, except that the surface treatment agent was changed to gum arabic (manufactured by Sumitomo Pharma Food & Chemical Co., Ltd.). ２ / g of component (A)-9 was obtained. The powder values ​​of the obtained component (A)-9 are shown in Table 6.

[0126] Reference Example 10: Preparation of surface-treated calcium carbonate particles (component (A)-10)) A calcium carbonate particle having a BET specific surface area of ​​28.0 m was prepared in the same manner as in Reference Example 4, except that 1 part by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) was added as a surface treatment agent to 100 parts by mass of calcium carbonate obtained in the same manner as in Reference Example 4. ２ / g of component (A)-10 was obtained. The powder values ​​of the obtained component (A)-10 are shown in Table 6.

[0127] Reference Example 11: Preparation of surface-treated calcium carbonate particles (Component (A)-11) A calcium carbonate particle having a BET specific surface area of ​​26.0 m was prepared in the same manner as in Reference Example 4, except that 3 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) as a surface treatment agent was added to 100 parts by mass of calcium carbonate obtained in the same manner as in Reference Example 4. ２ / g of component (A)-11 was obtained. The powder values ​​of the obtained component (A)-11 are shown in Table 7.

[0128] Reference Example 12: Preparation of surface-treated calcium carbonate particles (Component (A)-12) A calcium carbonate particle having a BET specific surface area of ​​21.0 m was prepared in the same manner as in Reference Example 4, except that 10 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) as a surface treatment agent was added to 100 parts by mass of calcium carbonate obtained in the same manner as in Reference Example 4. ２ / g of component (A)-12 was obtained. The powder values ​​of the obtained component (A)-12 are shown in Table 7.

[0129] Reference Example 13: Preparation of surface-treated calcium carbonate particles (Component (A)-13) A calcium carbonate particle having a BET specific surface area of ​​18.0 m was prepared in the same manner as in Reference Example 4, except that 15 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) as a surface treatment agent was added to 100 parts by mass of calcium carbonate obtained in the same manner as in Reference Example 4.２ / g of component (A)-13 was obtained. The powder values ​​of the obtained component (A)-13 are shown in Table 7.

[0130] Reference Example 14: Preparation of surface-treated calcium carbonate particles (Component (A)-14) The finely pulverized product was classified once to obtain heavy calcium carbonate (100 parts by mass). The same procedure as in Example 1 was repeated except that 1 part by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) was added as a surface treatment agent to produce surface-treated calcium carbonate particles having a BET specific surface area of ​​1.0 m. ２ / g of component (A) was obtained. The powder values ​​of the obtained component (A)-14 are shown in Table 7.

[0131] Reference Example 15: Preparation of surface-treated calcium carbonate particles (component (A)-15)) Calcium carbonate was obtained in the same manner as in Reference Example 4, and a BET specific surface area of ​​30.0 m was obtained in the same manner as in Reference Example 4, except that no surface treatment agent was added. ２ / g of component (A)-15 was obtained. The powder values ​​of the obtained component (A)-15 are shown in Table 7.

[0132] Reference Example 16: Preparation of surface-treated calcium carbonate particles (component (A)-16)) In the same manner as in Reference Example 2, calcium carbonate was synthesized by reacting a slaked lime slurry with carbon dioxide gas, and citric acid was added in an amount of 1.5% relative to calcium hydroxide to synthesize calcium carbonate, and the resulting mixture was concentrated using a rotary filter to obtain a calcium carbonate slurry.

[0133] Next, a calcium carbonate slurry having a BET specific surface area of ​​51.0 m was prepared in the same manner as in Example 2, except that 10 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.) was added as a surface treatment agent relative to 100 parts by mass of the calcium carbonate solid content contained in the calcium carbonate slurry. ２ / g of component (A)-16 was obtained. The powder values ​​of the obtained component (A)-16 are shown in Table 7.

[0134]

[0135]

[0136]

[0137] (Examples 1 to 13 and Comparative Examples 1 to 3: Preparation and Evaluation of Oral Care Compositions) 45.5 parts by mass of the surface-treated calcium carbonate (A) components-1 to 11 and 14 to 16 obtained in Reference Examples 1 to 11 and 54.5 parts by mass of the fluidity-imparting material (B) component were blended, mixed and stirred to obtain oral care compositions.

[0138] The details of component (B) were 26.0 parts by mass of glycerin, 2.5 parts by mass of polyethylene glycol, 1.0 part by mass of sodium carboxymethylcellulose, and 25.0 parts by mass of purified water. 10 parts by mass of purified water was added to 100 parts by mass of the obtained oral care composition and gently stirred to prepare a test solution, and the pH of this test solution was measured using a pH meter (D-210P, manufactured by Horiba, Ltd.).

[0139] The properties and evaluation results of the obtained oral care compositions are shown in Tables 8 to 10 and Table 14.

[0140] (Examples 14 to 17 and Comparative Examples 4 and 5: Preparation and Evaluation of Oral Care Compositions) Oral care compositions were obtained by adjusting the pH of the oral care composition obtained in Example 4 by adding citric acid or sodium hydroxide as appropriate. The property values ​​and evaluation results of the obtained oral care compositions are shown in Tables 11 and 14.

[0141] (Examples 18 to 23: Preparation and evaluation of oral care compositions) Oral care compositions with different mass ratios of component (A) / component (B) were obtained in the same manner as in Example 1, except that the surface-treated calcium carbonate particles (component (A)-4) obtained in Reference Example 4 were used and each constituent of component (B) of the fluidity-imparting material was changed as shown in Table 12. The property values ​​and evaluation results of the obtained oral care compositions are shown in Table 12.

[0142] (Examples 24 to 27: Preparation and evaluation of oral care compositions) Oral care compositions were obtained in the same manner as in Example 1, except that the surface-treated calcium carbonate particles ((A)-4) obtained in Reference Example 4 were used and each constituent of the fluidity-imparting material (B) was changed as shown in Table 13. The property values ​​and evaluation results of the obtained oral care compositions are shown in Table 13.

[0143] Comparative Example 6: Preparation and evaluation of oral care composition An oral care composition was obtained by adding 5 parts by mass of sodium polyacrylate (manufactured by Toagosei Co., Ltd.), which was used as a surface treatment agent, to 100 parts by mass of the calcium carbonate solids of the oral care composition obtained in Comparative Example 2. The property values ​​and evaluation results of the obtained oral care composition are shown in Table 14.

[0144]

[0145]

[0146]

[0147]

[0148]

[0149]

[0150]

[0151] As shown in Tables 8 to 14, the oral care compositions prepared in Examples 1 to 27 were able to effectively remove pellicles compared to those prepared in Comparative Examples 1 to 5, and were excellent in terms of appearance and workability of the formulation, formulation stability, and usability.

[0152] As shown in Tables 8 to 14, the oral care compositions prepared in Examples 1 to 27 were able to effectively remove pellicles compared to those prepared in Comparative Examples 1 to 5, and were excellent in terms of appearance and workability of the formulation, formulation stability, and usability.

[0153] Next, the oral care compositions obtained in Examples 4 (reevaluation) and 24 to 32, and Comparative Example 7, which will be described later, were evaluated in the above items (1) to (5) as well as the following item (6).

[0154] (6) Evaluation of plaque removal effect Test tooth specimens with artificially attached pellicle-like compositions (nitrogen compounds) and plaque were prepared according to the following procedure, and the degree of removal of discolored plaque was visually confirmed.

[0155] (6-1) Confirmation of Plaque Removal Artificial plaque (manufactured by Nissin Co., Ltd.) was applied to tooth specimens to which the pellicular composition (nitrogen compound) prepared in (2-2) above had been sufficiently attached, to prepare composite test tooth specimens consisting of pseudo-pellicles and artificial plaque. The excess artificial plaque adhering to the tooth specimens was washed away with purified water for 30 seconds, and then a test specimen was obtained by scrubbing the toothbrush (with nylon bristles) 20 times using an appropriate amount of the oral care composition prepared in the following examples at a pressure of approximately 100 to 150 g, followed by washing with purified water for 30 seconds. Five such test specimens were prepared for each example.

[0156] (6-2) Evaluation of Test Pieces The surface area of ​​the test piece obtained in (6-1) above was divided into 16 sections of approximately uniform size, and the number of sections in which the color of artificial plaque had disappeared within the surface area was counted visually, and the plaque removal rate (%) was calculated based on the following formula: Plaque removal rate (%) = (Number of sections in which the color of artificial plaque had disappeared / 16) × 100

[0157] The resulting plaque removal rate (%) was then evaluated according to the standards shown in Table 15, and the average score obtained was calculated, which was then further classified according to the following evaluation method.

[0158]

[0159] (Method for evaluating the average value of the plaque removal rate) A: Average score of 4.0 points or more and 5.0 points or less B: Average score of 3.0 points or more and less than 4.0 points C: Average score of 1.5 points or more and less than 3.0 points D: Average score less than 1.5 points

[0160] (Examples 24 and 25: Preparation and evaluation of oral care compositions) Using the surface-treated calcium carbonate ((A)-4) component obtained in Reference Example 4, a cleaning agent (C) component (heavy calcium carbonate (Calcy F#9860 [manufactured by Sankyo Seifun Co., Ltd.: Dx50=9.0 μm, Dx100=150.0 μm]), and a fluidity imparting agent (B) component, the components were blended as shown in Table 16, and the mixture was mixed and stirred to obtain oral care compositions. The property values ​​and evaluation results of the obtained oral care compositions are shown in Table 16.

[0161] Example 26: Preparation and evaluation of oral care composition The surface-treated calcium carbonate ((A)-4) component obtained in Reference Example 4, the cleaning agent (C) component (heavy calcium carbonate (calcium carbonate special grade #3 [manufactured by Sankyo Seifun Co., Ltd.: Dx50 = 24.8 μm, Dx100 = 125.0 μm]), and the fluidity imparting agent (B) component were blended with each other as shown in Table 16, and the mixture was mixed and stirred to obtain an oral care composition. The property values ​​and evaluation results of the obtained oral care composition are shown in Table 16.

[0162] (Examples 27 to 31: Preparation and evaluation of oral care compositions) Using the surface-treated calcium carbonate ((A)-4) component obtained in Reference Example 4, the cleaning agent (C) component (light calcium carbonate (Calpin F [manufactured by Yabashi Industries Co., Ltd.: Dx50 = 3.0 μm, Dx100 = 18.0 μm]), and the fluidity imparting agent (B) component, the components were blended as shown in Table 16, and mixed and stirred to obtain oral care compositions. The property values ​​and evaluation results of the obtained oral care compositions are shown in Table 16.

[0163] Example 32 Preparation and Evaluation of Oral Care Compositions Using the surface-treated calcium carbonate ((A)-4) component obtained in Reference Example 4, the cleaning agent (C) component (silica (OSC DA95 [manufactured by Oriental Silicas Corporation: Dx50=9.0 μm, Dx100=35.0 μm]), and the fluidity imparting agent (B) component, the components were blended as shown in Table 16, mixed, and stirred to obtain oral care compositions. The property values ​​and evaluation results of the obtained oral care compositions are shown in Table 16.

[0164] (Example 4: Reevaluation of Oral Care Composition) Evaluations, including evaluation of plaque removal effect, were carried out using the oral care composition obtained in Example 4. The property values ​​and evaluation results of the obtained oral care composition are shown in Table 16.

[0165] Comparative Example 7: Preparation and evaluation of oral care composition Without adding the surface-treated calcium carbonate (A), a cleaning agent (C) (light calcium carbonate (Calpin F [manufactured by Yabashi Industries Co., Ltd.: Dx50 = 3.0 µm, Dx100 = 18.0 µm])) and a fluidity imparting agent (B) were used, and the components were blended as shown in Table 16, mixed and stirred to obtain an oral care composition. The property values ​​and evaluation results of the obtained oral care composition are shown in Table 16.

[0166]

[0167] As shown in Table 16, the oral care compositions prepared in Examples 24 to 31 were able to effectively remove both plaque and pellicle compared to the composition prepared in Comparative Example 7. It can also be seen that the compositions of Examples 24 to 31 were excellent in terms of appearance and workability of the formulation, formulation stability, and usability.

[0168] The present invention is useful in technical fields such as the manufacturing of daily commodities and cosmetics, and dental products.

Claims

1. An oral care composition comprising a surface-treated calcium carbonate component (A) and a fluidity-imparting material component (B), The surface treatment calcium carbonate (A) component is 3 to 50 m ２ Particles having a BET specific surface area of ​​ / g and having a coating layer on the surface containing a surface treatment agent, The pH of the test solution obtained by adding 10 parts by mass of purified water to 100 parts by mass of the oral care composition is 8 to 12, and An oral care composition wherein the surface treatment agent is at least one selected from the group consisting of anionic surfactants and polysaccharides.

2. The oral care composition according to claim 1, wherein the surface treatment agent is at least one selected from the group consisting of sodium polyacrylate, sodium lauryl sulfate, gum arabic, and sodium carboxymethylcellulose.

3. The oral care composition according to claim 1 or 2, wherein the component (A) satisfies the following formulas (a), (b), and (c): (a)0.1≦As≦5(mg / m ２ ) (b) 0.05≦Dx50≦5 (μm) (c) 0.1≦Dx100≦100 (μm) As is the loss on heat (mg / g) of component (A) at 200-500°C (N １ ) and BET specific surface area (m ２ / g) (B １ ) ratio (N １ / B １ ) and; Dx50 is the median diameter (μm) of component (A) measured by a laser diffraction particle size distribution analyzer; Dx100 is the maximum diameter (μm) of component (A) measured by a laser diffraction particle size distribution analyzer.

4. The oral care composition according to claim 1, wherein component (B) is at least one selected from the group consisting of water, a wetting agent, a viscosity agent, and a binder.

5. The oral care composition according to claim 1, wherein the content of component (A) is 20 to 70% by mass based on the total mass of the composition.

6. The oral care composition according to claim 1, wherein the mass ratio (component (A) / component (B)) of component (A) to component (B) is 0.3 to 2.

0.

7. The oral care composition according to claim 1, further comprising a cleaning agent (C) component.

8. The oral care composition according to claim 7, wherein the (C) component is at least one selected from the group consisting of heavy calcium carbonate, light calcium carbonate, and silica.

9. The oral care composition according to claim 7, wherein the component (C) satisfies the following formulas (d) and (e): (d) 0.5≦Dx50≦20 (μm) (e) 5≦Dx100≦100 (μm) Dx50 is the median diameter (μm) of the (C) component measured by a laser diffraction particle size distribution analyzer; Dx100 is the maximum diameter (μm) of the (C) component measured by a laser diffraction particle size distribution analyzer.

10. The oral care composition according to claim 7, wherein the total content of component (A) and component (C) is 20 to 70% by mass based on the total mass of the composition, the content of component (A) is 5 to 60% by mass based on the total mass of the composition, and the content of component (C) is 10 to 65% by mass based on the total mass of the composition.

11. An oral care composition according to claim 1 or 7, used for removing pellicle from the oral cavity and tooth surface.