WO2010058522A1 - Method for removing solid product formed on surfaces of teeth - Google Patents

Abstract

Disclosed is a composition which has an excellent whitening effect on teeth and can give a luster to teeth. Also disclosed is a method for removing a solid product formed on the surfaces of teeth, which comprises applying an oral composition to teeth, wherein the oral composition contains 0.05 to 18 mass% of phytic acid or a salt thereof, contains no polyvalent cation or contains a polyvalent cation in an amount of less than 0.1-fold mole relative to the content of phytic acid, and wherein a diluted solution of the oral composition in water at a concentration of 30 mass% has a pH value of 5.5 to 6.5.

Description

Method for removing solid product formed on tooth surface

The present invention relates to a method for improving the gloss of a tooth by removing a solid product generated on a tooth surface.

The cause of coloration of human teeth is mainly caused by adhesion of various colored substances to tartar, plaque and the surface. Various physical or chemical methods have been reported as means for removing the cause of coloring of the tooth surface. As a physical method, in addition to polishing removal, n-butyl ether, butyl butyrate or the like is used to remove the colored material (Patent Document 1, Patent Document 2), or ceramic veneer or the like is used to coat the teeth. There are ways to improve color tone. As chemical methods, a method for promoting remineralization with an oral composition containing hydroxyapatite (Patent Document 3, Patent Document 4), an oxidative bleaching method using a peroxide (Patent Document 5), A method of using a tooth whitening composition in which a self-curing calcium phosphate compound and a fluorine compound are mixed with an oxide (Patent Document 6), and an oral composition containing a liquefied calcium phosphate compound promotes remineralization of enamel. A method (Patent Document 7) and the like are known. Moreover, the composition for oral cavity (patent document 8) which uses a polyvalent metal cation and polyphosphoric acid together and prevents tartar and dirt is known.

However, the method using ceramic veneer or the like needs to delete the tooth substance, and use of this method requires guidance and treatment by a dentist. In addition, the method of oxidative bleaching using peroxide requires the use of a high-concentration peroxide capable of oxidative bleaching of teeth, so it must be performed carefully according to expert guidance, and teeth are whitened. As a result, the gloss decreases. In addition, even under the guidance of experts, peroxides may cause damage to the teeth and gums and hypersensitivity.

On the other hand, the method of promoting tooth remineralization using calcium phosphate compounds such as hydroxyapatite mainly makes the teeth healthy by repairing the enamel surface with apatite. I can't say. Moreover, it cannot be said that there is a sufficient whitening effect even when polyphosphoric acid and a polyvalent metal cation are used in combination. And, these conventional whitening dentifrices do not provide a tooth that imparts gloss to the teeth, particularly to the teeth themselves.

In addition, phytic acid is known to have effects such as removal of tobacco crabs, tartar-inhibiting effects, and stabilization of tin fluoride, and phytic acid-containing cleaning agents and dentifrices have been reported ( Patent Document 9). Moreover, in order to improve the astringency when the composition containing phytic acid is applied to the oral cavity, amphoteric electrolytes such as amino acids and proteins (Patent Document 10) and specific perfume ingredients (Patent Document 11) are improved. ), Chain hydrocarbon compounds (Patent Document 12), polyvinyl alcohol, polyvinylpyrrolidone (Patent Document 13), and the like are known. In addition, there is a technique of blending an alkali metal sulfate salt to improve the convergence of polyphosphate (Patent Document 14).

JP-A-1-203316 JP-A-1-104004 JP-A-1-305020 JP-A-9-202718 Japanese Patent Publication No. 6-8248 JP-A-11-116421 JP-A-8-319224 JP-A-52-108029 JP-A-56-18913 Japanese Patent Publication No.61-23768 JP-A-62-198611 JP-A-10-87458 JP 2000-26259 A Japanese Unexamined Patent Publication No. 7-285839

An object of the present invention is to provide a method capable of imparting an excellent whitening effect to teeth and imparting gloss.

Therefore, the present inventor has examined the relationship between the tooth surface state, tooth whiteness and luster (gloss) using a scanning electron microscope, and most of the coloring substances generated on the tooth surface are caused by abrasives. Although it can be removed by tooth brushing or the like, it has been found that a small solid product having a height (thickness or diameter) of less than 1 μm cannot be appropriately removed by a conventional whitening agent or abrasive. And further examination showed that the presence or absence of such a small solid product has a great influence on the gloss of the teeth, and this small solid product has a certain range of pH and does not contain a polyvalent cation. The present inventors have found that it can be removed by a composition containing phytic acid, and that using this composition, both whitening and glossing of teeth can be achieved simultaneously.

In addition, when the inventor mixes a certain amount or more of erythritol with the composition containing phytic acid, in addition to the effect of removing the solid product generated on the tooth surface, there is a feeling of squeaky teeth due to phytic acid. It was found that an oral composition having a remarkably improved feeling of use while being remarkably improved can be obtained.

That is, the present invention contains phytic acid or a salt thereof in an amount of 0.05 to 18% by mass, does not contain a polyvalent cation, or contains less than 0.1 times mol of phytic acid, and 30% by mass with water. The present invention provides a method for removing a solid product formed on the surface of a tooth by applying an oral composition having a pH of 5.5 to 6.5 when diluted to the tooth.
Further, the present invention contains 0.05 to 5% by mass of phytic acid or a salt thereof, does not contain a polyvalent cation, or contains less than 0.1 times mol of phytic acid, and 30% by mass with water. The present invention provides use of an oral composition having a pH of 5.5 to 6.5 when diluted to remove a solid product formed on a tooth surface.
Furthermore, the present invention contains 0.05 to 18% by mass of phytic acid or a salt thereof, does not contain a polyvalent cation, or contains less than 0.1 times mol of phytic acid, and 30% by mass with water. An object of the present invention is to provide a method for imparting gloss by removing a solid product produced on the surface of a tooth, wherein a composition for oral cavity having a pH of 5.5 to 6.5 when diluted is applied to the tooth.

The present invention also includes the following components (A) and (B):
(A) Phytic acid or a salt thereof 0.01 to 10% by mass
(B) Erythritol 3-60% by mass
And a composition for oral cavity in which the mass ratio (B / A) of the component (B) to the component (A) is from 5 to 1,000.
In addition, said water is purified water, Comprising: Ion exchange water or distilled water is meant.

According to the present invention, since a small solid product having a thickness of less than 1 μm deposited on the surface of a tooth that could not be removed by a conventional dentifrice can be removed, the teeth become white and the teeth can be given luster.
In addition, if an oral composition containing erythritol in a certain amount or more with respect to phytic acid is used, a small solid product on the surface of the tooth can be removed, and the squeaking feeling peculiar to phytic acid is improved, and A refreshing feeling is obtained. Here, the squeaky feeling of the teeth refers to the feeling when the teeth are brought into contact with each other or rubbed together, and is a physical discomfort. ADVANTAGE OF THE INVENTION According to this invention, the usability | feel felt by a tooth | gear is favorable and can provide the composition for oral cavity which improved the texture of the surface of a tooth | gear.

The photograph which observed the surface of the tooth before and behind the brushing process with the electron microscope is shown (50 times). The photograph which observed the surface of the tooth after a brushing process with the electron microscope is shown (50000 times). It is a SEM observation photograph of (a) white tooth A and (b) colored tooth B. (A) Tooth B after immersion in a composition containing phytic acid, (b) SEM observation photograph of tooth B before immersion.

The active ingredient of the oral composition used in the method for removing a small solid product having a thickness of less than 1 μm formed on the tooth surface of the present invention is phytic acid or a salt thereof, which acts as a gloss-imparting agent. Phytic acid is also called myo-inositol hexaphosphate, and is a phosphate compound. Among various phosphoric acid compounds, phytic acid or a salt thereof is particularly excellent in the gloss imparting effect of the present invention.
Examples of the salt include alkali metal salts such as sodium and potassium, ammonium salts, and the like, and alkali metal salts are preferable from the viewpoint of taste and odor.

The composition for oral cavity used in the present invention contains 0.05% by mass to 18% by mass of phytic acid or a salt thereof in the composition.
From the viewpoint of sufficiently exhibiting the effect of removing the fine solid product and the effect of imparting gloss of the present invention, those containing phytic acid or a salt thereof in the composition in an amount of 0.05% by mass or more, preferably 0.1% by mass or more From the viewpoint of suppressing the decalcification of teeth and the viewpoint of taste and squeaking, it is 18% by mass or less, preferably 10% by mass or less. In the case where the solid product removing composition of the present invention is a toothpaste, 0.05 to 5% by mass of phytic acid or a salt thereof is contained in the toothpaste from the viewpoint of feeling of use such as taste and creaking. Those are preferred. The content of phytic acid or a salt thereof in the solid product removing composition of the present invention is measured by neutralizing with potassium hydroxide or sodium hydroxide, and the total amount is converted to an acid.

It is preferable that the composition for oral cavity used in the present invention keeps the content of polyvalent cation low. This is because the polyvalent cation makes phytic acid insoluble or reduces the effect of removing the solid product, thereby preventing the reduction of the effect. The content is measured by ICP emission spectrometry (ICP emission analyzer: Perkin Elmer Optima 5300DV), and is preferably less than 0.1-fold mol, more preferably 0.02-fold mol or less with respect to phytic acid as polyvalent cations. Is preferred. That is, it is desirable not to add an agent that mainly supplies polyvalent cations such as aluminum, calcium, magnesium, iron, and zinc, and those that substantially do not contain polyvalent cations are preferable.
In addition to cationic antibacterial agents, adsorbents such as zeolite and activated carbon reduce the solid product removal effect by phytic acid, so that it is preferably less than 0.001% by mass in the oral composition, and further 0 It is preferable that it is 0.0001 mass% or less, and the thing which does not contain substantially is preferable.

The oral composition used in the present invention has a pH of 5.5 to 6.5 when diluted to 30% by mass with water.
That is, when the composition is applied to the oral cavity, the solid product is removed and the composition is diluted to 30% by mass with water from the viewpoint of suppressing the decalcification of the tooth surface and exerting a gloss imparting effect. The pH is preferably 5.5 or more, more preferably 5.8 or more, and the pH is 6.5 or less, and 6.2 or less from the viewpoint of sufficiently exerting the gloss imparting effect by removing the solid product. Is preferred.
Since the pH cannot be measured accurately in the case of a highly viscous oral composition such as toothpaste, the pH of the composition is obtained by diluting the composition to 30% by mass with water. . What was diluted to 30% by mass with water was assumed to be applied to the oral cavity of the composition. The water is purified water, and distilled water or ion exchange water is used.
In order to adjust the pH of the composition to the above range, it is preferable to use a pH adjuster, and as the pH adjuster, it does not inhibit solid product removal by phytic acid and can suppress tooth decalcification. Organic acids such as acetic acid, fumaric acid, malic acid, lactic acid, gluconic acid and tartaric acid, phosphoric acids other than phytic acid (for example, orthophosphoric acid), inorganic acid salts such as hydrochloric acid and sulfuric acid, and hydroxides such as sodium hydroxide And basic amino acids such as ammonia, aqueous ammonia, lower alkanolamines, arginine and lysine, etc., may be used alone or in combination of two or more. Among these pH adjusters, the content of organic acid and inorganic acid (excluding phytic acid) is 5% or less by mass ratio to phytic acid from the viewpoint of not inhibiting the solid product removal effect of phytic acid. Is preferable, and it is further preferable that it is 1% or less.

The oral composition used in the present invention preferably further contains erythritol. Erythritol is preferably contained in an amount of 10 to 60% by mass from the viewpoint of imparting gloss, more preferably 15 to 60% by mass, particularly preferably 20 to 60% by mass, and further 20 to 20% in consideration of the refreshing feeling and taste. It is preferable to contain 50 mass%. Erythritol can be blended into the oral composition of the present invention in the form of powder or particles having a particle diameter of less than 35 μm from the viewpoints of feeling of use, refreshment and taste.
As the structure of erythritol, there are three isomers of L-erythritol, D-erythritol, and meso-erythritol, and any of these structures can be used in the present invention. As erythritol, those which are usually available can be used, and examples thereof include crystalline erythritol obtained by recrystallization after fermentation of glucose. As crystalline erythritol, commercially available products such as those manufactured by Nikken Chemical Co., Ltd., Mitsubishi Chemical Foods Co., Ltd., Celestor, Cargill, etc. are available. Moreover, the thing with a large particle size can use what adjusted the particle diameter by grind | pulverizing. A roller mill, a hammer mill, a high-speed pulverizer, a pulverizer, etc. are generally used to pulverize erythritol, but a high-speed pulverizer and hammer mill that are easy to adjust the particle size and excellent in production efficiency. Is preferred.

When the oral composition used in the present invention is a dentifrice, it is desirable that erythritol is dispersed in the dentifrice in the form of powder or particles. For this purpose, erythritol is preferably added in the form of powder or particles to the final production step. In addition, from the viewpoint that a cool sensation continues in the oral cavity, the particle size is preferably 45 μm or more and less than 355 μm, more preferably 53 μm or more and less than 300 μm, and even more preferably 75 μm or more and less than 250 μm. Erythritol particles having a particle size of 45 μm or more are preferred because they do not dissolve instantaneously in the mouth and a long cool feeling. Moreover, the thing less than 355 micrometers can melt | dissolve easily in an oral cavity, and can exhibit a cool feeling.

The erythritol particle size is measured as follows.
Sieve: JIS standard sieve φ75mm
Opening: From the upper stage, a receiver is provided under a sieve having openings of 500 μm, 355 μm, 250 μm, 180 μm, 125 μm, 90 μm and 45 μm, respectively.
Shaker: Micro type electromagnetic vibrator M-2 type (Tsutsui Rikenki Co., Ltd.)
Method: Place 15 g of sample on 500 μm sieve and classify with electromagnetic vibrator for 5 minutes. The total amount of erythritol present on a sieve having openings of 250 μm, 180 μm, 125 μm, 90 μm and 45 μm is defined as erythritol having a particle size of 45 μm or more and less than 355 μm.

In the present invention, the solid product produced on the tooth surface refers to a solid product produced on the tooth surface and having a thickness of less than 1 μm, which can be confirmed by an electron microscope (SEM: Hitachi S-4800). The solid material having a thickness of less than 1 μm generated on the tooth surface includes a collection of solid materials having a thickness of 500 nm or less. As can be understood from the SEM photograph of FIG. 2B described later, this fine solid product is a deposit of nano-level solid product having a thickness of 200 nm or less, preferably 100 nm or less. It is thought that it is formed by depositing components such as protein, calcium, and phosphorus, and the formed deposit is deposited. In addition, this fine solid product is likely to be deposited and generated due to deterioration of the oral environment due to aging or decrease in saliva secretion.

As described above, according to the method of the present invention, a solid product having a tooth surface height of less than 1 μm, and further a solid product having a height of 0.5 μm or less can be removed without forming irregularities on the tooth surface. Good gloss is imparted to the teeth. As described above, according to the composition of the present invention, since the nano-level solid product can be selectively removed without damaging the tooth surface, the tooth surface can be smoothed and gloss can be imparted. Play.

In addition, as described above, the inventor contains (A) 0.01 to 10% by mass of phytic acid or a salt thereof, and (B) 3 to 60% by mass of erythritol, and B / A = 5 to 1000 It has been found that a certain composition for oral cavity has an excellent tooth whitening effect and an effect of imparting gloss to the teeth, and there is no squeaky feeling of the teeth and a good feeling of use.

The oral composition of the present invention contains phytic acid or a salt thereof (A) in an amount of 0.01 to 10% by mass in the composition. Phytic acid or a salt thereof (A) is preferably contained in an amount of 0.05% by mass or more, more preferably 0.1% by mass or more from the viewpoint of teeth whitening action and gloss imparting action. The salt (A) is preferably contained in the composition in an amount of 5% by mass or less, and more preferably 2% by mass or less. When the oral composition of the present invention is a mouthwash, phytic acid or a salt thereof (A) is preferably 3% by mass or less, more preferably 1% by mass or less. In addition, the content of phytic acid or a salt thereof in the present invention is measured by neutralizing with potassium hydroxide or sodium hydroxide, and the total amount is converted to an acid.

The oral composition of the present invention contains 3 to 60% by mass of erythritol (B). By blending erythritol within this range, the squeaking feeling of phytic acid is improved and a good feeling of use is obtained. A more preferable content of erythritol is 4 to 50% by mass, and more preferably 5 to 45% by mass. When the oral composition of the present invention is a mouthwash, erythritol is preferably 30% by mass or less, more preferably 20% by mass or less.

The mass ratio (B / A) of the component (B) to the component (A) in the present invention is important in terms of the effect of improving the squeakiness of teeth and the feeling of use by phytic acid, and is 5 to 1000, more preferably 10 to 800, Further, 15 to 500, particularly 20 to 500 are preferable. When the oral composition of the present invention is a mouthwash, the mass ratio (B / A) of component (B) to component (A) is 5 to 300, more preferably 10 to 300, more preferably 15 to 300, particularly 20 to 300 are preferred.

As mentioned above, phytic acid is a kind of phosphoric acid compound, and other phosphoric acid compounds such as polyphosphoric acid have a squeaky sensation of teeth, but the squeaking sensation of phytic acid is unique. Even if erythritol is blended, the squeaky sensation of teeth due to polyphosphoric acid is not improved, so the action of the present invention is considered to be peculiar to the combination of phytic acid and erythritol.

In addition, the oral composition used in the present invention includes sodium fluoride, potassium fluoride, ammonium fluoride, and monofluorolin as long as the gloss imparting effect by phytic acid or a salt thereof is not inhibited (content, dosage form, etc.). Fluoride such as sodium acid (fluorine ion supply compound) may be blended. The fluoride is not contained in the composition or is preferably less than 500 ppm in terms of fluorine atoms, and more preferably contains 300 ppm or less.

The oral composition used in the present invention includes, in addition to the above-mentioned components, for example, foaming agents, foaming aids, abrasives, wetting agents, thickeners, gelling agents, binders, bulking agents, sweeteners, preservatives. , Fungicides, medicinal components, pigments, dyes, fragrances and the like can be appropriately contained, and the composition can be produced according to various dosage forms. Moreover, combined use, such as polyethyleneglycol which is a whitening component used conventionally, is not restrict | limited.

The oral composition used in the present invention is prepared in a dosage form such as a solution, a gel, or a paste, and is used for oral use such as a powder dentifrice, a moisturizing dentifrice, a toothpaste, a liquid dentifrice, and a mouthwash. It can be used as a composition or food such as chewing gum, troche and candy, or can be used as an oral hygiene device such as dental floss by impregnating a sheet material, cloth or fiber.
In any of these dosage forms, polyethylene glycol, propylene glycol, glycerin, sorbitol, maltitol, xylitol, lactitol and the like can be contained for the purpose of a wetting agent or a thickening agent.

Further, as a thickening agent for a solution-like composition or a gelling agent for a gel-like composition, and as a binder for a paste-like composition, sodium carboxymethylcellulose, hydroxyethylcellulose, carboxyvinyl polymer, xanthan gum, carrageenan, alginic acid Sodium, hydroxypropyl cellulose, guar gum, sodium chondroitin sulfate and the like can be contained alone or in combination. Among these, it is preferable to select a binder other than sodium alginate from the viewpoint of sufficiently exerting the gloss imparting effect of phytic acid or a salt thereof.
In particular, in the case of a high salt concentration due to the buffer system, one or more kinds of nonionic polymers, that is, hydroxyethyl cellulose, guar gum, hydroxypropyl cellulose and the like can be contained.

When the composition of the present invention is a toothpaste, the content of phytic acid or a salt thereof is preferably 0.05 to 5% by mass from the viewpoint of use feeling. The toothpaste preferably has a viscosity at 25 ° C. of 10 to 300 Pa · s, more preferably 20 to 250 Pa · s, particularly preferably 30 to 200 Pa · s, from the viewpoint of a sufficient gloss imparting effect. Within this range, even if the content of phytic acid is 5% by mass or less, the dispersibility in the mouth is enhanced, so that phytic acid is quickly diffused and effectively applied to the fine solid product deposited on the tooth surface. Works. When the viscosity is too low, the operability is deteriorated because it hangs down from the toothbrush, and when the viscosity is too high, dispersibility in the mouth is lowered. It can no longer be obtained. Here, the viscosity can be measured using a helipath type viscometer at a measurement temperature of 25 ° C. and measurement conditions of rotor C, 2.5 r / min, and 1 minute.

When the composition of the present invention is a dentifrice, a granule can also be blended, but from the viewpoint of suppressing the formation of minute irregularities on the surface of the enamel of the tooth and not inhibiting the gloss formation, the granule is not blended or It is preferable to contain granules having a disintegration strength of 10 g / piece or less in a dry state, preferably granules having a disintegration strength of 10 g / piece or less in the presence of moisture. Moreover, it is also possible to contain an abrasive within a range that does not impair the gloss forming effect of the present invention. For example, it is preferable to use a silica-based abrasive such as hydrous silica, anhydrous silica, or silica gel.

In order to apply the composition of the present invention to teeth, it may be applied as it is, or includes both cases where it is applied in a state diluted to about 30% by mass with water or saliva. That is, in the case of a mouthwash, it is applied to teeth without dilution. On the other hand, in the case of a toothpaste, etc., it is applied to the teeth in a state diluted to about 30% by mass with saliva.
Such a composition on a human tooth for 10 seconds to 10 hours (10 seconds or more for a mouthwash, 30 seconds or more for a dentifrice, 5 minutes or more for an applicator), for example When applied 1-5 times a day, preferably 1-16 weeks, damage to the tooth enamel itself by selectively removing nano-level (less than 1 μm) solid product on the tooth enamel surface By smoothing the enamel surface of the tooth at the nano level and suppressing the reflected light from the enamel surface while suppressing the above, the natural gloss of the tooth itself can be obtained. That is, even with long-time use or repeated use, natural gloss and glossy teeth can be obtained while suppressing damage to the enamel surface of the teeth.

As described above, the action of the composition of the present invention to whiten teeth and impart natural luster and luster to the teeth is considered to occur by removing nano-level solid products on the tooth enamel surface. However, it is considered that the composition of the present invention has an action of re-forming the trabecular space inside the tooth enamel, and the whitening action of the tooth is also caused by the re-formation action of the trabecular space.

The enamel of a tooth is made up of a collection of columnar bodies made of hydroxyapatite polycrystals called enamel trabeculae. In general, in the youth, a space (gap), that is, a trabecular space exists between the enamel trabeculae and the enamel trabeculae, and is filled with water, saliva components, and the like. In such a tooth, the incident light to the enamel is scattered due to a large difference in refractive index between the enamel trabeculae and the space between the trabeculae, and the teeth appear white.
However, if the substance dissolved in saliva continues to accumulate in the trabecular space of the tooth enamel surface, for example due to aging, the trabecular space is filled, and as a result, the refractive index of the enamel trabecular space is smaller than that of the trabecular space. As the difference becomes smaller, the enamel becomes more transparent and incident light tends to reach the dentin, which is yellow or brown, located deep in the enamel, and the teeth appear yellow.
Therefore, the present inventors have formed enamel by selectively removing from the trabecular space a material (hereinafter referred to as “trabecular space material”) present in the trabecular space of the tooth enamel surface layer. By re-forming the trabecular gap while suppressing damage to the enamel trabecula itself, and increasing the reflected light from the inside of the enamel by light scattering by the space of the trabecular gap, natural white teeth can be obtained Thought.
Therefore, when the composition of the present invention was applied to the teeth and the action on the trabecular space was evaluated, as shown in the examples described later, the composition of the present invention had an excellent effect of promoting trabecular gap re-formation. I found it.

In the following examples,% means mass%.

Test Example 1: Surface condition of teeth after treatment with composition Table 1 shows each component and content of a toothpaste containing 1% phytic acid. A toothpaste (Example 1) in which these components were mixed was prepared as a test solution. The polyvalent cations such as magnesium, aluminum, calcium and the like in the test solution of Example 1 were less than 0.1-fold mol with respect to phytic acid as measured by IPC emission spectrometry. In Comparative Example 1, a dentifrice containing no phytic acid was prepared as a test solution.
The pH of the test solution of Example 1 is the pH when diluted to 30% by mass with ion-exchanged water. Since Comparative Example 1 did not contain phytic acid, the pH was neutral, and the pH was not adjusted with potassium hydroxide. The teeth used for the test were human teeth (extracted teeth) that were not treated to remove dirt due to polishing or the like.

The brushing process was performed according to the following procedure. While immersing human teeth (extracted teeth) in each test solution at room temperature for 2 minutes, brushing with a toothbrush (clear clean multi-care toothbrush, normal: manufactured by Kao Corporation) is performed. Then, it was immersed in artificial saliva at room temperature for 8 hours. This cycle was performed 28 times. Artificial saliva is an aqueous solution of calcium chloride (1.0 mM), potassium hydrogen phosphate (0.9 mM), HEPES (4- (2-hydroxyethyl) -1-piperazine etheric acid) (2.0 mM). And adjusted to pH = 7. In this case, the change in luminance value Δ before and after the 28th cycle was measured. The change Δ luminance was obtained from (luminance after immersion−luminance before immersion). In addition, three human teeth (extracted teeth) were used, and Δ luminance was evaluated by an average value of measured values of the three human teeth.

As a luminance measurement method, a method of measuring the surface reflected light intensity from image analysis using polarized light was used. As a device for taking images for evaluation, the camera is a digital single-lens reflex camera Nikon D70, the lens is Ai AF Micro Nikkor 105mm F2.8D, and the strobe emission is wireless remote speedlight SB-R200 (all manufactured by Nikon). The installed one was used. Photographing was carried out by placing a plastic polarizing plate (manufactured by Edmond) in front of the light emitting part of the speedlight and the lens so that the transmission axes intersected 30 degrees. For the captured image, the average brightness of the highlight portion was determined using Adobe Photoshop CS3 (manufactured by Adobe System). Luminance means that the larger the value, the higher the gloss.

The unevenness of the surface state in Table 1 is evaluated by observing the teeth after the brushing treatment of the above-mentioned 28 cycles with the naked eye using a magnifying glass (magnification 10 times). On the other hand, FIGS. 1 and 2 show photographs obtained by observing the tooth surface before and after the brushing process with an electron microscope (SEM: Hitachi S-4800). (A) After the brushing process with the test solution of Example 1 (B) After the brushing treatment with the test solution of Comparative Example 1, (c) After the brushing treatment while being immersed in ion-exchanged water without using the test solution, (d) A photograph of the tooth surface before the brushing treatment. FIG. 1 is a photograph taken 50 times, and FIG. 2 is a photograph taken 50000 times.
As shown in FIG. 1, a solid product smaller than 1 mm (μm level) can be confirmed on the tooth surface of the photograph (c) after the treatment using only the brushing without using the test solution. In the photograph (b) after the brushing treatment using the test solution of Comparative Example 1, it is recognized that a solid product remains as a part of the dullness. The photograph (a) after the brushing treatment using the test solution of Example 1 is smooth and no solid product is observed. On the other hand, in the photograph of FIG. 2, although a solid product of less than 1 μm is observed in the photograph (b) after the brushing treatment using the test solution of Comparative Example 1, the brushing treatment using the test solution of Example 1 In the later photograph (a), almost no solid product of less than 1 μm is observed. The human teeth after the brushing treatment with the test solution of Comparative Example 1 hardly changed in luminance, whereas the human teeth after the brushing treatment according to Example 1 had a high Δ luminance and a gloss imparting effect was recognized. Further, the human teeth after the brushing treatment according to Example 1 looked whiter than the human teeth after the treatment according to Comparative Example 1. Therefore, by removing the solid product of less than 1 μm generated on the tooth surface, not only the teeth become white, but also the total reflected light can be increased and high brightness, that is, gloss and gloss can be obtained. Conceivable.

Test Example 2: Relationship with Other Organic Acid Content Table 2 shows each component and content of a toothpaste containing 1% phytic acid. A toothpaste in which these components were mixed was prepared as a test solution. The polyvalent cations such as magnesium and aluminum in the test solution were less than 0.1 times mol of phytic acid as measured by IPC emission spectrometry.
(1) Each toothpaste was diluted to 30% by mass with ion-exchanged water to obtain a test solution. Human teeth were immersed in the test solution for 48 hours at room temperature without brushing, and the luminance before and after immersion was measured. Change in luminance before and after immersion ΔBrightness was determined from (luminance after immersion−luminance before immersion). The human teeth are extracted teeth that have not been subjected to dirt removal treatment such as polishing as in Test Example 1 above, and the change in luminance before and after immersion with the test solution is measured. Performed as in Example 1.

Table 3 shows the toothpaste test solution in Example 1 in Table 2 and 1% by mass of phytic acid in Example 1, 1% by mass of orthophosphoric acid, 1% by mass of polyphosphoric acid, phytic acid and polyphosphoric acid, respectively. For test solutions prepared with the same components and blending ratios as in Example 1 except that the mixture was replaced by 1% by mass, human teeth were immersed in each test solution for 48 hours at room temperature in the same manner as in Test Example 2 and measured before and after immersion. The luminance change Δ luminance and the surface condition of the extracted tooth after immersion are shown. As shown in Table 3, human teeth treated with a test solution containing polyphosphoric acid and a mixture of polyphosphoric acid and phytic acid were found to be damaged with irregularities observed on the surface of the enamel, and Δ luminance was negative. (Gloss is decreasing). Human teeth treated with a test solution containing orthophosphoric acid showed almost no damage to the enamel surface, but a solid product remained on the tooth surface, resulting in a small Δ luminance value and a gloss-enhancing effect. Was not recognized. On the other hand, phytic acid had a large Δ luminance value, and the tooth surface was smooth and no damage was observed, and a high gloss imparting effect was observed. In addition, pyrophosphoric acid and metaphosphoric acid were also tested in the same manner as polyphosphoric acid, but no gloss imparting effect was observed because the surface of the teeth was damaged.
Therefore, phytic acid is most excellent in the effect of imparting gloss among these phosphoric acid compounds, and it is considered that the selective removal effect of the solid product on the tooth surface is high due to the increase in total reflected light. Furthermore, the following tests were conducted on test solutions containing phytic acid.

Test Example 3: Composition pH and Phytic Acid Content of Composition (1) Preparation of Composition and Test Object Table 2 shows each of the toothpastes of Examples 1 to 10 in Table 2, and Comparative Examples 2 to 9 in Table 4. Ingredients and their contents are shown. The pH of these toothpastes (test solutions) is the pH when diluted to 30% by mass with ion-exchanged water.
When the content of phytic acid in the toothpaste is 1% by mass and this pH is diluted to 30% by mass with ion-exchanged water, 3.0, 4.0, 5.0, 5.5, 6. Test solutions of toothpastes (Examples 1 to 3 and Comparative Examples 2 to 6) adjusted to 0, 6.5, 7.0, and 8.0 were prepared. The content of polyvalent cations such as magnesium and aluminum in each of these test solutions was less than 0.1 times mol of phytic acid as measured by IPC emission spectrometry.
Further, each test solution of toothpaste adjusted to pH 6.0 with the content of phytic acid in the toothpaste being 0, 0.05, 0.1, 10, 18, 19, 20% by mass (implemented) Examples 4-7 and comparative examples 7-9) were prepared. A phytic acid content of 1% by mass was considered as Example 2. The content of polyvalent cations such as magnesium and aluminum in each of these test solutions was also less than 0.1 times mol with respect to phytic acid as measured by IPC emission spectrometry.
The condition of the human teeth used in the test is the same as in Test Example 1. The change in luminance before and after immersion with each test solution Δ, the measurement of the tooth surface condition (surface irregularities) are the same as in Test Example 1 above. The same was done.
As shown in Comparative Examples 2 to 4, in the region where the pH is lower than 5.5, unevenness is formed on the tooth surface, and the luminance of the tooth surface is lowered. On the other hand, teeth treated with a test solution having a pH of 7.0 or higher in Comparative Examples 5 and 6 do not have unevenness on the surface, but no solid product removal effect is observed, and Δ luminance is low and gloss is not obtained. It was. On the other hand, the solid product removing composition of the present invention has a pH of 5.5 or more and 6.5 or less, and not only teeth appear white under these conditions but also Δ luminance is sufficiently large and high gloss is imparted. The effect was demonstrated, and a smooth surface was also observed by SEM observation.
As described above, the phytic acid (inositol 6-phosphate) and its salt in the region of pH 5.5 to 6.5 according to the present invention hardly damage the enamel surface, and 1 μm formed on the surface. Less than solid product can be selectively removed.

Further, even when the concentration of phytic acid is 0.05%, not only teeth become white, but also a high luminance imparting Δ luminance is 4.5, and when it is 0.1% or more, Δ luminance is 5.8 or higher and high gloss is obtained. The imparting effect was shown. However, as shown in Comparative Examples 8 and 9, it was observed that the tooth surface was uneven at a concentration of 19% by mass or more. Moreover, the density | concentration of 10 mass% or less and also the density | concentration of 5 mass% or less are preferable also from a viewpoint of taste. In Comparative Example 7, in which phytic acid was not blended and lactic acid was blended at 1%, the tooth surface was uneven and gloss was lowered (Δ luminance was negative).

Furthermore, Examples 8 to 10 containing erythritol have higher Δ luminance than Example 1 of the same pH containing the same amount of phytic acid, and Examples 8 to 10 are among Examples 1 to 10. The Δ brightness was high. It was confirmed that the gloss imparting effect was improved by further containing erythritol in phytic acid.

Test Example 4: Content of polyvalent cation in composition The toothpastes of Example 1 and Comparative Examples 10 and 11 shown in Table 5 were prepared as test solutions. Comparative Example 9 in which the content of phytic acid in the toothpaste is 1% by mass, and the total amount of magnesium and aluminum is 5000 ppm with respect to Example 1 in which the polyvalent cation is not substantially mixed, the total of magnesium and aluminum A test solution of Comparative Example 11 containing 500 ppm was prepared. The pH of these toothpastes (test solutions) is the pH when diluted to 30% by mass with ion-exchanged water. In addition, the polyvalent cation of Example 1 is magnesium 18.4 ppm (0.05 times mol with respect to phytic acid), aluminum 16.4 ppm (0.04 times mol with respect to phytic acid), and the total of polyvalent cations. The amount is 36.8 ppm and is less than 0.1 times mol of phytic acid, and Comparative Example 9 contains 5000 ppm of magnesium and contains 13.6 times mol or more of polyvalent cation with respect to phytic acid. 10 contained 500 ppm of aluminum and contained 1.2 times or more of polyvalent cation with respect to phytic acid.
The condition of the human teeth used in the test is the same as in Test Example 1, and the change in luminance before and after immersion with each test solution Δ, the measurement of the unevenness of the tooth surface condition, and the measurement of the unevenness of the tooth surface condition are the same as in Test Example 1 above. I went there.
In Comparative Example 10 containing 5000 ppm of magnesium and Comparative Example 11 containing 500 ppm of aluminum, a state in which the solid product before the test remained on the tooth surface was observed, and the teeth appeared yellow compared to Example 2, and Δ luminance And the solid product removal effect and gloss imparting effect by phytic acid were suppressed.
Thus, phytic acid and its salts in the presence of polyvalent cations that do not contain polyvalent cations or are less than 0.1-fold mol of phytic acid have a reduced solid product removal effect by phytic acid. In addition to having the effect of whitening the teeth, it can sufficiently function as a gloss imparting agent.

Test Example 5 Density of Dentifrice The toothpastes of Examples 11 to 13 shown in Table 6 were prepared as test solutions. The content of magnesium and aluminum in each of these test solutions was less than 0.1 times mol of phytic acid as measured by IPC emission spectrometry. In contrast to Example 11 in which the content of phytic acid in the toothpaste was 1% by mass and the viscosity was adjusted to 90 Pa · s, the amount and quality (degree of etherification) of sodium carboxymethylcellulose and the purified water were adjusted. The toothpaste of 12 was prepared at 220 Pa · s, and the toothpaste of Example 13 was prepared at 400 Pa · s. Viscosity was measured using a helipath viscometer at a measurement temperature of 25 ° C. under rotor C at 2.5 r / min (2.5 rpm) for 1 minute. In the test, each test solution was diluted to 30% by mass with ion-exchanged water, human teeth were immersed in the diluted test solution for 48 hours, luminance before and after immersion was measured, and luminance change before and after immersion Δ luminance (immersion Subsequent luminance-luminance before immersion) was determined. The state of the human teeth was the same as in Test Example 1, and the change in luminance Δ before and after immersion with each test solution, the measurement of the luminance, and the observation of the unevenness of the tooth surface were performed in the same manner as in Test Example 1. The test solution was diluted to 30% by mass with ion-exchanged water, assuming that the toothpaste was applied to the oral cavity, and the toothpaste having the composition of Examples 11 to 13 was diluted to 30% by mass. Then, the viscosity becomes 1/8 to 1/10. For example, the viscosity of the toothpaste of Example 10 diluted with 30% by mass is about 30 Pa · s. In each of Examples 11 to 13, it was recognized that the surface was smooth and the teeth were white, but the Δ luminance of the low viscosity example was higher, especially when the viscosity of the toothpaste was 250 Pa · s or less. Brightness was obtained.

Test Example 6: Observation of tooth trabecular gap by SEM FIGS. 3 and 4 show photographs of tooth trabecular gap observed by an electron microscope (SEM: Hitachi S-4800). FIG. 3A shows a photograph of white teeth A (10th generation human teeth) observed with an electron microscope (SEM), and FIG. 3B shows colored teeth B (50th generation human teeth).
As shown in the photographs in FIGS. 3A and 3B, the trabecular space can be observed with the white teeth A, but the trabecular space can hardly be observed with the colored teeth B.
FIG. 4 (b) shows the tooth B before dipping in the composition containing phytic acid of the present invention, and FIG. 4 (a) shows that after dipping in the composition containing phytic acid of the present invention (Example 2). The photograph observed with the electron microscope of the tooth | gear B of is shown. As shown in the photographs of FIGS. 4 (a) and 4 (b), the trabecular space can hardly be observed in the photograph of FIG. 4 (b) before immersion of the tooth B, but small in the photograph of FIG. 4 (a) after immersion. The column gap was observed, and it was confirmed that a small column gap was formed. Tables 2 and 4 show the results of observing the trabecular space of the teeth by SEM for the examples and comparative examples.

Test Example 7
Mouthwashes described in Tables 7 and 8 were prepared and the squeaky feeling of the teeth was evaluated.
The mouth was rinsed with mouthwash for 20 seconds and the mouthwash was discharged, and then the teeth were rubbed together to evaluate the feeling of squeezing. The evaluation was performed in the following four stages, and an evaluation common to two or more of the three subjects was adopted.
AA: I don't feel any squeaky teeth.
A: Little squeaky teeth are felt.
B: Slightly squeaky teeth and good.
C: I feel a squeaky tooth.
The evaluation results are also shown in Table 7.

As shown in Example 25 of Table 7, the mouthwash having a pH of 6 and containing 0.3% by mass of phytic acid had a feeling of squeaky teeth (C). On the other hand, as shown in Table 7, the mouthwash of Example 21 in which glycerin was blended with 0.3% by mass of phytic acid did not improve the squeaking feeling of the teeth, and conversely, the squeaking feeling of the teeth was strong. became. In addition, the squeakiness of teeth was not improved in Examples 22 and 23 in which the same amounts of sorbitol and xylitol as erythritol were blended. Furthermore, the squeakiness of the teeth was not improved in Example 24 in which sorbitol was blended in 0.1% by mass of phytic acid. In addition, sorbitol blended had a sweet taste but low refreshing feeling, and xylitol blended had a sweet taste but a refreshing refreshing feeling was not obtained.

On the other hand, Example 31 containing erythritol was effective in improving the squeaky sensation of teeth by phytic acid. Further, as shown in Table 8, when the ratio of erythritol / phytic acid is 5 or more, the effect of improving the squeaking feeling of the tooth is obtained, and when it is 15 or more, the effect of improving the squeaking of the tooth is excellent. It was found that the effect of the squeaky teeth was even better. Moreover, the feeling of use of the obtained mouthwash was good because the squeakiness of the teeth was improved and the refreshing feeling was excellent.

Test Example 8
Table 8 shows the result of measuring the change in b ^* as an evaluation of the whitening effect of the teeth and the result of measuring the luminance (Δ luminance) as an evaluation of the gloss or gloss of the teeth. The whitening effect and the gloss of the teeth are evaluated with the removed human teeth, and the whitening is performed with a toothbrush (Purera toothbrush compact hair hardness: normal) made in ion-exchanged water for 2 minutes. Thus, human teeth from which the enamel surface was removed were used, and human teeth without brushing treatment were used for gloss evaluation. The whitening effect and gloss were evaluated by immersing human teeth in each mouthwash at room temperature for 48 hours, and measuring changes in b ^* (Δb ^* ) and luminance (Δ luminance) before and after the immersion. Three human teeth were used, and Δb ^* and Δ luminance were evaluated based on the average value of the three data.

B * change [Delta] b ^* is the human teeth before and after immersion in each mouthrinse, - obtained from (after immersion b ^* before immersion b ^*). This b ^* value is an image taken with a digital camera D1x, Ai AF Zoom Micro Nikkor ED 70-180mm F4.5-F5.6D (all manufactured by Nikon) and a white flash light source (manufactured by Konica Minolta). Was expressed in the L ^* a ^* b ^* color system using Adobe Photoshop CS3 (manufactured by Adobe Systems). A positive b ^* value closer to 0 means less yellowness and whiteness, and a larger -Δb ^* (Δb ^* absolute value) means whiteness. Among Examples 21 to 30, Examples 28 and 29 having a high pH have a small absolute value of Δb ^* .

The change in luminance (Δ luminance) of human teeth before and after immersion in each mouthwash was obtained from (luminance after immersion-luminance before immersion). As a luminance measurement method, a method of measuring the surface reflected light intensity from image analysis using polarized light was used. As a device for taking images for evaluation, the camera is a digital single-lens reflex camera Nikon D70, the lens is Ai AF Micro Nikkor 105mm F2.8D, and the strobe emission is wireless remote speedlight SB-R200 (all manufactured by Nikon). The installed one was used. Photographing was carried out by placing a plastic polarizing plate (manufactured by Edmond) in front of the light emitting part of the speedlight and the lens so that the transmission axes intersected 30 degrees. For the captured image, the average brightness of the highlight portion was determined using Adobe Photoshop CS3 (manufactured by Adobe System). The larger the numerical value, the higher the gloss, and the higher the numerical value of Δ, the higher the gloss.

The prescription for the mouthwash and toothpaste of the present invention is shown below. The evaluation of the mouthfeel of the mouthwash was performed under the same conditions as in Test Example 7, and whitening evaluation and gloss evaluation were performed under the same conditions as in Test Example 8. Evaluation of toothpaste of toothpaste was performed on 3 subjects, brushed with toothpaste for 2 minutes, rinsed mouth, then rubbed into teeth and evaluated for squeaky feeling. Evaluation was adopted. The whitening effect and gloss evaluation of the toothpaste were performed by immersing human teeth in a solution obtained by diluting the toothpaste twice, and evaluation was performed under the same conditions as in Test Example 8.

Example 41 (Mouth Wash)
Phytic acid (50% aqueous solution) 0.5
Erythritol 6
Glycerin 6
Ethanol 4
Polyglycerin laurate 0.5
Saccharin sodium 0.01
Fragrance 0.2
Potassium hydroxide aqueous solution (48% aqueous solution) Adjust to pH 6
Purified water remaining
Total 100 (%)
Erythritol / phytic acid (mass ratio) 24
Teeth squeak evaluation AA
Whitening evaluation Δb * = − 5.4, gloss evaluation Δluminance = 7.4

Example 42 (Toothpaste)
Phytic acid (50% aqueous solution) 1
Erythritol 40
Sorbitol solution (70% aqueous solution) 25
Sodium carboxymethylcellulose 0.8
Xanthan gum 0.1
Polyethylene glycol 5
Saccharin sodium 0.1
Abrasive silica 11
Sodium lauryl sulfate 1.5
Sodium hydroxide solution (48% aqueous solution) Adjusted fragrance to pH 6 1
Purified water remaining
Total 100 (%)
Erythritol / phytic acid (mass ratio) 80
Teeth squeak evaluation AA
Whitening evaluation Δb * = − 5.6, gloss evaluation Δluminance = 7.6

Claims (12)

1. Contains 0.05 to 18% by mass of phytic acid or a salt thereof, does not contain a polyvalent cation, or contains less than 0.1 times mol of phytic acid, and has a pH when diluted to 30% by mass with water. A method for removing a solid product formed on a tooth surface, wherein an oral composition of 5.5 to 6.5 is applied to the tooth.
2. The said composition for oral cavity removes the solid product produced | generated on the tooth | gear surface of Claim 1 which contains further 5 mass% or less of organic acids and inorganic acids other than phytic acid with respect to phytic acid or its salt. how to.
3. The method for removing a solid product generated on the tooth surface according to claim 1 or 2, wherein the composition for oral cavity further contains erythritol.
4. The method for removing a solid product formed on the tooth surface according to claim 3, wherein the content of erythritol is 10 to 60% by mass.
5. The method for removing a solid product formed on the tooth surface according to claim 1 or 2, wherein the composition for oral cavity is a toothpaste having a viscosity at 25 ° C of 10 to 300 Pa · s.
6. Contains 0.05 to 18% by mass of phytic acid or a salt thereof, does not contain a polyvalent cation, or contains less than 0.1-fold mol of phytic acid, and has a pH when diluted to 30% by mass with water. A method for imparting gloss by removing a solid product formed on the surface of a tooth, wherein the oral composition of 5.5 to 6.5 is applied to the tooth.
7. Contains 0.05 to 5% by mass of phytic acid or a salt thereof, does not contain a polyvalent cation, or contains less than 0.1 times mol of phytic acid, and has a pH when diluted to 30% by mass with water. Use of an oral composition of 5.5 to 6.5 to remove solid products produced on the tooth surface.
8. The use according to claim 7, wherein the oral composition is a toothpaste having a viscosity of 10 to 300 Pa · s at 25 ° C.
9. The following components (A) and (B):
   (A) Phytic acid or a salt thereof 0.01 to 10% by mass
   (B) Erythritol 3-60% by mass
   And a composition for oral cavity in which the mass ratio (B / A) of component (B) to component (A) is 5 to 1000.
10. The composition for oral cavity according to claim 9, wherein the pH when diluted to 30% by mass with water is 5.5 or more and 8 or less.
11. The oral composition according to claim 9 or 10, wherein the content of (A) phytic acid or a salt thereof is 0.05 to 5% by mass.
12. The composition for oral cavity according to claim 9 or 10, which has a pH of 5.5 to 6.5 when diluted to 30% by mass with water.

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