JP2008074774A - Oral composition - Google Patents

Abstract

[Solution]
(A) 1.0 to 4.0% by mass of protein hydrolyzate derived from soybean or wheat, (B) selected from zinc chloride, zinc nitrate, zinc sulfate, zinc acetate, zinc lactate, zinc gluconate and zinc citrate The water-soluble zinc compound is contained in an amount of 0.5 to 2.0% by mass, and the mass ratio (A / B) of the component (A) to the component (B) is 1.5 to 2.0. Oral composition.
[Effect] The present invention has the excellent anticalculus formation effect of the present invention and a good feeling of use (improvement of feeling of strangeness such as a metallic taste derived from a zinc compound). In particular, even when the blending concentration of the zinc compound is reduced from the usual blending amount, the combined use of the protein hydrolyzate has both an excellent calculus formation inhibitory effect and a good feeling of use.
[Selection figure] None

Description

  The present invention inhibits calculus formation by blending a water-soluble zinc compound, which is a calculus formation inhibitory component, and a protein hydrolyzate derived from soybeans or wheat containing a large amount of acidic amino acids such as glutamic acid and aspartic acid at a specific ratio. The present invention relates to a composition for oral cavity that is excellent in effect and has a good feeling of use with improved metallic taste derived from a water-soluble zinc compound.

  The formation of tartar is considered to be a distant cause of periodontal disease, and is also a major factor in bad breath. On the other hand, the removal is accompanied by a great deal of labor and pain for the patient. In addition, frequent calculus removal leads to healthy tooth grinding and damages the tooth. From these facts, prevention of calculus formation is significant in terms of dentistry.

  In recent years, focusing on the fact that the calculus component is made of calcium phosphate crystals (mainly hydroxyapatite and dicalcium phosphate), the application of zinc compounds (zinc citrate, zinc chloride) from the viewpoint of suppressing the crystal growth Technology has been developed (Non-Patent Document 1). Zinc ions (plus charge) of these zinc compounds have an action of strongly adsorbing to negatively charged sites (phosphate groups, hydroxyl groups) on the crystal surface of calcium phosphate to suppress mineral mineralization.

  However, the calculus formation inhibitory effect by these zinc compounds is not yet sufficient, and further improvement of the effect is desired. However, when these zinc compounds are blended in a preparation at a high concentration in order to obtain a higher effect, there is a problem that a problem occurs in the feeling of use (a metallic taste derived from the zinc compound is expressed). In this connection, as a method for reducing the strong metallic taste of zinc compounds, a composition containing zinc oxide that is sparingly soluble in water (ZnO: not necessarily for the purpose of suppressing calculus formation) has been known. The calculus formation inhibitory effect of zinc oxide was completely insufficient in the test results of the present applicant. No specific technique has yet been developed to improve the feeling of use of zinc compounds formulated in oral compositions, and many rely on masking with fragrances. However, it is also true that there is a limit to the improvement in the feeling of use by this masking (such as blending of strong fragrances and special fragrances). Therefore, the development of a new technology that has a high calculus formation inhibitory effect and excellent usability has been desired.

  On the other hand, a composition applicable to the human body, which is a combination of a zinc compound and a protein hydrolyzate, is disclosed. For example, drinking water that improves bone metabolism by adding a protein hydrolyzate and a specific plant extract to a yeast containing a zinc compound (Patent Document 1: Japanese Patent Laid-Open No. 2002-363086); Antioxidant added with hydrolyzate and specific plant extract (Patent Document 2: Japanese Patent Laid-Open No. 2003-81744), Stress inhibitor added zinc compound and protein hydrolyzate to theanine (Patent Document 3) : JP 2003-321355 A), an antistatic agent obtained by adding a zinc compound and a protein hydrolyzate to polyglutamic acid (Patent Document 4: JP 2005-008837 A), a zinc compound and a protein hydrolyzate to a sicon pigment Hypoallergenic cosmetic composition and anti-inflammatory / analgesic agent (Patent Document 5: Japanese Patent Application Laid-Open No. 2003-276741), Ascorbi Stabilized composition of ascorbic acid ester obtained by adding zinc compound and protein hydrolyzate to acid ester (Patent Document 6: JP 2005-187465 A, Patent Document 7: JP 2005-187466 A), and A salt-resistant cosmetic composition in which a zinc compound and a protein hydrolyzate are added to a specific hydrocarbon compound (Patent Document 8: JP-A-2005-239633). The tartar formation inhibitory effect by these patent technologies is not mentioned at all.

JM ten Cate, “Recent Advances in the study of Dental Calculus”, IRL Press (Oxford), ISBN 0-19-96312-0, 1989, P143-258. JP 2002-363086 A JP 2003-81744 A JP 2003-321355 A JP 2005-008837 A Japanese Patent Laid-Open No. 2003-276741 JP 2005-187465 A JP 2005-187466 A JP 2005-239633 A

  This invention is made | formed in view of the said situation, and it aims at providing the composition for oral cavity containing the zinc compound which exhibits the outstanding calculus formation inhibitory effect and has a favorable usability | use_condition.

  As a result of intensive studies to achieve the above object, the present inventor has identified a specific water-soluble zinc compound and a protein hydrolyzate derived from soybean or wheat containing a large amount of acidic amino acids such as glutamic acid and aspartic acid. By blending into the oral composition at a ratio of 2%, these two components can act synergistically without increasing the blending amount of the water-soluble zinc compound, or even if the blending amount of the water-soluble zinc compound is small. The present inventors have found that an excellent calculus formation inhibitory effect can be exhibited and that the feeling of use can be further improved, and the present invention has been made.

  Conventionally, when a zinc compound (especially zinc citrate or zinc chloride), which is one of the ingredients for inhibiting calculus formation, is used in the oral cavity, there is room for improvement in the feeling of use due to the uncomfortable feeling caused by the metallic taste derived from zinc. . As an improvement measure, the compounding amount of the zinc compound (the usual compounding amount of the zinc compound in the oral composition is 0.5 to 2.0% by mass of the entire composition, and 0.17 to 0.96% by mass as zinc) ) Can be reduced, but if the blending amount is reduced, the calculus formation inhibitory effect is lowered. Moreover, when the compounding quantity of a zinc compound is increased in order to obtain a higher calculus formation inhibitory effect, the feeling of use is further deteriorated. Therefore, it has been difficult to obtain an oral composition containing a zinc compound that has both an excellent calculus formation inhibitory effect and a good usability.

  In view of such circumstances, the present invention has been intensively studied so that there is almost no problem in usability even when a zinc compound is blended and an excellent calculus formation inhibitory effect is exhibited. By using a decomposed product and a specific water-soluble zinc compound in combination, the synergistic effect of both components has almost no discomfort due to the metallic taste derived from the zinc compound, and has a good feeling of use, and high unprecedented calculus formation It has been found that the inhibitory effect is exerted.

In this invention, the action mechanism of the tartar formation inhibitory effect by the protein hydrolyzate derived from soybean or wheat is estimated as follows. That is, protein hydrolyzate derived from soybean or wheat contains a large amount (about 40% of all amino acids) of acidic amino acids such as glutamic acid molecules and aspartic acid molecules in peptide molecules. It is thought that the negative charge) is strongly electrostatically adsorbed on the surface of the calcium phosphate (plus charge) and suppresses the mineralization of mineral ions.
In addition, the action mechanism of the calculus formation-inhibiting effect by the zinc compound is as described above. The zinc ion (plus charge) of the zinc compound is strongly and electrostatically applied to the minus charge portion (phosphate group, hydroxyl group) on the calcium phosphate crystal surface. It adsorbs and has the effect | action which suppresses the calcification formation of a mineral ion.
In the present invention, the combined use of a protein hydrolyzate derived from soybean or wheat and a water-soluble zinc compound causes both of these components to be adsorbed at both negative and positive charge sites on the calcium phosphate crystal surface, and thus synergistic as described above. It is presumed that a functional effect can be obtained.

  In addition, although protein hydrolyzate and a zinc compound are each known as a compounding component to a composition for oral cavity (refer patent documents 1-8), as above-mentioned, specific protein hydrolyzate and water-soluble zinc compound It is a new finding of the present inventor that a composition for oral cavity having both an excellent calculus formation inhibitory effect and a good feeling of use can be obtained by using together at a specific ratio.

  Accordingly, the present invention provides (A) 1.0-4.0% by mass of protein hydrolyzate derived from soybean or wheat, (B) zinc chloride, zinc nitrate, zinc sulfate, zinc acetate, zinc lactate, zinc gluconate And 0.5 to 2.0% by mass of a water-soluble zinc compound selected from zinc citrate, and the mass ratio (A / B) of the component (A) to the component (B) is 1.5 to 2.0. An oral composition is provided.

  The oral composition of the present invention is an excellent tartar by blending protein hydrolyzate derived from soybean or wheat containing a large amount of acidic amino acids such as glutamic acid and aspartic acid with a specific water-soluble zinc compound at a specific ratio. It has a formation-inhibiting effect and a good feeling of use (improvement of feeling of strangeness such as a metallic taste derived from a zinc compound). In particular, even if the blending amount of the zinc compound is small, the combined use of these protein hydrolysates has both an excellent calculus formation inhibitory effect and a good feeling of use.

  Hereinafter, the present invention will be described in more detail. The oral composition of the present invention contains (A) a protein hydrolyzate derived from soybeans or wheat and (B) a specific water-soluble zinc compound. It is a feature.

  The protein hydrolyzate of component (A) used in the present invention preferably contains a large amount of acidic amino acids such as glutamic acid and aspartic acid, and is derived from soybean or wheat containing a large amount of these acidic amino acids. Protein hydrolysates are used.

The protein hydrolyzate used in the present invention can be obtained by subjecting the raw material soybean or wheat to decomposition treatment using an acid or alkali, an enzyme, an oxidizing / reducing agent and the like.
Specifically, in the decomposition treatment with an acid, a dilute acid (an inorganic acid such as hydrochloric acid, phosphoric acid or sulfuric acid or an organic acid such as acetic acid or citric acid) is heated to about 60 to 120 ° C. and treated for 10 minutes or more. preferable.
The decomposition treatment with alkali is preferably performed by heating a dilute alkali solution (inorganic alkaline agent such as sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate) to about 60 to 180 ° C. for 10 minutes or more.
The enzymatic decomposition treatment is performed in an enzyme solution having protease activity (for example, an enzyme such as pepsin or papain), and is preferably performed at about 10 to 60 ° C. for 10 minutes or more at each optimum pH.
The decomposition treatment with the redox agent is preferably performed at a temperature of about 10 to 100 ° C. for 10 minutes or more in a diluted solution of the redox agent. As the redox agent, compounds such as sulfite, hydrogen peroxide, hypochlorite, ersorbitan, and hydrazine can be used.
The above decomposition treatment methods may be performed alone or in combination of two or more.
The protein hydrolyzate derived from soybean or wheat thus obtained is preferably used after purification (desalting, deodorizing, decolorizing, etc.). The obtained protein hydrolyzate contains molecules (amino acids, amino acid oligomers, peptides) having various molecular weights depending on the degradation conditions and purification conditions.

  Furthermore, the number average molecular weight of these protein hydrolysates is preferably in the range of 300 to 4,000. A more preferable range is 500 to 2,000. When the number average molecular weight is less than 300, it exists in a state where about two amino acids are bonded, the adsorptive power to the tooth surface is relatively small, and the effect of inhibiting calculus formation may be insufficient, and 5,000 When it exceeds, steric hindrance becomes remarkable in the molecular structure, and as a result, the adsorptive power also decreases and the calculus formation inhibitory effect may also decrease.

The number average molecular weight of these protein hydrolysates is calculated by the following formula based on the total nitrogen amount in the molecule, the amino acid nitrogen amount, and the average molecular weight of the constituent amino acids.
In the following formula, the average molecular weight of the constituent amino acids is obtained by multiplying the abundance ratio (%) of constituent amino acids determined by ordinary amino acid analysis by the molecular weight of each amino acid, and the total nitrogen amount is the value of the general test method for cosmetic raw material standards. The first nitrogen determination method or gas chromatography (GC), and the amount of amino nitrogen can be measured by a formol titration method.

As such a protein hydrolyzate derived from soybean or wheat, there is a product of Seiwa Kasei Co., Ltd. as an industrially available product. These protein hydrolysates derived from soybean or wheat are particularly preferably used in the present invention because acidic amino acids such as glutamic acid and aspartic acid account for about 40% of all amino acids. Incidentally, protein hydrolysates other than these (for example, collagen (rich in glycine, proline and hydroxyproline) and silk (rich in glycine, alanine and serine)) do not contain such a high concentration of acidic amino acids.
For example, as a protein hydrolyzate derived from wheat, trade name: Promois WG (number average molecular weight: 700), or as a protein hydrolyzate derived from soybean, trade name: Promois WS and WS-H (number average molecular weight: 700). It can be suitably used. All of these products are available as 25% aqueous solutions. In addition, even if it is not a product of the company, any protein hydrolyzate derived from soybean or wheat and having similar characteristics can be used in the present invention. Moreover, these protein hydrolysates derived from soybean or wheat may be used alone or in combination of two or more.

  (A) The amount of protein hydrolyzate of soybean or wheat (in terms of pure content) is 1.0 to 4.0% (mass%, the same applies hereinafter) of the whole composition, and particularly 2.0 to 3 0.0% is preferable. If the blending amount is less than 1.0%, no significant improvement in the effectiveness (calculus formation inhibitory effect) of the zinc compound is observed. Moreover, even if it exceeds 4.0%, the improvement of the calculus formation inhibitory effect tends to be saturated, and the unique taste derived from the protein hydrolyzate becomes too strong.

  In the present invention, a water-soluble zinc compound is blended as the component (B). Here, as a zinc compound, it supplies free zinc ions in the composition and can be used as long as it has no harmful effect on the living body and is water-soluble, but is hardly soluble in water (for example, zinc oxide). In addition, those that form a strong complex (for example, fatty acid zinc such as stearyl acid), and those that themselves have strong irritation (for example, phenol zinc sulfate) cannot be used. As the component (B) of the present invention, water-soluble inorganic and organic acid compounds are preferable from the viewpoint that the blending amount can be reduced. Zinc chloride, zinc nitrate, and zinc sulfate are used as inorganic salts, and zinc acetate and zinc lactate are used as organic acid zinc. Zinc gluconate and zinc citrate are used (both manufactured by Wako Pure Chemical Industries, Ltd.). Among these, zinc chloride is preferably used as the inorganic salt, and zinc acetate, zinc lactate, zinc gluconate, and zinc citrate are preferably used as the organic acid zinc because of the feeling of use such as compoundability and taste in the preparation. Zinc, zinc citrate, zinc lactate and zinc gluconate are preferred. In addition, these water-soluble inorganic or organic acid zinc compounds may be used individually by 1 type, or may be used in combination of 2 or more types arbitrarily.

  (B) The compounding quantity of a water-soluble zinc compound is 0.5 to 2.0% of the whole composition, and 0.5 to 1.5% is especially preferable. When the compounding amount of the zinc compound is less than 0.5%, the effectiveness (calculus formation inhibitory effect) is remarkable even when the protein hydrolyzate of the component (A) is compounded twice or more with respect to the compounding amount of the water-soluble zinc compound. However, when the compounding amount exceeds 2.0%, the effectiveness is satisfactory, but a large amount (compounding amount exceeding 4.0%) of protein can be obtained. Even if a hydrolyzate is blended, no further improvement in the feeling of use is observed.

  Furthermore, in the present invention, (A) the amount of protein hydrolyzate derived from soybean or wheat (in terms of pure content) and (B) the proportion of water-soluble zinc compound (A / B) are 1. 5 to 2.0. If the blending ratio is less than 1.5, the effect of adding the protein hydrolyzate to the effectiveness of the zinc compound is insufficient, and the feeling of use is not sufficiently improved. If it exceeds 2.0, the effect of adding the protein hydrolyzate to the effectiveness of the zinc compound tends to be saturated, and the unique taste derived from the protein hydrolyzate becomes too strong.

  The composition for oral cavity of the present invention is prepared in various forms such as toothpaste, toothpaste, toothpaste such as liquid toothpaste, mouthwash, mouth freshener, gargle tablet, denture cleaner, troche, chewing gum and the like. Each composition can be prepared by an ordinary method according to the characteristics, using other optional components in addition to the above essential components within a range not impairing the effects of the present invention.

  As the optional component, a proper component corresponding to the type of oral composition is used. For example, abrasives, binders, thickeners, sweeteners, preservatives, fragrances, colorants, pH adjusters, excipients, various medicinal ingredients, and the like can be blended.

  In this case, for example, silica-based abrasives such as silicic anhydride, aluminum hydroxide, aluminum oxide, aluminosilicate, dicalcium phosphate, insoluble sodium metaphosphate, insoluble potassium metaphosphate, titanium oxide, synthetic resin, etc. are required as the abrasive. It is preferably used depending on. These abrasives may be used alone or in combination of two or more (the amount is usually 3 to 90% of the total composition).

  Examples of the surfactant include water-soluble salts of higher alkyl sulfates having 8 to 18 carbon atoms in the alkyl group, such as sodium lauryl sulfate and sodium myristyl sulfate, sodium lauryl monoglyceride sulfonate, sodium coconut monoglyceride sulfonate, and the like. Water-soluble salts of higher fatty acid monoglyceride sulfonic acids having 10 to 18 carbon atoms of fatty acid groups, olefin sulfonic acids, paraffin sulfonic acids and other anionic activators, stearyl monoglycerides, sucrose mono and dilaurate, etc. Sucrose fatty acid ester, lactose fatty acid ester, lactitol fatty acid ester, maltitol fatty acid ester, stearic acid monoglyceride, polyoxyethylene sorbitan monora having a number of 12 to 18 Nonionic activators such as rate, polyoxyethylene hydrogenated castor oil, sorbitan monostearate condensate added with about 60 mol of ethylene glycol, polymer of ethylene oxide and propylene oxide, and derivatives such as polyoxyethylene polyoxypropylene monolauryl ester , Surfactants such as amphoteric surfactants such as betaine type and amino acid type are used (usually 0.01 to 7% of the total composition).

  Examples of binders include carrageenan, sodium carboxymethylcellulose, methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, cellulose derivatives such as sodium carboxymethylhydroxyethylcellulose, alkali metal alginate such as sodium alginate, propylene glycol alginate, xanthan gum, tragacanth gum, caraya gum, arabic 1 such as gums such as gums, synthetic binders such as polyvinyl alcohol, sodium polyacrylate, carboxyvinyl polymer, polyvinylpyrrolidone, gelling silica, gelling aluminum silica, bee gum, laponite, etc. A seed | species or 2 or more types may be mix | blended (The compounding quantity is 0.5 to 10% of the whole composition normally).

  As the thickener, one or more of sorbitol, glycerin, ethylene glycol, propylene glycol, 1,3-butylene glycol, polyethylene glycol, polypropylene glycol, xylit, maltite, lactit and the like can be blended (ordinary amount of blending) 1-50%).

  In addition, sodium saccharin, stepioside, xylitol, neohesperidyl dihydrochalcone, glycyrrhizin, perilartine, thaumatin, aspartylphenylalanine methyl ester, p-methoxycinnamic aldehyde, sodium cyclamate, etc. as a sweetener, p-hydroxymethylbenzoic as a preservative Acid, p-hydroxyethyl benzoic acid, p-hydroxypropyl benzoic acid, p-hydroxybutyl benzoic acid, sodium benzoate, lower fatty acid monoglyceride and the like, winter green oil, spearmint oil, peppermint oil, sassafras oil, Clove oil, eucalyptus oil, etc. may be blended.

  Gelatin, peptone, albumin, brightener, silicone, pigment, and other components can be blended. Furthermore, fluorides such as sodium fluoride, sodium monofluorophosphate, tin fluoride, epsilon aminocaproic acid, tranexamic acid, dextranase, protease, mutanase, lysozyme, lytic enzyme, lytechenzyme, chlorhexidine salts, One or more active ingredients such as dihydrocholesterol, glycyrrhetin salts, glycyrrhetinic acid, caropeptide, vitamins, antibacterial agents, and hyposensitivity agents such as potassium nitrate can be blended.

  The pH of the composition for oral cavity of the present invention is not particularly limited as long as it is in a range that does not cause safety problems in the oral cavity and the human body, but is preferably pH 6-9, more preferably 7-9. is there. If necessary, acetic acid, hydrochloric acid, sulfuric acid, nitric acid, citric acid, phosphoric acid, sodium hydroxide, potassium hydroxide, sodium acetate, sodium carbonate, sodium citrate, sodium hydrogen citrate, phosphorus An appropriate amount of sodium acid, sodium hydrogen phosphate, or the like can be blended.

  EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In addition, all the compounding quantity (%) of each component in each example is a mass percentage.

Examples and comparative examples
Dentifrices and mouthwashes having the compositions shown in Tables 1 to 3 were prepared by the following methods and evaluated by the following tests. The results are shown in Tables 1-3.

(1) Preparation of dentifrice (Examples 1-12, Comparative Examples 1-12)
A phase A was prepared by mixing and dissolving water-soluble components (protein hydrolyzate, water-soluble zinc compound, sodium fluoride, sodium monofluorophosphate, sodium saccharin, xylitol, glycerin, 70% sorbit, etc.) at room temperature in purified water. .

The protein hydrolyzate in the examples is derived from wheat (trade name: Promois WG, number average molecular weight: 700) or derived from soybean (trade name: Promois WS, number average molecular weight: 700, product name: WS-H, number average molecular weight: 700) was used. The number average molecular weights of these protein hydrolysates were measured using the first nitrogen determination method of the cosmetic raw material standard general test method for the total nitrogen content and the formol titration method for the amino nitrogen content, and the above formula ([ Formula 1]). On the other hand, as a comparative component, a product in which soy protein is not hydrolyzed (Fuji Oil Co., Ltd., New Fuji Pro E; soy protein powder “91.2% purity”), and a peptide having a low content of acidic amino acids Examples of silk peptides (Neutral amino acids such as glycine, alanine, and serine account for about 80% of all amino acids: Seiwa Kasei Co., Ltd. Promois-Silk 1000P, number average molecular weight about 1,000), and number average Silk powder having a molecular weight of 5,000 (silk powder FD from Kanebo Co., Ltd.) was used. The amino acid mixture was prepared from commercially available reagents) (consisting of 10% glutamic acid as acidic amino acid, 10% aspartic acid, and 80% glycine as neutral amino acid (total 100%)).
Moreover, zinc oxide and zinc stearylate (both manufactured by Wako Pure Chemical Industries, Ltd.) that hardly dissolve in water were used as comparative components of the zinc compound.

  Next, a B phase was prepared by dissolving and dispersing oil-soluble components such as triclosan, isopropylmethylphenol and sodium carboxymethylcellulose in propylene glycol at room temperature. Next, B phase was added and mixed in A phase under stirring, and C phase was prepared. In Phase C, a fragrance, an abrasive such as silicic acid anhydride, and other components (sodium lauryl sulfate, etc.) are added, mixed at room temperature using a 1.5 L kneader (manufactured by Ishiyama Kogakusho), and decompressed to 4 kPa After defoaming, 1.0 kg of a dentifrice was obtained.

(2) Preparation of mouthwash (Examples 13 to 15)
A specified amount of purified water is put into a stainless steel container equipped with a three-one motor and a stirrer with rotating blades, and water-soluble components (protein hydrolyzate, water-soluble zinc compound, sodium fluoride, monofluoro) among the blended components. Sodium phosphate, sodium saccharin, xylitol, glycerin, etc.) were added and dissolved with stirring. At the same time, a specified amount of an organic solvent such as ethanol was charged into another stainless steel container equipped with a three-one motor and a stirrer having rotating blades, and the oil-soluble component among the blended components was charged and dissolved. Further, the above oil-soluble component was added to a container in which the water-soluble component was dissolved, and the mixture was stirred for 1 to 30 minutes to obtain a mouthwash as a uniform solution.

(3) Test method Zinc chloride is known as a water-soluble zinc compound that has been reported to be effective in clinical trials for the effects of calculus-preventing dentifrices (compound concentration: about 2%). In that case, it is necessary to improve the usability as a real problem. Therefore, in the examples of the present invention, the effect was tested with a formulation in which the amount used in the dentifrice or mouthwash was reduced to improve the feeling of use. Caused. In order to reinforce the reduction in this effect, a certain amount of protein hydrolyzate derived from soybeans or wheat was blended with this formulation, and a dentifrice was formulated with the composition shown in Table 1 (Examples). In addition, a comparative example is a composition as shown in Table 2.
The composition of the mouthwash is as shown in Table 3.

  About each dentifrice and mouthwash, the tartar formation inhibitory effect and usability were evaluated by the method shown below. The evaluation was compared with the case of dentifrice I having the following composition containing 2% zinc chloride. In the case of a mouthwash, since it is rarely diluted with saliva during use like a dentifrice, a mouthwash I having the following composition with a zinc chloride concentration of 1.0% was prepared. This was evaluated by comparison with this.

Composition of dentifrice I containing 2% zinc chloride:
Zinc chloride 2.0%
Silicic anhydride 20.0
Propylene glycol 3.0
Sodium carboxymethylcellulose 2.0
Glycerin 30.0
Xylitol 8.0
Sodium lauryl sulfate 1.0
Saccharin sodium 0.02
Fragrance 0.8
Triclosan 0.3
Isopropylmethylphenol 0.1
Sodium fluoride 0.2
Purified water balance
Total 100.0%
pH 7.5 (adjusted with hydrochloric acid or sodium hydroxide)

Composition of mouthwash I containing 1.0% zinc chloride:
Zinc chloride 1.0%
Glycerin 10.0
Xylitol 3.0
Ethanol 8.0
Saccharin sodium 0.1
Citric acid 0.01
Sodium citrate 0.3
Fragrance 0.3
Triclosan 0.15
Isopropylmethylphenol 0.1
Sodium monofluorophosphate 0.2
Purified water balance
Total 100.0%
pH 7.5 (adjusted with hydrochloric acid or sodium hydroxide)

Evaluation of calculus formation inhibitory effect Instead of human enamel, bovine enamel having similar properties was used. The bovine enamel was polished with sandpaper (# 1,500) to give a glossy flat surface, which was coated with nail polish except for an area of 1 × 1 mm, and this was used as a test sample. The evaluation target dentifrices (Examples and Comparative Examples) were each diluted twice with distilled water, and the test sample was immersed in the slurry for 3 minutes. The test sample was lightly washed with water to remove excess slurry, and immersed in an artificial plaque solution (2 mL) (37 ° C., 24 hours). In the case of the mouthwash, the test sample was immersed in the mouthwash for 1 minute without diluting with distilled water. In order to remove the excess mouthwash solution, the test sample was lightly washed and immersed in an artificial plaque solution (2 mL) (37 ° C., 24 hours). A calculus-like substance (complex of various calcium phosphates) is formed by the binding of calcium ions and phosphate ions contained in this artificial plaque solution, and is deposited on the surface of bovine enamel. At this time, the formation of tartar-like substances is suppressed by the active ingredients contained in the dentifrice or mouthwash to be evaluated.

The artificial plaque solution used here was prepared by referring to the literature (Journal Dental research 67 (12): 1468-1475, 1988) (artificial plaque solution: CaCl ₂ = 4.1 mM, KH ₂ PO ₄ = 15.5 mM). Acetic acid = 100 mM, NaCl = 100 mM, pH 6.35: 1 adjusted with 1N aqueous sodium hydroxide solution, all reagents are manufactured by Wako Pure Chemical Industries, Ltd.

  The effect of suppressing the formation of calculus-like substances was performed by an electron microscope observation method. That is, after 24 hours, a test sample was taken out from the artificial plaque solution, sufficiently washed and dried, and then gold deposition was performed on the sample surface. When this was observed with an electron microscope, it was recognized that the sample surface was covered with acicular calcium phosphate crystals.

  Note that the coverage was obtained by analyzing an electron microscope image of the obtained formed article using a general-purpose image analyzer. Specifically, in the electron microscope image, an area where deposits are present appears black, and an area where no deposits are present appears whitish. A threshold (brightness) for classifying the difference between the areas was set, and the entire observation area was binarized. And the ratio of the area | region which the deposit occupies with respect to the whole observation area | region was made into coverage (%). The value of a coverage here is an average value when three test samples are used for each dentifrice and mouthwash. This covering degree was evaluated by the following four evaluation points.

Effectiveness evaluation point Coverage (%)
4 to 24
3 25-49
2 50-74
1 75-100

  That is, when the coverage is 75 to 100%, the evaluation score is 1 point (no effect or little), 2 for the coverage of 50 to 74%, and 3 for the coverage of 25 to 49%. The case of 0 to 24% coverage was taken as 4 points. In addition, the degree of coating when treated with the above-described dentifrice compounded with 2.0% zinc chloride (however, in the case of mouthwash, 1.0% compounded in consideration of 2-fold dilution with dentifrice). Since it was a point, the case of an evaluation point higher than this was made into the standard of this invention.

They were allowed to use each dentifrice to a healthy person of feeling five people. About 1 g of a dentifrice was taken on a toothbrush portion of a normal toothbrush and brushed for 3 minutes, and then rinsed three times with about 10 mL of tap water, and the feeling of use was written on the entry form.
The evaluation criteria for use feeling is that the use feeling when brushed with Dentifrice I containing 2.0% of the above-mentioned zinc chloride is 1 point (strongly feels uncomfortable feeling such as zinc-derived metal taste), and also contains zinc chloride 3 points (feeling no metallic taste) when brushed with a normal dentifrice that is not applied, and 2 points (not feeling very slightly) in the middle, 2 points and 3 points of evaluation Was the standard of the present invention, and the average value (rounded integer value) of five persons was calculated. In addition, when a lot of silk peptides are blended (over 4.0%), the unique taste derived from the same component becomes strong, and even if there is no problem in the feeling of use derived from zinc, there is a problem in the feeling of use as a whole. Even when judged, the evaluation score was 1 point (see the following evaluation criteria).

  In the case of a mouthwash, it was carried out according to the case of a dentifrice, but the amount of mouthwash used was 5 mL, the mouthwash time was 1 minute, and the mouth rinse was lightly performed once. And the usability | use_condition at the time of mouthwashing with the said mouthwash I containing 1.0% of said zinc chloride was made into 1 point, and it evaluated similarly to the case of said dentifrice.

Usability evaluation criteria:
Evaluation point Discomfort of zinc-derived metal taste, etc. Unique taste derived from silk peptide Relevance 3 Not felt at all Not felt at all 2 Feeling at a very low level Feeling at a slight level Both at 1 Feeling strongly Feeling strongly Both or Which
Applicable to either

Comprehensive evaluation Two evaluations of calculus formation inhibitory effect and usability were comprehensively evaluated according to the following criteria.
Evaluation criteria for comprehensive evaluation:
◎ When effectiveness is 4 points and usability rating is 3 points ○ When effectiveness and usability rating are both 3 points
Or when the effectiveness is 4 points and the usability evaluation score is 2 points × When the effectiveness reference point (3 points) and the usability reference point (2 points) are not satisfied at the same time

* 1; Promois WG (Seiwa Kasei Co., Ltd., using 25% aqueous solution (the amount shown in the table indicates the amount converted to pure content))
* 2: Promois WS (Seiwa Kasei Co., Ltd., using a 25% aqueous solution (the amount shown in the table indicates the amount converted to pure content))
* 3: Promois SH (Seiwa Kasei Co., Ltd., using a 25% aqueous solution (the amount shown in the table indicates the amount converted to pure content))

* 1; Promois WG (Seiwa Kasei Co., Ltd .: 25% aqueous solution is used (the amount in the table indicates the amount in terms of pure content))
* 4: New Fuji Pro E (Fuji Oil Product: Unhydrolyzed soy protein)
* 5: Promois-Silk 1000P (Seiwa Kasei Co., Ltd .: Protein hydrolyzate with low content of acidic amino acids and mainly neutral amino acids such as glycine)
* 6; Silk powder FD (Kanebo Co., Ltd .: number average molecular weight is 5,000)
* 7: Amino acid mixture (prepared from commercially available reagents) (consisting of 10% glutamic acid as acidic amino acid, 10% aspartic acid, 80% glycine as neutral amino acid (total 100%))

* 1; Promois WG (Seiwa Kasei Co., Ltd., 25% aqueous solution is used (the amount in the table indicates the amount in terms of pure content))
* 2: Promois WS (Seiwa Kasei Co., Ltd., using a 25% aqueous solution)
* 3: Promois SH (Seiwa Kasei Co., Ltd., using a 25% aqueous solution (the amount shown in the table indicates the amount converted to pure content))

Claims (1)

  (A) 1.0 to 4.0% by mass of protein hydrolyzate derived from soybean or wheat, (B) selected from zinc chloride, zinc nitrate, zinc sulfate, zinc acetate, zinc lactate, zinc gluconate and zinc citrate The water-soluble zinc compound is contained in an amount of 0.5 to 2.0% by mass, and the mass ratio (A / B) of the component (A) to the component (B) is 1.5 to 2.0. Oral composition.