JP5891749B2 - Dentifrice composition - Google Patents

Description

  The present invention relates to a dentifrice composition that exhibits a high stain adhesion suppressing effect and stain removal effect, has low irritation to the oral mucosa, is excellent in use feeling such as taste and foaming, and has good storage stability.

Stain, a kind of colored stain on teeth, is formed by tannin pigments contained in coffee, tea, etc., oral proteins such as albumin, metal ions, and the like. Stain adhesion to the tooth surface is one of the major problems in oral aesthetics. As a means for solving the problem caused by the stain, it is effective to remove the stain or suppress the adhesion of the stain. Many dentifrice compositions have been proposed so far to solve the problem caused by stain.
The removal of the stain has been performed by the mechanical action of an abrasive compounded in the composition. However, it was inevitable that the abrasive mucosa, particularly the soft tooth neck, was worn by the abrasive.

Thus, various techniques for removing stains by chemical action have been proposed.
The applicant has so far proposed a composition that removes stains on the tooth surface by a chemical action, not by a mechanical action (Patent Document 1; JP-A-9-12438, Patent Document 2; JP-A-11). -343220, Patent Document 3; JP-A-2002-47161). In Patent Document 3, as a liquid dentifrice containing phenoxyethanol, which is a chemical cleaning base for tooth surfaces and tongue surfaces, 0.2% by mass of sodium N-lauroylglutamate and 0.1% by mass of sodium lauroylglycine in Example 4 were used. A composition containing 1.0% by mass of sodium lauryl sulfate, 4.0% by mass of tetrasodium pyrophosphate, 1.5% by mass of sodium tripolyphosphate, and 1.0% by mass of polyethylene glycol is described. However, this dentifrice cannot be said to have sufficient feeling of use such as irritation to the oral mucosa, foaming, and storage stability, and has room for improvement.

  On the other hand, acylamino acid salts have been proposed as a component that inhibits the formation of stains on teeth and has high safety and the same effect (Patent Document 4; JP-A-10-17444). In Patent Document 4, as Example 4, 0.6% by mass of sodium lauroyl-methyl-β-alanine, 1.0% by mass of sodium lauryl sulfate, 1.0% by mass of tetrasodium pyrophosphate, polyethylene glycol A toothpaste containing 5.0% by weight is described. However, this dentifrice has a problem in use feeling such as taste. Furthermore, liquid separation occurred and there was a problem in the storage stability of the preparation.

  In addition, it is known that acylamino acid salts have a peculiar taste (bitterness), and a composition in which bitterness is reduced by blending paratinite has been proposed (Patent Document 5; JP 2000-319148 A). ). However, this technique has not been enough to reduce bitterness.

Japanese Patent Laid-Open No. 9-12438 JP 11-343220 A JP 2002-471161 A Japanese Patent Laid-Open No. 10-17444 JP 2000-319148 A

As described above, the dentifrice composition effective for the adhesion of dental stains has been problematic in terms of irritation to the oral mucosa, feeling of use such as taste and foaming, and storage stability. Therefore, a new technique effective for the adhesion of dental stains has been desired.
The present invention has been made in view of the above circumstances, has a high stain adhesion inhibitory effect and a stain removal effect, is low irritation to the oral mucosa, is excellent in use feeling such as taste and foaming, and has a good storage stability. An object is to provide a dentifrice composition having the same.

As a result of intensive studies to achieve the above object, the present inventors have (A) acyl glutamate , (B) alkyl sulfate, (C) water-soluble polyphosphate, and (D). When blended with polyethylene glycol and the components (C) and (D) are in appropriate amounts, it has a high stain adhesion inhibiting effect and stain removal effect, and is less irritating to the oral mucosa and has a good taste. It was found that a dentifrice composition with a moderate amount of foaming, excellent usability, and good storage stability, especially when prepared as a toothpaste, which suppresses liquid separation and gives a stable appearance. .
Furthermore, in addition to components (A), (B), (C) and (D), (E) one or more water-soluble polymers selected from carrageenan, xanthan gum, sodium polyacrylate, and sodium hydroxyethylcellulose It has been found that, by blending, the foam retention is improved and the usability can be further improved.

In more detail, when the present inventors proceeded with studies to solve the above-mentioned problems, it is known that water-soluble polyphosphates and acylamino acid salts are effective against tooth stain adhesion. Even if the components (A) and (B) are blended, the stain adhesion inhibiting effect and the stain removing effect are inferior, and the bitterness derived from the component (A) is produced, resulting in inferior feeling in use, and the components (C) and (B ), The stain removal effect is inferior, the stain adhesion inhibiting effect is inferior, the oral mucosa is irritated, the foaming amount is low and the usability is inferior. Therefore, as a result of further studies to solve such problems, when the components (A), (B), (C) are combined and the component (D) is blended, all of the above problems are unexpectedly solved, and the stain is increased. The present inventors have found that it is excellent in adhesion suppressing effect and stain removal effect, is excellent in use feeling such as oral mucosal irritation, taste and foaming amount, and storage stability, and gives a special action effect. In this case, the combined use of the components (A), (B), (C), and (D) remarkably increases the stain adhesion suppressing effect, and cannot be obtained when any of the essential requirements of the present invention is lacking. A stain adhesion-inhibiting effect can be imparted, and by blending component (D), a unique taste derived from component (A) can be suppressed and a good feeling without bitterness can be imparted.
Thus, the combined use of the components (A), (B), (C) and (D) gives a preparation having a high stain removal effect and a stain adhesion suppressing effect, and having excellent usability and storage stability, The present inventors have newly found that the above-mentioned special effects are achieved.

Accordingly, the present invention provides the following dentifrice composition.
[1]
(A) one or two or more acyl glutamates selected from sodium N-lauroyl-L-glutamate, sodium N-myristoyl-L-glutamate and N-coconut oil fatty acid acyl-L-glutamate potassium ,
(B) alkyl sulfate,
(C) The following general formula (1)
M _{n + 2} P _n O _{3n + 1} (1)
(In the formula, M represents Na or K, and n is an integer of 2 or 3.)
And (D) polyethylene glycol having an average molecular weight of 200 to 6,000 , and the amount of component (A) is 0.1 to 2% by mass. The compounding amount of the component (B) is 0.3 to 1.8% by mass, the compounding amount of the component (C) is 0.3 to 1.5% by mass, and the compounding amount of the component (D) is 0.3 to 3%. The dentifrice composition characterized by being the mass%.
[2]
The dentifrice composition according to [1], wherein (B) / (C) is 0.5 to 3 as a mass ratio.
[3]
The dentifrice composition according to [1] or [2] , wherein the component (D) is polyethylene glycol having an average molecular weight of 380 to 3,800 .
[4]
And (E) 0.2 to 3% by mass of one or more water-soluble polymers selected from carrageenan, xanthan gum, sodium polyacrylate, and hydroxyethyl cellulose sodium [1], [2] Or the dentifrice composition as described in [3].
[5]
The dentifrice composition according to any one of [1] to [4], which is used for suppression of dental stain adhesion.

  According to the present invention, there is provided a dentifrice composition that exhibits a high stain adhesion suppressing effect and stain removal effect, is low irritation to the oral mucosa, has an excellent feeling of use such as taste and foaming, and has a good storage stability. Can be provided. Therefore, the dentifrice composition of the present invention is extremely effective for the adhesion of dental stains.

  The present invention will be described in further detail below. The dentifrice composition of the present invention comprises (A) an acyl amino acid salt, (B) an alkyl sulfate, (C) a water-soluble polyphosphate, and (D) polyethylene glycol.

  As the acyl amino acid salt of component (A), an acyl group having 8 to 20 carbon atoms, particularly 12 to 16 carbon atoms is preferable. Examples of the amino acid group include glutamic acid, aspartic acid, glycine, sarcosine, alanine, methionine, phenylalanine, leucine, and isoleucine, with glutamic acid being particularly preferred. Examples of the salt include alkali metal salts such as sodium and potassium, alkaline earth metal salts, and organic amine salts.

Examples of acyl amino acid salts include acyl glutamates such as sodium N-lauroyl-L-glutamate, sodium N-myristoyl-L-glutamate, potassium N-coconut fatty acid acyl-L-glutamate, and N-lauroyl-L-aspartic acid. Examples include acyl aspartates such as sodium, acyl glycine salts such as N-coconut oil fatty acid acyl glycine potassium, and the like. These may be used alone or in combination of two or more.
Specifically, Amino Surfact ALMS-P1 (N-lauroyl-L-glutamate sodium, Asahi Kasei Chemicals Corporation), Amisoft LS-11 (N-lauroyl-L-glutamate sodium, Ajinomoto Healthy Supply Co., Ltd.), Amino Surf Fact AMMS-P1 (N-myristoyl-L-glutamate sodium, Asahi Kasei Chemicals Corporation), Amisoft MS-11 (N-myristoyl-L-glutamate sodium, Ajinomoto Healthy Supply Co., Ltd.), Aminoformer FLDS-L (N- Products that have been commercialized under trade names such as Lauroyl-L-sodium aspartate, Asahi Kasei Chemicals Corporation), Amilite GCK-12K (N-coconut oil fatty acid acylglycine potassium, Ajinomoto Healthy Supply Co., Ltd.) You can use.

  As the component (A), acylglutamate is particularly suitable for giving the effects of the present invention because it has a different taste (bitterness) than those having other amino acid residues.

  The blending amount of the component (A) is preferably 0.1 to 2% (mass%, the same applies hereinafter) of the whole composition, more preferably 0.3 to 1.5%. If it is less than 0.1%, the stain adhesion inhibiting effect and foaming may be inferior.

Examples of the alkyl sulfate of component (B) include alkali metal salts of alkyl sulfates such as lauryl sulfate and myristyl sulfate, and one or more of them can be used. As the alkyl sulfate, sodium lauryl sulfate is particularly preferable because it can be easily incorporated into a dentifrice composition.
As the alkyl sulfate, commercially available products such as those manufactured by Toho Chemical Industry Co., Ltd. can be used.

  The blending amount of the component (B) is preferably 0.3 to 1.8%, more preferably 0.5 to 1.0% of the whole composition. If it is less than 0.3%, the stain adhesion inhibiting effect and the removing effect may be inferior, and foaming may be inferior. If it exceeds 1.8%, irritation to the oral mucosa may occur and the feeling of use may decrease.

As the water-soluble polyphosphate of component (C), the following general formula (1)
M _{n + 2} P _n O _{3n + 1} (1)
(In the formula, M represents Na or K, and n is an integer of 2 or 3.)
1 type or 2 types or more of the linear water-soluble polyphosphate represented by these are used.

For example, sodium pyrophosphate or potassium pyrophosphate having a polymerization degree n = 2, sodium tripolyphosphate having n = 3, or the like can be used. Among these, sodium tripolyphosphate is more preferable from the viewpoint of stain removal effect and irritation to the oral mucosa.
Specifically, commercially available products such as those manufactured by Taihei Chemical Industry Co., Ltd. can be used.

  The compounding quantity of a component (C) is 0.3 to 1.5% of the whole composition, Preferably it is 0.5 to 1.0%. If it is less than 0.3%, the stain adhesion suppressing effect and the stain removing effect are inferior, and if it exceeds 1.5%, irritation to the oral mucosa occurs and the feeling of use decreases. Moreover, foaming falls and it is inferior to storage stability.

In the present invention, it is more effective to mix the component (B) and the component (C) at an appropriate ratio, particularly to suppress irritation to the oral mucosa and to exert a high stain adhesion suppression and removal effect.
The blending ratio of the component (B) and the component (C) is preferably (B) / (C) as a mass ratio of 0.3 to 5, more preferably 0.5 to 3. If it is less than 0.3, stimulation may not be suppressed. Moreover, liquid separation stability may be inferior. If it exceeds 5, the mucosal irritation is strong and the feeling of use may be lowered, and the stain adhesion suppression and removal effects may be inferior.

  In the present invention, by further blending (D) polyethylene glycol, the effect of inhibiting the adhesion of stain due to the combined use of components (A), (B) and (C) is further improved, and the acylamino acid salt of component (A) It is possible to suppress the nasty taste derived from it and improve the feeling of use.

As the polyethylene glycol, those having a large average molecular weight are more effective for effect expression, but those having an average molecular weight of 200 to 6,000 are preferable, and those having an average molecular weight of 400 to 4,000 are particularly preferable. If it is less than 200, the effect which suppresses the unique taste derived from a component (A) may not fully be acquired. If it exceeds 6,000, a taste derived from polyethylene glycol is produced, and the usability may be deteriorated.
In addition, an average molecular weight shows the average molecular weight of quasi-drug material raw material specification 2006 here (hereinafter, the same).
Specific examples include polyethylene glycol 400 (average molecular weight 380 to 420), polyethylene glycol 600 (average molecular weight 570 to 630), polyethylene glycol 4000 (average molecular weight 2,600 to 3,800), and the like.
As the polyethylene glycol, for example, a commercially available product manufactured by Sanyo Chemical Industries, Ltd. can be used.

  The compounding amount of component (D) is preferably 0.3 to 3% of the total composition, more preferably 0.5 to 2%. If it is less than 0.3%, the off-flavor may not be suppressed, and if it exceeds 3%, liquid separation may occur, resulting in poor formulation stability. In addition, an unusual taste derived from polyethylene glycol may be produced, resulting in poor use feeling.

In the present invention, it is preferable to further blend (E) a water-soluble polymer selected from carrageenan, xanthan gum, sodium polyacrylate, and sodium hydroxyethylcellulose. By mix | blending a component (E), the retainability of the foam | bubble in an oral cavity can be improved and a usability | use_condition can be improved more. In the present invention, the component (E) is particularly effective as the water-soluble polymer for the above effect, and even if a water-soluble polymer other than the component (E) is used, such an effect cannot be obtained.
As a component (E), 1 type (s) or 2 or more types of the said water-soluble polymer can be mix | blended. In particular, a combination of two or more types, particularly a combination of xanthan gum and carrageenan and / or sodium polyacrylate is more preferable because the foam retainability is increased and the feeling during use is further improved.
A commercially available thing can be used as a component (E).

  When mix | blending a component (E), 0.2 to 3% of the whole composition is preferable, and, as for the compounding quantity, More preferably, it is 0.4 to 1.5%. If it is less than 0.2%, the blending effect may not be obtained. If it exceeds 3%, the dentifrice composition becomes hard, the dispersibility in the oral cavity during tooth brushing decreases, foam does not easily form, and the feeling of use is reduced. May be inferior.

  The dentifrice composition of the present invention is particularly suitably prepared as a toothpaste. In this case, if necessary, known components other than the above components can be blended within a range not impeding the effects of the present invention. For example, abrasives, thickeners, binders, surfactants, sweeteners, preservatives, colorants, fragrances, various active ingredients, and the like are blended.

Examples of the abrasive include silica-based abrasives such as silica gel, precipitated silica, and aluminosilicate, dicalcium phosphate dihydrate and anhydrous, tertiary calcium phosphate, tertiary magnesium phosphate, tetrabasic calcium phosphate, calcium pyrophosphate, etc. Examples thereof include calcium phosphate compounds, calcium carbonate, aluminum hydroxide, alumina, magnesium carbonate, zirconium silicate, hydroxyapatite, and synthetic resin abrasives.
The blending amount of these abrasives is usually 10 to 50%, preferably 10 to 30% of the entire composition.

  Examples of the thickener include sugar alcohols such as sorbit and xylit, and polyhydric alcohols such as glycerin and propylene glycol. These compounding amounts are usually 5 to 50%, particularly 20 to 45%.

  As a binder, you may mix | blend well-known binders other than the water-soluble polymer of a component (E) in the range which does not prevent the effect of this invention. For example, polyvinyl alcohol, guar gum, sodium alginate, cationized cellulose, thickening silica, montmorillonite, gelatin, carboxymethylcellulose sodium and the like can be mentioned. When blending these binders, the blending amount is preferably in the range of 0.2 to 5% including the component (E).

As the surfactant, known surfactants such as anionic surfactants other than components (A) and (B), nonionic surfactants, and cationic surfactants can be blended. Specifically, examples of the anionic surfactant include N-acyl sarcosine sodium such as N-lauroyl sarcosine sodium and N-myristoyl sarcosine sodium. Nonionic surfactants include sugar fatty acid esters such as sucrose fatty acid ester, maltose fatty acid ester and lactose fatty acid ester, sugar alcohol fatty acid esters such as maltitol fatty acid ester and lactitol fatty acid ester, polyoxyethylene sorbitan monolaurate, poly Polyoxyethylene sorbitan fatty acid ester such as oxyethylene sorbitan monostearate, polyoxyethylene fatty acid ester such as polyoxyethylene hydrogenated castor oil, lauric acid mono- or diethanolamide, sorbitan fatty acid ester, polyoxyethylene higher alcohol ether, polyoxyethylene Polyoxypropylene copolymers, polyoxyethylene polyoxypropylene fatty acid esters, and the like are used. Examples of the cationic surfactant include alkyl ammonium.
The blending amount of these surfactants is preferably 1 to 5%, particularly 1.5 to 4%, including the components (A) and (B).

Examples of the sweetener include saccharin sodium, and examples of the preservative include paraoxybenzoic acid ester and sodium benzoate.
Examples of the colorant include blue No. 1, yellow No. 4, titanium dioxide and the like.

  Perfumes include peppermint oil, spearmint oil, anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, Lime oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, grapefruit oil, sweetie Natural fragrances such as oil, bran oil, Iris concrete, absolute peppermint, absolute rose, orange flower, and processing of these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder Perfumes, etc.) and menthol, Rubon, Anethole, Cineol, Methyl salicylate, Synamic aldehyde, Eugenol, 3-1-Mentoxypropane-1,2-diol, Thymol, Linalol, Linarel acetate, Limonene, Menthone, Menthyl acetate, N-Substituted paramenthane 3-carboxamide, pinene, octyl aldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allylcyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, Hexanal, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cycloten, furfural, trimethylpyrazine, ethyl lactate, ethyl Oral compositions such as single flavors such as o-acetate, and other flavors such as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mix flavor, tropical fruit flavor, etc. It can be used in combination with known perfume materials used in the above.

  Various active ingredients include fluorides such as sodium fluoride and sodium monofluorophosphate, water-soluble phosphate compounds such as potassium salt and sodium salt of orthophosphate, glucanases such as dextranase and mutanase, and allantochlorhydroxyaluminum. , Hinokitiol, ascorbic acid, lysozyme chloride, glycyrrhizic acid and its salts, sodium chloride, tranexamic acid, epsilon aminocaproic acid, acetic acid dl-tocophenol, α-bisabolol, isopropylmethylphenol, chlorohexidine salts, cetylpyridinium chloride, azulene, glycyrrhetinic acid , Copper compounds such as copper chlorophyllin sodium, copper gluconate, aluminum lactate, strontium chloride, potassium nitrate, berberine, hydroxamic acid and its derivatives, zeo Ito, amylase, methoxyethylene, maleic anhydride copolymer, polyvinylpyrrolidone, epidihydrocholesterin, benzethonium chloride, dihydrocholesterol, trichlorocarbanilide, zinc citrate, sweet cherry extract, buckwheat extract, clove, rosemary, ougone And extracts such as safflower. In addition, the said active ingredient can be mix | blended in an effective amount in the range which does not prevent the effect of this invention.

  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 the following examples, “%” means “% by mass” unless otherwise specified.

[Examples and Comparative Examples]
Dentifrice compositions (toothpastes) having the compositions shown in Tables 1 to 4 were prepared by the following method and evaluated as follows. The results are shown in Tables 1-4.

Preparation of test dentifrice composition:
(1) Water-soluble components (excluding binder, propylene glycol, etc.) were mixed and dissolved in purified water at room temperature, and sorbite and thickening silica were added and mixed to prepare phase A.
(2) A phase B in which a binder was dispersed at room temperature in propylene glycol was prepared.
(3) B phase was added and mixed in A phase under stirring, and C phase was prepared.
(4) In the C phase, ingredients other than water-soluble ingredients such as fragrances, abrasives, and surfactants are mixed at room temperature using a 1.5 L kneader (manufactured by Ishiyama Institute) and defoamed under reduced pressure (4 kPa). To obtain 1.2 kg of a dentifrice composition.

Details of the raw materials used are as follows.
(A) sodium N-lauroyl-L-glutamate;
Asahi Kasei Chemicals Corporation (trade name: Amino Surfact ALMS-P1)
N-lauroyl-L-sodium aspartate;
Asahi Kasei Chemicals Corporation (trade name: Aminoformer FLDS-L)
N-coconut oil fatty acid-cocoyl glycine potassium;
Ajinomoto Healthy Supply Co., Ltd. (trade name: Amilite GCK-12K)
(B) Sodium lauryl sulfate; Toho Chemical Industry Co., Ltd. (C) Sodium tripolyphosphate; Taihei Chemical Industry Co., Ltd. Tetrasodium pyrophosphate; Taihei Chemical Industry Co., Ltd. (D) PEG400; Polyethylene glycol 400, Sanyo Chemical Industries Co., Ltd. PEG4000; Polyethylene glycol 4000, Sanyo Kasei Kogyo Co., Ltd. (E) Carrageenan; Sansho Co., Ltd. Sodium polyacrylate; Toa Gosei Co., Ltd. Hydroxyethylcellulose sodium; Daicel Chemical Industries, Ltd. Xanthan gum; DSP Gokyo Food & Chemical Co., Ltd. Used was quasi-drug material standard compliant.

<1> Evaluation of Stain Adhesion Suppression Effect <1-1> Stain Adhesion Inhibition Test After treatment with a sandblast of an untreated hydroxyapatite pellet (HAP) surface (made by HOYA, diameter 7 mm × thickness 3.5 mm), It was cleaned with an ultrasonic cleaner in a neutral detergent solution. After washing with water and natural drying, the ΔE value (ΔE0) of HAP before the adhesion of stain was measured using a spectroscopic color difference meter (manufactured by Nippon Denshoku Industries Co., Ltd., model: SE-2000).
Moreover, the dentifrice composition was diluted with twice the amount of purified water, and a supernatant was obtained by centrifugation at 3,000 rpm for 10 minutes to obtain a dentifrice dispersion. The HAP is immersed in a dentifrice dispersion heated to 50 ° C. for 10 minutes, washed with purified water to remove surface moisture, then 0.5% albumin solution → tannin extract → 0.6% quencher. An operation of repeatedly immersing in an order of the iron (III) acid ammonium solution at 50 ° C. for 10 minutes each was performed. Tannin extract is made up of 1,200 mL of boiling ion-exchanged water, 50 g of Japanese tea (brand: Oimatsu), 5 bags of black tea (made by Unilever Japan Co., Ltd., Brisk tea bag), instant coffee (trade name Nescafe, Nestlé Japan Co., Ltd.) (Made by company) 12g was added and allowed to stand overnight, and Japanese tea and black tea were removed by filtration. The above operation was repeated 5 times, the HAP surface was air-dried, and the ΔE value (ΔE1) of the surface was measured again.
Instead of the dentifrice dispersion, ΔE of the initial HAP when the same treatment was performed with purified water was ΔE0b, and ΔE after the treatment was ΔE1b. The stain adhesion inhibition rate was calculated by the following formula.
Stain adhesion inhibition rate (%) =
[(ΔE1b−ΔE0b) − (ΔE1−ΔE0)] / (ΔE1b−ΔE0b) × 100

The stain adhesion inhibitory effect was evaluated from the stain adhesion inhibition rate according to the following criteria.
Evaluation criteria for stain adhesion inhibition effect ◎: Stain adhesion inhibition rate is 80% or more ○: Stain adhesion inhibition rate is 70% or more and less than 80% △: Stain adhesion inhibition rate is 60% or more and less than 70% ×: Stain adhesion inhibition rate is Less than 60%

<2> Evaluation of stain removal effect <2-1> Method for producing stain-attached HAP Hydroxyapatite pellet (HAP) surface (made by HOYA, diameter 7 mm × thickness 3.5 mm) is treated with sand blast, and then neutral Washed with an ultrasonic cleaner in an aqueous detergent solution. Etching the surface with a 30% aqueous phosphoric acid solution (10 minutes), washing with water, drying naturally, and then using a spectroscopic color difference meter (manufactured by Nippon Denshoku Industries Co., Ltd., model: SE-2000), HAP before stain adhesion The Lab value (L0) of was measured. For the above HAP, an operation of repeatedly dipping in an aqueous solution of 0.5% albumin → tannin extract → 0.6% aqueous solution of iron (III) ammonium citrate for 1 hour was repeated 50 times, and after air drying at room temperature for 1 day, Washed with running water and air-dried again to produce stain-attached HAP. The tannin extract was prepared in 1200 mL of boiling ion-exchanged water, 50 g of Japanese tea (brand name: Oimatsu), 5 bags of black tea (made by Unilever Japan Co., Ltd., Blis Teaback), instant coffee (trade name Nescafe, Nestlé) (Made by Nippon Co., Ltd.) 12 g was added and allowed to stand overnight, and Japanese tea and black tea were removed by filtration. The surface color of the produced stain-attached HAP was measured, and the value was defined as L1.

<2-2> Stain removal test The dentifrice composition was diluted with twice the amount of purified water to prepare a dentifrice dispersion. Stain-attached HAP produced by the above method is immersed in a dentifrice dispersion and an automatic polishing tester (Miyakawa Shoten Co., Ltd., weight 200 g, temperature 37 ° C.) set with a flat toothbrush (PC CLINICA, manufactured by Lion Corporation) The HAP Lab value (L2) after brushing was measured 200 times.
The stain removal rate was calculated based on the following formula.
Tannin iron stain removal rate (%) = [(L1-L2) / (L1-L0)] × 100
The stain removal effect was evaluated from the stain removal rate according to the following criteria.
Evaluation criteria for stain removal effect ◎: Stain removal rate of 50% or more ○: Stain removal rate of 40% or more and less than 50% △: Stain removal rate of 30% or more and less than 40% ×: Stain removal rate of less than 30%

<3> Evaluation of Dentifrice Foaming About 5 g of the dentifrice composition was diluted 4-fold with artificial saliva, and 10 mL of the aqueous solution was added to a 100 mL Epton tube. The mixture was shaken up and down 20 times per 10 seconds, the foam height after standing for 1 minute was measured, and the foaming of the dentifrice was evaluated according to the following criteria.
Evaluation standard of foaming ◎: 20 mm or more ○: 15 mm or more and less than 20 mm △: 10 mm or more and less than 15 mm ×: less than 10 mm

<4> Evaluation of irritation to oral mucosa Using 10 panelists sensitive to mucosal irritation, about 1 g of dentifrice composition on a toothbrush, and the degree of irritation to the oral mucosa when brushing for 3 minutes Got an answer. Among the answers, the average score of 10 people was 4 points for "I don't feel stimulation", 3 points for "I hardly feel stimulation", 2 points for "I feel stimulation", and 1 point for "I feel strong stimulation" The usability was evaluated according to the following criteria.
Evaluation criteria for stimuli ◎: Average score of 3.5 to 4.0 points ○: Average score of 3.0 to less than 3.5 points △: Average score of 2.0 to less than 3.0 points ×: Average score 1.0 to less than 2.0

<5> Bitter taste evaluation when brushing teeth Using 10 dental specialist panelists, about 1 g of the dentifrice composition was put on a toothbrush, brushed for about 3 minutes, and then answered in four stages regarding the degree of bitterness when brushing. Obtained. Among the answers, there were 4 points for "I feel no bitterness", 3 points for "I hardly feel bitterness", 2 points for "I feel slightly bitterness", and 1 point for "I feel very bitterness" The feeling of use was evaluated according to the following criteria from the average score.
Evaluation criteria for bitterness ◎: Average score of 3.5 to 4.0 points ○: Average score of 3.0 to less than 3.5 △: Average score of 2.0 to less than 3.0 ×: Average score 1.0 to less than 2.0

<6> Evaluation of Storage Stability of Formulation After storing three dentifrice compositions contained in a tube container at 40 ° C. for one month, liquid separation stability was determined according to the following scoring criteria. Evaluated by criteria.
Score standard for liquid separation 4 points: There was no liquid separation.
3 points: Slight liquid separation was recognized at the mouth (no problem level).
2 points: Liquid separation at the mouth part and the kneaded surface was slightly intense.
1 point: When the dentifrice composition is pushed out of the tube, the separated liquid drips from the mouth of the tube
It was recognized to the extent.
Evaluation criteria for storage stability ◎: 4.0 points ○: 3.0 points or more and less than 4.0 points △: 2.0 points or more and less than 3.0 points ×: Less than 2.0 points

<7> Evaluation of foam retention in the oral cavity Using 10 dental specialist panelists, about 1 g of the dentifrice composition was put on a toothbrush and brushed for about 3 minutes. About foam retention in the oral cavity, 4 I got an answer at the stage. Among the answers, the average of 10 people, 4 points for "No dripping from the mouth", 3 points for "Little from the mouth", 2 points for "Slightly dripping from the mouth", and 1 point for "Dropping from the mouth" From the point, the feeling of use was evaluated according to the following criteria.
Evaluation criteria for foam retention ◎: Average point of 3.5 points or more and 4.0 points or less ○: Average point of 3.0 points or more and less than 3.5 points △: Average point of 2.0 points or more and less than 3.0 points × : Average score of 1.0 or more and less than 2.0

Claims (5)

(A) one or two or more acyl glutamates selected from sodium N-lauroyl-L-glutamate, sodium N-myristoyl-L-glutamate and N-coconut oil fatty acid acyl-L-glutamate potassium ,
(B) alkyl sulfate,
(C) The following general formula (1)
M _{n + 2} P _n O _{3n + 1} (1)
(In the formula, M represents Na or K, and n is an integer of 2 or 3.)
And (D) polyethylene glycol having an average molecular weight of 200 to 6,000 , and the amount of component (A) is 0.1 to 2% by mass. The compounding amount of the component (B) is 0.3 to 1.8% by mass, the compounding amount of the component (C) is 0.3 to 1.5% by mass, and the compounding amount of the component (D) is 0.3 to 3%. The dentifrice composition characterized by being the mass%.   The dentifrice composition according to claim 1, wherein (B) / (C) is 0.5 to 3 as a mass ratio. The dentifrice composition according to claim 1 or 2, wherein component (D) is polyethylene glycol having an average molecular weight of 380 to 3,800. Further, (E) 0.2 to 3 mass% of one or more water-soluble polymers selected from carrageenan, xanthan gum, sodium polyacrylate, and sodium hydroxyethylcellulose are blended. The dentifrice composition described. The dentifrice composition according to any one of claims 1 to 4, which is used for suppressing stain adhesion of teeth.