JP2006001901A - Dentifrice composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a dentifrice composition excellent in gloss of preparation and having good shape-retaining property and dispersibility during use. <P>SOLUTION: The dentifrice composition is obtained by formulating a dentifrice composition containing (A) a fluorine compound and (B) a calcium hydrogen phosphate dihydrate with (C) 5-30 mass% humectant, (D) 0.1-3 mass% carboxymethylcellulose sodium having 2.0-2.8 etherification degree and (E) 0.5-5 mass % thickening silica. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a dentifrice composition which is excellent in gloss of a preparation, has good shape retention and good dispersibility during use.

  Conventionally, a fluorine compound is blended in many dentifrices as an anti-corrosive active ingredient of a dentifrice composition. In addition, calcium hydrogen phosphate dihydrate is widely used as an abrasive for dentifrice because of its excellent cleaning power and feeling of cleaning.

  However, a dentifrice containing a fluorine compound and calcium hydrogen phosphate dihydrate has a problem that the surface of the preparation is not glossy and is aesthetically inferior.

  On the other hand, carboxymethyl cellulose is frequently used as a binder for dentifrices and is used in various dentifrices. Carboxymethylcellulose is used in a composition intended to prevent periodontal disease and improve treatment, improve antifoaming and storage stability, reduce bitterness and bad aftertaste, etc. together with fluorine compounds and calcium hydrogenphosphate dihydrate. However, these techniques do not improve the gloss of the preparation surface.

  In general, carboxymethyl cellulose is produced by introducing a carboxymethyl group into the hydroxyl group of the cellulose. By changing the degree of substitution (the degree of etherification), carboxymethyl cellulose having various characteristics is produced. Is done.

  However, conventionally, the degree of etherification of carboxymethylcellulose is generally 0.5 to 1.5, and the production of carboxymethylcellulose having an etherification degree outside this range has been theoretically possible. It was actually difficult and was not commercialized.

  In recent years, with the development of science and technology, it has become possible to produce carboxymethylcellulose with a high degree of etherification, and its formulation has been studied. Patent Document 5 uses this technique to create a dentifrice blended with microfibrillated cellulose. It is described that the use of a carboxymethylcellulose alkali salt having a degree of etherification of 2.0 or more in the composition improves skin gloss and shape retention when the dentifrice is pushed out of the container. However, this is an effect when used in combination with microfibrillated cellulose, and there is no description regarding a composition containing a fluorine compound and calcium hydrogen phosphate dihydrate.

  As described above, although the usefulness of the fluorine compound and calcium hydrogen phosphate dihydrate in the oral cavity in the dentifrice is clear, the preparation containing the fluorine compound and calcium hydrogen phosphate dihydrate Has the disadvantage that it has no gloss on the surface and is aesthetically inferior, and no means has been found so far to improve the gloss of such preparations. Furthermore, in this case, in the dentifrice used by many people, the gloss of the appearance is improved, and at the same time, when the dentifrice is pushed out on the toothbrush, the dentifrice does not fall off and has excellent shape retention. A dentifrice with good dispersibility during use is desired.

JP 2001-302476 A JP-A-8-325126 JP 60-48919 A JP 2001-89339 A JP-A-4-134024

  This invention is made | formed in view of the said situation, and it aims at providing the dentifrice composition which is excellent in the gloss of a formulation, and has good shape retention property and the dispersibility in use.

  As a result of intensive studies to achieve the above object, the present inventor has obtained a dentifrice composition containing (A) a fluorine compound and (B) calcium hydrogen phosphate dihydrate, and (C) a wetting agent and , (D) carboxymethyl cellulose having an etherification degree of 2.0 to 2.8 or an alkali metal salt thereof, and (E) a thickening silica in combination at a specific ratio, whereby a fluorine compound and calcium hydrogen phosphate 2 The present inventors have found that a dentifrice composition with improved shape retention and good dispersibility during use can be obtained by improving the gloss of a dentifrice composition containing a hydrate. It was.

  Accordingly, the present invention provides a dentifrice composition containing (A) a fluorine compound and (B) calcium hydrogen phosphate dihydrate, (C) 5-30% by mass of a wetting agent, and (D) etherification. Dentifrice comprising 0.1 to 3% by mass of carboxymethylcellulose having a degree of 2.0 to 2.8 or alkali metal salt thereof and 0.5 to 5% by mass of (E) thickening silica An agent composition is provided.

  ADVANTAGE OF THE INVENTION According to this invention, it can provide the dentifrice composition which is excellent in the gloss of a formulation, has good shape retention property, and good dispersibility in use, and contains a fluorine compound and calcium hydrogenphosphate dihydrate. The dentifrice composition can be widely used as a toothpaste.

  Hereinafter, the present invention will be described in more detail. The dentifrice composition of the present invention can be prepared as a toothpaste and contains (A) a fluorine compound and (B) calcium hydrogen phosphate dihydrate. , (C) a wetting agent, (D) carboxymethyl cellulose having an etherification degree of 2.0 to 2.8 or an alkali metal salt thereof, and (E) a thickening silica.

Examples of the fluorine compound used here include sodium fluoride, potassium fluoride, stannous fluoride, strontium fluoride, sodium monofluorophosphate, and the like, and one or more of these are used.

  The blending amount of the fluorine compound with respect to the entire dentifrice composition is 0.1 to 0.3% (mass%, the same applies hereinafter) in the case of sodium fluoride, and 0.3 to 1.0% in the case of sodium monofluorophosphate. Usually, about 1000 ppm is blended as fluorine in Japan.

  Next, as calcium hydrogen phosphate dihydrate, an average particle size usually used in a dentifrice is 10 to 50 μm and a liquid absorption amount of 0.5 to 0.9 mL / 2 g can be blended. Specifically, Tosoh Finechem Co., Ltd .: Dentifrice calcium phosphate dihydrate, Rhodia Corporation: Victor DF, etc. are mentioned.

  The blending amount of the calcium hydrogen phosphate dihydrate is preferably 21 to 60%, particularly 25 to 60%, particularly 35 to 50% of the whole dentifrice composition. If the blending amount is less than 21%, the shape retention may be inferior, and if it exceeds 60%, the gloss of the preparation may be inferior.

  In the present invention, examples of the wetting agent include sorbit, glycerin, propylene glycol, polyethylene glycol having an average molecular weight of 400 to 4000, xylit, malt, lactit and the like, and one or more of these are used. Of these, sorbite, propylene glycol, and xylite are particularly preferable.

  The blending amount of these wetting agents is 5 to 30% of the whole composition in terms of pure content, and is particularly preferably 15 to 20%. When the blending amount is less than 5%, the dentifrice surface gloss is exhibited. If it exceeds 30%, the dispersibility when using the dentifrice is impaired.

  Furthermore, in the present invention, examples of carboxymethylcellulose or alkali metal salts thereof include carboxymethylcellulose, sodium carboxymethylcellulose, and the like, and the degree of etherification is 2.0 to 2.8, preferably 2.2 to 2.5. A range is used. In the present invention, by using carboxymethyl cellulose having such a specific degree of etherification or an alkali metal salt thereof, it is possible to make the surface of the dentifrice excellent in gloss, shape retention, etc. When the degree of conversion is less than 2.0, the gloss of the surface of the dentifrice is not satisfactorily exhibited, and when it exceeds 2.8, the shape retention of the dentifrice is not maintained, and when the dentifrice is pushed out to the toothbrush, the dentifrice is dentifrice. There is a risk of the agent dripping down.

  The blending amount of carboxymethyl cellulose having the specific degree of etherification or the alkali metal salt thereof is 0.1 to 3%, preferably 0.2 to 2%, particularly preferably 0.2 to 1% of the whole composition. is there. If the blending amount is less than 0.1%, gloss of the dentifrice surface is not exhibited, and if it exceeds 3%, dispersibility when using the dentifrice is impaired.

Further, as the thickening silica, the specific surface area according to the BET method is 100 to 300 m ² / g, particularly 150 to ²⁰⁰ m ² / g, the liquid absorption is ² to 3 mL / g, particularly 2.1 to 2.7 mL / g. Those obtained by a known production method such as igneous silica and precipitated silica can be used.

  The blending amount of the thickening silica is 0.5 to 5% of the entire composition, preferably 1 to 4%, particularly preferably 2 to 3%, and the blending amount is less than 0.5%. Dentifrice becomes inferior in shape retention, and if it exceeds 5%, gloss of the dentifrice is not satisfactorily exhibited.

  The dentifrice composition of the present invention can contain other additives as optional components in addition to the above essential components, depending on the dosage form, and can be blended as long as the effects of the present invention are not hindered. It can be manufactured by the method.

  In the case of toothpaste, for example, calcium hydrogen phosphate dihydrate, abrasive other than silica, binder other than carboxymethyl cellulose having an etherification degree of 2.0 to 2.8 or an alkali metal salt thereof, interface Activators, fragrances, sweeteners, preservatives, various active ingredients other than the above fluorine compounds, colorants, and the like can be blended, and these ingredients can be mixed with water.

As abrasives, silica-based abrasives such as silica gel, aluminosilicate, zirconosilicate, calcium hydrogen phosphate anhydrate, calcium pyrophosphate, calcium carbonate, aluminum hydroxide, alumina, magnesium carbonate, tribasic magnesium phosphate, zeolite , Zirconium silicate, tricalcium phosphate, hydroxyapatite, quaternary calcium phosphate, synthetic resin-based abrasive and the like.
When mix | blending these other abrasive | polishing agents, it is preferable that the compounding quantity shall be 2 to 20% of the whole dentifrice composition, especially 10 to 15%.

As binder, cellulose derivatives such as sodium carboxymethyl cellulose having a degree of etherification of less than 2.0, hydroxyethyl cellulose, carrageenan, guar gum, sodium alginate, cationized cellulose, montmorillonite, gelatin, sodium polyacrylate, polyvinyl alcohol, polyvinylpyrrolidone , Tragacanth gum, karaya gum, bee gum, xanthan gum and the like.
When these other binders are blended, the blending amount can be a normal amount as long as the effects of the present invention are not hindered, but it is 0.1 to 2% of the entire dentifrice composition, particularly 0. 3 to 1% is preferable.

As the surfactant, an anionic surfactant, a nonionic surfactant, a cationic surfactant, and an amphoteric surfactant can be blended. Anionic surfactants include sodium alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate, sodium N-acyl sarcosine such as sodium N-lauroyl sarcosine, sodium N-myristoyl sarcosine, sodium dodecylbenzenesulfonate, hydrogenated coconut fatty acid Sodium monoglyceride monosulfate, sodium lauryl sulfoacetate, N-acyl glutamate such as sodium N-palmitoyl glutamate, sodium N-methyl-N-acyl taurate, sodium N-methyl-N-acylalanine, sodium α-olefin sulfonate, etc. Is mentioned. Nonionic surfactants include sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, fatty acid esters such as sucrose fatty acid esters, glycerin fatty acid esters, polyglycerin fatty acid esters, polyoxyethylene glycerin fatty acid esters, polyethylene glycol fatty acid esters. Such as polyhydric alcohol fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene polyoxypropylene copolymer, polyoxyethylene alkylphenyl ether, polyoxyethylene hydrogenated castor oil, and other ether type activators, lauric acid diethanolamide, etc. And fatty acid alkanolamides. Examples of the cationic surfactant include alkyl ammonium and alkyl benzyl ammonium salts. Examples of amphoteric surfactants include betaine acetate, imidazolinium betaine, and lecithin.
The blending amount of these surfactants is preferably 0.1 to 3%, particularly 0.5 to 1.5% of the entire dentifrice composition.

  Examples of the sweetener include saccharin sodium, and examples of the preservative include paraoxybenzoic acid ester and sodium benzoate.

  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, coconut 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, menthol, etc. Carvone, anethole, cineol, methyl salicylate, synamic aldehyde, eugenol, 3-l-mentoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone, menthyl acetate, N-substituted paramentan 3-carboxamide, pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane 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.

  As various active ingredients, water-soluble phosphate compounds such as potassium phosphate and sodium salt of normal phosphate, glucanases such as dextranase and mutanase, allantoinchlorohydroxyaluminum, hinokitiol, ascorbic acid, lysozyme chloride, glycyrrhizic acid and salts thereof , Sodium chloride, tranexamic acid, epsilon aminocaproic acid, dl-tocopherol acetate, α-bisabolol, isopropylmethylphenol, chlorohexidine salts, cetylpyridinium chloride, azulene, glycyrrhetinic acid, copper chlorophyllin sodium, copper glucophilin, copper gluconate, etc., aluminum lactate , Strontium chloride, potassium nitrate, berberine, hydroxamic acid and its derivatives, sodium tripolyphosphate, zeolite, amylase, methoxyethyl , Maleic anhydride copolymer, Polyvinylpyrrolidone, Epidihydrocholesterin, Benzethonium chloride, Dihydrocholesterol, Trichlorocarbanilide, Zinc citrate, Toki soft extract, Oat extract, Clove, Rosemary, Ogon, Safflower etc. Is mentioned. 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.

  As the colorant, Blue No. 1, Yellow No. 4, Green No. 3, titanium dioxide and the like can be blended in usual amounts.

  The material in particular of the container which accommodates the dentifrice composition of this invention is not restrict | limited, Usually, the container used for a dentifrice composition can be used. Specifically, plastic containers such as polyethylene, polypropylene, polyethylene terephthalate, and nylon can be used.

  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, the blending amount is mass%.

In addition, the average particle diameter of calcium hydrogenphosphate dihydrate and the thickening silica was measured using Nikkiso Microtrac particle size distribution measuring device Model 7995-10.
To measure the liquid absorption of calcium hydrogen phosphate dihydrate and thickening silica, weigh a certain amount of sample on a smooth glass plate and loosen it well with a spatula so that the liquid is evenly mixed. Glycerol (42.5%) is dropped, and finally the sample is collected in the center of the glass plate with a spatula, peeled off from the glass plate with a spatula, and the end point is the time when it can be removed cleanly, and the amount of glycerin required for the sample per weight It was set as the amount of liquid absorption.

Examples and comparative examples
Toothpaste compositions having the compositions shown in Tables 1 to 3 below were prepared by the following production method.
Manufacturing method:
(1) A phase was prepared by mixing and dissolving water-soluble components (excluding binder, propylene glycol, etc.) in purified water at room temperature.
(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 phase C, ingredients such as a fragrance, an abrasive, and a surfactant are mixed at room temperature using a 1.5 L kneader (manufactured by Ishiyama Institute), defoamed under reduced pressure, and dentifrice composition 1. 2 kg was obtained.
In addition, regarding the dentifrice composition which does not have propylene glycol in a composition, a binder was added and mixed with the A phase under stirring, and C phase was prepared.

  Regarding the dentifrice compositions shown in Tables 1 to 3, an appropriate amount was taken on a toothbrush by 10 subjects and observed, and the following criteria were used for the degree of gloss of the dentifrice surface, shape retention, and dispersibility during use. The sensory test by absolute evaluation was performed and average value was calculated. The results are shown in Tables 1-3.

Dentifrice surface gloss:
(Score) 3 points: There is gloss on the surface of the dentifrice.
2 points: There is a slight gloss on the surface of the dentifrice.
1 point: There is no gloss on the surface of the dentifrice.
(Evaluation criteria for gloss)
A: The average gloss of the dentifrice surface 2.0 points or more
○: Shine average point of dentifrice surface 1.5 points or more and less than 2.0 points
X: average gloss of dentifrice surface, less than 1.5 points

Shape retention:
(Score) 3 points: The shape of the paste is maintained on the toothbrush and does not fall off from the toothbrush
.
2 points: The shape of the paste on the toothbrush is slightly broken, but it falls off the toothbrush
No.
1 point: The shape of the paste collapses on the toothbrush and falls off the toothbrush.
(Evaluation criteria for shape retention)
◎: Average shape retention point of 2.0 points or more
○: Average shape retention point of 1.5 points or more and less than 2.0 points
×: Average shape retention point less than 1.5 points

Dispersibility in use:
About the toothpaste compositions shown in Tables 1-3, 10 subjects took 1 g of toothpaste (manufactured by Lion Corporation, Clinica Habrush 4-row head, medium), brushed for 5 seconds, and then extruded. The amount of the dentifrice remaining undissolved was subjected to a sensory test by relative evaluation according to the following criteria to obtain an average value.
(Score)
3 points: There is no undissolved residue.
2 points: Undissolved, but less than Comparative Example 3.
1 point: Compared with Comparative Example 3, there is an undissolved residue equal to or more than that.
(Dispersibility evaluation criteria in use)
A: Dispersibility average point in use 2.0 points or more
○: Dispersibility average point in use 1.5 points or more and less than 2.0 points
×: Dispersibility average point in use less than 1.5 points

In addition, the average particle diameter of calcium hydrogenphosphate dihydrate used in this test is 17.5 μm, the liquid absorption is 0.7 mL / 2 g, and the thickening silica has a BET specific surface area of 200 m ² / g. Precipitated silica having a liquid absorption amount of 2.2 mL / g was used.

  From the results in Tables 1 to 3, a dentifrice composition containing sodium monofluorophosphate and calcium hydrogen phosphate dihydrate, a wetting agent, carboxymethyl cellulose having a specific degree of etherification, and thickening silica in a specific ratio (implementation) Example) was found to have good gloss, shape retention, and dispersibility during use. On the other hand, when one of the essential requirements of the present invention is not satisfied (Comparative Example), the gloss of the dentifrice is inferior, the shape retention is poor, the dispersibility during use is inferior, and sufficient effects are obtained. It was proved that the object of the present invention could not be achieved.

Claims (1)

To a dentifrice composition containing (A) a fluorine compound and (B) calcium hydrogen phosphate dihydrate, (C) 5-30% by mass of a wetting agent, and (D) a degree of etherification of 2.0-2. A dentifrice composition comprising 0.1 to 3% by mass of .8 carboxymethylcellulose or an alkali metal salt thereof and 0.5 to 5% by mass of (E) thickening silica.