JP4496429B2 - Dentifrice composition and dentifrice product - Google Patents

Description

  The present invention relates to a dentifrice composition containing vitamin E or a derivative thereof. More specifically, vitamin E or a derivative thereof is stably held in a container, has excellent appearance stability, and has sufficient foaming properties. The present invention relates to a dentifrice composition that is secured, easy to manufacture and tastes good. Moreover, this invention relates to the dentifrice product in which this dentifrice composition was accommodated in the specific container.

  Periodontal disease is counted as one of the major causes of tooth loss, and its prevention is expected to lead to an improvement in QOL (Quality of Life). Metabolic activation by promoting blood circulation is said to be effective in preventing periodontal diseases, and vitamin E or its derivatives, sodium chloride, herbal medicines, etc. are formulated in oral compositions including dentifrices and mouthwashes. ing. Among them, vitamin E or a derivative thereof is widely used because of its high effect. Since vitamin E or a derivative thereof is oil-soluble, it is widely used to solubilize using a surfactant when blended in a dentifrice.

  Vitamin E referred to in the present invention is α-tocopherol, β-tocopherol, γ-tocopherol, δ-tocopherol, or a mixture thereof. The vitamin E derivative of the present invention is a compound in which an ester group is introduced into the hydroxyl group of vitamin E, and representative examples include tocopherol acetate, tocopherol succinate, and tocopherol nicotinate.

  However, vitamin E or a derivative thereof has a problem in stably blending in the preparation, such as a decrease in the residual amount over time due to adsorption to the innermost layer of the container and a cause of discoloration of the preparation due to oxidative degradation.

  So far, various studies have been made to improve the stability of vitamin E or its derivatives. In particular, with regard to adsorption to a container, it has been found that when an anionic surfactant is added, adsorption to the container is promoted. For this reason, studies have been made to change the material of the container to various container materials (Patent Document 1: Japanese Patent Laid-Open No. 1-305021, Patent Document 2: Japanese Patent Laid-Open No. 2-69411). However, Patent Document 1 is a technique that uses a container having a specific acrylonitrile copolymer as the innermost layer. However, since the container becomes hard, there is a problem that it is difficult to squeeze out when the innermost layer is a tube. This technique uses a container in which the innermost layer of the trunk and shoulders is formed of high-density polyethylene, polypropylene, or low-density polyethylene crosslinked with metal, but there is a problem in terms of cost because a special container is used.

  In addition to the above, several techniques relating to containers have been proposed. For example, the applicant of the present invention proposes a technique for a packaging body in which a liquid oral cavity composition containing a fragrance is filled in a casting polypropylene container. (Patent Document 3: JP 2000-191485 A). Although the Example which uses tocopherol acetate and a polyoxyethylene (20) cetyl ether together is shown here, the stability of tocopherol acetate is not mentioned. Moreover, it does not contain an anionic surfactant, an abrasive, polyoxyethylene hydrogenated castor oil, and there is no description that the average added mole number of ethylene oxide of polyoxyethylene alkyl ether is 3-8. In addition, when the tube is made with casting polypropylene as the innermost layer, the tube becomes hard and there is a problem in usability. The technology described in this publication can adsorb vitamin E or its derivative in the dentifrice composition to the container. It is different from the technology to prevent.

  In terms of composition, a salt such as sodium bicarbonate (Patent Document 4: Japanese Patent Laid-Open No. 63-192712) or a salt of hydrochloric acid, sulfuric acid, carbonic acid, phosphoric acid, etc. (Patent Document 5: Japanese Patent Laid-Open No. 62-161715) It is known that the micelle structure of the anionic surfactant becomes rigid by blending, and the container adsorption of vitamin E or its derivative is suppressed. However, this technique has a problem that the binder that can be blended is limited to a salt-resistant one, and the flavor is restricted due to the metallic taste and bitterness of the salt. In addition, Patent Document 4 describes an example in which either one of polyoxyethylene nonylphenyl ether, an anionic surfactant, and a vitamin E derivative is blended. The polyoxyethylene alkyl ether and polyoxyethylene nonylphenyl ether used in the invention are different.

  An anionic surfactant is added in an amount of 0.3% or more, preferably 0.5 to 2.0% for oral cleaning, oral dispersibility of the preparation, and solubilization of oil-soluble components such as fragrances, vitamin E or derivatives thereof. Furthermore, a technique for blending polyoxyethylene hydrogenated castor oil has also been proposed (Patent Document 6: Japanese Patent Laid-Open No. 58-96012). According to this technique, the micelle structure of the anionic surfactant becomes rigid as in the case of addition of salt, and adsorption of vitamin E or its derivative to the container can be suppressed. However, since vitamin E or a derivative thereof has an oily taste, there is a problem that it is difficult to brush it for a long time and apply it to the oral mucosa.

  On the other hand, a technique has been proposed in which the innermost layer contains an oral composition containing dl-α-tocopherol acetate, sodium lauryl sulfate, anhydrous silica, and a polyoxyethylene polyoxypropylene copolymer in a synthetic resin container ( (Patent Document 7: Japanese Patent Laid-Open No. 10-139641) has a problem that foaming power is lowered when a polyoxyethylene polyoxypropylene copolymer and an anionic surfactant are used in combination. Furthermore, since the polyoxyethylene polyoxypropylene copolymer has poor solubility, it is liable to become lumps and it is difficult to produce a dentifrice.

  Also, a mouthwash technique using a combination of tocopherol acetate, polyoxyethylene (60) hydrogenated castor oil, and polyoxyethylene (8) tridecyl ether is known (see Patent Document 8: Japanese Patent Application Laid-Open No. 11-255629). However, this technique is intended to increase the permeability of cationic fungicides to microbial aggregates, and is not mentioned regarding the stability of tocopherol acetate, and the effects obtained from the examples are plaques. Only the promotion of bactericidal activity of cetylpyridinium chloride in the model bactericidal testing method is described. In addition, the dosage form is different from that of the present invention, which is a dentifrice composition containing an abrasive, and the chain length of the alkyl chain of the polyoxyethylene alkyl ether is different. Furthermore, since an anionic surfactant is not used in this technique, problems that occur when an anionic surfactant is used in combination with vitamin E and its derivatives do not occur in the first place.

  In addition, the present applicant has added vitamin E or a derivative thereof by blending an ascorbic acid phosphate salt with an oral composition containing vitamin E or a derivative thereof, an anionic surfactant and a nonionic surfactant. A technique for stabilizing and blending has been proposed (see Japanese Patent Application No. 2003-124644).

  In addition, the present applicant has applied a technique for filling a dentifrice composition containing vitamin E and a derivative thereof, polyoxyethylene hydrogenated castor oil, and an anionic surfactant into a container in which the innermost layer is formed of polyethylene (Japanese Patent Application). 2003-42816).

  Accordingly, a toothpaste that does not use a special container, does not impair the foaming property of the preparation, does not taste oily, has excellent appearance stability, is easy to manufacture, and can be stably formulated with vitamin E or its derivatives. Development of an agent composition has been demanded.

JP-A-1-305021 JP-A-2-69411 JP 2000-191485 A JP-A-63-192712 Japanese Patent Laid-Open No. 62-161715 JP 58-96012 A Japanese Patent Laid-Open No. 10-139641 JP-A-11-255629

  The present invention has been made in view of the above circumstances, and even after long-term storage, there is little adsorption of vitamin E or its derivative to the container, and vitamin E or its derivative is stably blended over a long period of time, and the effect is sustained. To provide a dentifrice composition that is exerted, has excellent appearance stability, has sufficient foaming power, is easy to manufacture, and has a good taste, and a dentifrice product that contains this dentifrice composition in a container. Objective.

The present inventors, upon diligent result of extensive investigations, formulating vitamin E or a derivative thereof and an anionic surfactant dentifrice compositions containing abrasive order to achieve the above object, (A) the number of carbon atoms 0.4 to 5.0% by mass of polyoxyethylene alkyl ether having an alkyl group of 14 to 18 and an average addition mole number of ethylene oxide of 3 to 8 and (B) an average addition mole number of ethylene oxide of 10 and 0.5 to 5 wt% polyoxyethylene hydrogenated castor oil is to 80, (a) component: (B) component 1: 9 to 9: was mixed and dispersed within an amount of 1 mass ratio with surfactant By blending as an active agent mixture , even after long-term storage, there is little adsorption of vitamin E or its derivative to the container, vitamin E or its derivative is stably blended, and its medicinal effect is exerted continuously. It was also found that a dentifrice composition having excellent appearance stability, high foaming power, easy production and good taste can be obtained.

  In addition, ensuring good foamability of the anionic surfactant and stabilization of vitamin E or its derivative in the dentifrice composition containing the abrasive in the present invention has an alkyl group having 14 to 18 carbon atoms. A mass of 1: 9 to 9: 1 of polyoxyethylene alkyl ether having an average added mole number of ethylene oxide of 3 to 8 and polyoxyethylene hydrogenated castor oil having an average added mole number of ethylene oxide of 10 to 80 It is presumed that the stability and orientation of the anionic surfactant was improved in the composite micelle of the surfactant mixture mixed and dispersed at a ratio, and according to the present invention, the above specific components are combined and blended. Can ensure the stability and foamability of the above-described excellent vitamin E or its derivative, and it has no oiliness, and vitamin E or its derivative and anionic field. The above object of the active agent dentifrice composition containing those can solve the.

Accordingly, the present invention provides a dentifrice composition containing vitamin E or a derivative thereof, an anionic surfactant, and an abrasive, (A) an average addition of ethylene oxide having an alkyl group having 14 to 18 carbon atoms. 0.4 to 5.0% by mass of polyoxyethylene alkyl ether having 3 to 8 moles and 0.5 to 0.5% of polyoxyethylene hydrogenated castor oil having an average added mole number of (B) ethylene oxide of 10 to 80 and 5 wt%, (a) component: (B) component at a mass ratio of 1: 9 to 9: dentifrice composition, characterized in that blended as a surfactant mixture was mixed and dispersed in 1 scope Offer things. Moreover, this invention provides the dentifrice product characterized by filling this dentifrice composition in the container whose container innermost layer consists of linear low density polyethylene.

  The dentifrice composition of the present invention has little appearance of vitamin E or a derivative thereof adsorbed on a container or the like even after long-term storage, the medicinal effect of vitamin E or a derivative thereof is continuously exerted, and is excellent in appearance stability and manufactured. Is easy and has good foaming properties and taste.

  As vitamin E or a derivative thereof blended in the dentifrice composition of the present invention, various vitamin E or a derivative thereof usually blended in a dentifrice composition, such as dl-α-tocopherol, dl-α-tocopherol acetate, And nicotinic acid dl-α-tocopherol, succinic acid dl-α-tocopherol and the like. In the present invention, among these, dl-α-tocopherol acetate is particularly preferred in that the color is colorless or pale yellow and hardly affects the color tone or appearance of the preparation. This dl-α-tocopherol acetate can be obtained from DSM Nutrition Japan Co., Ltd. under the trade name of tocopherol acetate, for example.

  The compounding amount of vitamin E or a derivative thereof is preferably 0.01 to 5.0% by mass, particularly 0.05 to 1.0% by mass based on the whole composition in terms of effectiveness and taste. If the blending amount is less than 0.01% by mass, sufficient pharmacological effects may not be exhibited. If the blending amount exceeds 5.0% by mass, it becomes difficult to solubilize in the preparation, causing problems in appearance stability, It may become inferior in terms of taste.

  As the anionic surfactant used in the present invention, those which are usually blended in a dentifrice composition can be used. Specifically, octyl sulfate, decyl sulfate, lauryl sulfate, myristyl sulfate, palmityl sulfate, and alkyl sulfates such as alkali metal salts such as sodium, potassium and lithium of stearyl sulfate, N-lauroyl sarcosine sodium, N-myristoyl sarcosine sodium Acyl sarcosine sodium, sodium dodecylbenzene sulfonate, hydrogenated coconut fatty acid sodium monoglyceride monosulfate, sodium lauryl sulfoacetate, sodium N-palmitoyl glutamate, N-acyl glutamate, N-methyl-N-acyl taurate sodium, N -Methyl-N-acylalanine sodium, sodium α-olefin sulfonate, sodium dioctyl sulfosuccinate, etc. can be used, especially alkyl sulfate in terms of taste and odor It is preferred to use, it is preferred to use sodium lauryl sulfate which is excellent in inter alia foaming. The blending amount of the anionic surfactant is preferably 0.1 to 5.0% by mass, more preferably 0.5 to 2.5% by mass with respect to the whole composition in terms of foamability and taste. is there. If the blending amount is less than 0.1% by mass, sufficient foaming properties may not be obtained, and if it exceeds 5.0% by mass, bitterness may occur or irritation to the oral mucosa may be strong and the feeling of use may be reduced. is there.

  The abrasive used in the present invention includes silica gel, precipitated silica, aluminosilicate, zirconosilicate, amorphous anhydrous silicic acid, dibasic calcium phosphate dihydrate, dibasic calcium phosphate anhydride, tricalcium phosphate, tetracalcium phosphate, 8 calcium phosphate, calcium pyrophosphate, aluminum hydroxide, alumina, insoluble calcium metaphosphate, light calcium carbonate, heavy calcium carbonate, magnesium carbonate, tertiary magnesium phosphate, zeolite, polymethyl methacrylate, nylon powder, silk powder, cellulose powder, And glucomannan. The blending amount is preferably 1 to 50% by mass, particularly 10 to 50% by mass in terms of the tooth cleaning effect. If the amount is less than 1% by mass, the tooth cleaning effect cannot be sufficiently obtained, and if it exceeds 50% by mass, the tooth cleaning effect may not be further improved.

As polyoxyethylene alkyl ether blended in the dentifrice composition of the present invention, the following formula (1)
R—O— (EO) _n H (1)
(However, R represents an alkyl group having 14 to 18 carbon atoms, n represents the average number of added moles of ethylene oxide (EO), and n is in the range of 3 to 8).
The one shown in is used. The polyoxyethylene alkyl ether has an alkyl group having 14 to 18 carbon atoms, preferably 16 to 18 carbon atoms. If the alkyl group has less than 14 carbon atoms, sufficient foaming properties cannot be obtained. When the number of carbons in the group exceeds 18, there is a problem that a unique taste and oiliness are generated during use of the dentifrice. Specific examples of such polyoxyethylene alkyl ether include polyoxyethylene cetyl ether, polyoxyethylene myristyl ether, polyoxyethylene stearyl ether, and the like, and polyoxyethylene stearyl ether is particularly preferable. Moreover, the average addition mole number of the ethylene oxide of the said polyoxyethylene alkyl ether is 3-8 mol, Preferably it is the range of 3-5 mol. If the average added mole number is lower than 3 moles, the release of liquid components occurs in the dentifrice formulation, and if it exceeds 8 moles, the characteristic oiliness and flavor will deteriorate and the feeling of use will be inferior. End up. The blending amount of the polyoxyethylene alkyl ether is preferably 0.4 to 5.0% by weight, particularly 0.6 to 2.5% by weight of the whole composition in terms of foamability and taste. If the amount is less than 0.4% by mass, the foaming property immediately after use tends to be suppressed, and if the blending amount exceeds 5.0% by mass, bitterness and peculiar stickiness occur, which causes a problem in the feeling of use. May occur. Examples of such polyoxyethylene alkyl ethers include Emulex 105, 107, 603, 605, and 608 of Nihon Emulsion Co., Ltd., NIKKOL BS-4 of Nikko Chemicals Co., Ltd., EMALGEN 1108 of Kao Co., Ltd., Aoki Yushi Kogyo Co., Ltd. ) BLAUNON CH-305, CH-308, SR-705, SR-707, etc. can be used.

  Next, in this invention, as polyoxyethylene hydrogenated castor oil, the average added mole number of ethylene oxide is 10-80, Preferably it uses 20-60. If the average number of added moles is less than 10 moles, roughening of the preparation at low temperatures occurs and the appearance deteriorates. If the average number of added moles exceeds 80 moles, vitamin E or a derivative thereof, an oil-soluble active ingredient, a fragrance ingredient, etc. The solubilizing ability of the lipophilic component is inferior and the lipophilic component is liberated. The blending amount of the polyoxyethylene hydrogenated castor oil is preferably 0.5 to 5% by mass, particularly 0.6 to 2% by mass, based on the stability and taste of vitamin E or its derivatives. It is. If the amount is too small, the stability of vitamin E or a derivative thereof may be lowered, and if it is too much, a unique bitter taste may be expressed, and a problem may occur in the feeling of use. Examples of such polyoxyethylene hydrogenated castor oil include NIKKOL HCO-10, HCO-20, HCO-30, HCO-40, HCO-50, HCO-60, HCO-80, Nihon Emulsion (Nikko Chemicals Co., Ltd.) Commercially available products such as HC-10, HC-20, HC-30, HC-40, HC-60, HC-80, BLAUNON RCW-20, 40, 60, 80 of Aoki Yushi Kogyo Co., Ltd. be able to.

  Furthermore, in this invention, the compounding ratio of said polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil shall be 1: 9-9: 1 by mass ratio, Especially the range of 3: 7-7: 3. It is desirable to mix and disperse in terms of appearance stability, foamability, taste, and production suitability. When the blending ratio of polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil is less than 1: 9, sufficient stability of vitamin E or a derivative thereof cannot be ensured, and when the blending ratio is greater than 9: 1, sufficient occurrence occurs. No foamability can be obtained.

  The dentifrice composition of the present invention comprises the above-mentioned vitamin E or a derivative thereof, an anionic surfactant, an abrasive, a polyoxyethylene alkyl ether having the above-mentioned specific carbon number and an average added mole number of ethylene oxide, and a specific ethylene oxide. Although the polyoxyethylene hydrogenated castor oil having an average added mole number is essential, in the present invention, the specific polyoxyethylene alkyl ether and the specific polyoxyethylene hydrogenated castor oil are mixed and dispersed in advance. It is preferable to prepare a surfactant mixture, and to prepare this surfactant mixture by a conventional method using vitamin E or a derivative thereof, an anionic surfactant, an abrasive, and other components. When polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil are blended without preparing the above surfactant mixture in advance, foaming properties are remarkably suppressed, insoluble ribs are generated in the preparation, and the appearance is deteriorated. There is a case. In particular, polyoxyethylene alkyl ether has a low melting point and is easily solidified at room temperature, so that it is easy to generate lumps. In addition, the mixture of the specific polyoxyethylene alkyl ether and the specific polyoxyethylene hydrogenated castor oil can be prepared as a uniform mixture by heating at 60 to 80 ° C., and can be stored as a waxy solid at room temperature. .

  The dentifrice composition of the present invention may contain other additives as optional components in addition to the above essential components. For example, wetting agents, binders, surfactants other than the above, sweeteners, preservatives, various active ingredients, pH adjusters, colorants, fragrances, etc. can be blended, and these ingredients and the above essential ingredients are mixed with water. Thus, a dentifrice composition can be produced.

  Examples of the wetting agent include glycerin, sorbitol, propylene glycol, polyethylene glycol having a molecular weight of 200 to 6000, 1,3-butylene glycol, xylitol, maltitol, lactitol, erythritol, palatinose, trehalose and other polyhydric alcohols, sugar alcohols, and the like. The blending amount is usually 1 to 50% by mass, particularly 1 to 40% by mass.

  Binders include xanthan gum, sodium polyacrylate, carrageenan, sodium alginate, propylene glycol alginate, carboxyvinyl polymer, tragacanth gum, guar gum, hydroxypropyl guar gum, tara gum, locust bean gum, karaya gum, quince seed gum, tamarind gum, carboxy Sodium methylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, cellulose, gellan gum, gelatin, curdlan, gum arabic, agar, pectin, sodium caseinate, polyvinyl alcohol, polyvinylpyrrolidone, pullulan, thickening silica, beegum, smectite , Laponite, montmorillonite, bentonai Etc. The. A compounding quantity is 0.1-5 mass% normally with respect to the whole composition.

  As the surfactant, a nonionic surfactant other than the specific polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil, a cationic surfactant, an amphoteric surfactant and the like are within the range not impeding the effects of the present invention. Can be added. For example, polyoxyethylene polyoxypropylene block copolymer, sucrose fatty acid ester, sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbit fatty acid ester, polyoxyethylene glycerin fatty acid ester, Nonionic such as polyoxyethylene lanolin, polyoxyethylene alkylamine and polyoxyethylene fatty acid amide, polyoxyethylene alkylphenyl formaldehyde condensate, polyoxyethylene polyoxypropylene alkyl ether, polyoxyethylene alkylphenyl ether and fatty acid alkanolamide Surfactant, alkyl ammonium, alkyl benzyl ammonium salt, etc. On surfactants, betaine, an amphoteric surfactant such as imidazolinium betaine. The compounding quantity of these other surfactant can be 0-5 mass% of the whole composition.

  Examples of the sweetening agent include saccharin sodium, stevioside, stevia extract, dipotassium glycyrrhizinate, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, perilartin, thaumatin, sucralose, acesulfame potassium, aspartame and the like.

  Examples of the preservative include parabens such as methyl paraben, butyl paraben, and ethyl paraben, benzoic acid and its salt, salicylic acid and its ester or salt, and the like.

  In addition to vitamin E or its derivatives, active ingredients include fluorides such as sodium fluoride, potassium fluoride, stannous fluoride, strontium fluoride, ammonium fluoride, sodium monofluorophosphate, triclosan, isopropylmethylphenol, Fungicides such as thymol, cetylpyridinium chloride, benzethonium chloride, benzalkonium chloride, decalinium chloride, chlorhexidine hydrochloride, chlorhexidine gluconate, dodecyldiaminoethylglycine, hinokitiol, phenol, antiplasmin agents such as tranexamic acid, epsilon aminocaproic acid, ascorbine Acids and their derivatives, riboflavin, pyridoxine hydrochloride, cyanocobalamin, β-carotene, ergocalciferol, vitamins such as menadione, ubiquinone, glycyl Citrates, glycyrrhetinic acid, allantoins, plant extracts such as buckwheat, auren, hornon, hamamelis, clove, chamomile, latania, myrrh, toki, rosemary, safflower, dextranase, mutanase, lysozyme, amylase, protease, Enzymes such as lytic enzymes, superoxide dismutase, sodium chloride, potassium nitrate, sodium polyphosphate, carbonates, bicarbonates, salts such as sesquicarbonate, γ-oryzanol, dihydrocholesterol, α-bisabolol, azulene, methoxyethylene, anhydrous Maleic acid copolymer, trichlorocarbanilide, alanine, glycine, proline, L-arginine, sodium L-aspartate, trimethylglycine, copper chlorophyllin sodium, copper gluconate, zinc chloride, cup Phosphate zinc, zeolite, water-soluble inorganic phosphoric acid compounds may be formulated with one or more aluminum lactate and the like. The amount of the active ingredient added can be an effective amount as long as the effects of the present invention are not hindered.

  Examples of pH adjusters include citric acid, malic acid, lactic acid, tartaric acid, succinic acid, acetic acid, phosphoric acid, pyrophosphoric acid, glycerophosphoric acid, various salts such as potassium salt, sodium salt and ammonium salt, sodium hydroxide, hydrochloric acid Etc. These can be blended alone or in combination of two or more so that the pH of the composition is in the range of 5-9. The compounding quantity is 0.01 to 2 mass% of the whole composition normally.

  As colorants, Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green No. 3 and other legal dyes, safflower dyes, gardenia dyes, cochineal dyes, anato dyes, bengara, mica titanium, titanium oxide and the like.

  In addition, as perfumes, 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, Iris concrete , Absolute Peppermint, Absolute Rose, Orange Flower, and other natural fragrances, and processed natural fragrances (front cut, rear cut, fractional distillation, liquid-liquid extraction, essence, powder fragrance, etc.) And menthol, carvone, anethole, cineole, sa Methyl tyrate, cinnamic aldehyde, eugenol, 3-l-mentoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone, menthyl acetate, N-substituted-paramentane-3-carboxamide, pinene , Octyl aldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, hexanal, ethyl alcohol, Propyl alcohol, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cycloten, furfural, trimethylpyrazine, ethyl lactate, ethyl Oral compositions such as single flavors such as thioacetate, 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. The well-known perfume material used for can be used, and it is not limited to the perfume of an Example.

  Although the container filled with the dentifrice composition of this invention is not specifically limited, It is preferable to fill the container which an innermost layer consists of a linear low density polyethylene. When a tube is used as a container, linear low density polyethylene, low density polyethylene, polypropylene, nylon, polyvinyl chloride, polyvinyl alcohol, polyacrylonitrile copolymer, etc. are mainly used for the innermost layer. Among these, linear low density polyethylene and low density polyethylene are widely used because of their high flexibility and excellent heat sealability. In particular, linear low-density polyethylene can be suitably used because of its excellent mechanical strength, heat resistance, and cold resistance, and excellent contamination adherence and sealability and high manufacturing suitability.

  As the container used in the present invention, for example, from the outer layer, low density polyethylene / ethylene / acrylic acid copolymer resin / aluminum / ethylene / acrylic acid copolymer resin / linear low density polyethylene (innermost layer), low Density polyethylene / ethylene / vinyl alcohol copolymer / low density polyethylene / ethylene / vinyl alcohol copolymer / linear low density polyethylene (innermost layer), and low density polyethylene / polyethylene terephthalate / low density polyethylene / glass vapor deposition Examples thereof include those having a laminate layer structure composed of polyethylene terephthalate / ethylene / methacrylic acid copolymer resin / linear low density polyethylene (innermost layer) and the like.

Linear low density polyethylene is also known as linear low density polyethylene (LLDPE). As a production method, in a high density polyethylene production process, an α-olefin (for example, butene-1, hexene-1,4-methyl) is added to a linear polymer. Penten and octene-1) are copolymerized, and short-chain branches are introduced to reduce the density. Linear low-density polyethylene for extrusion coating has a density of 0.915 to 0.938 g / cm ³ . Things are commonly used.

  The thickness of the linear low density polyethylene of the innermost layer is not particularly limited, but a thickness of about 25 to 100 μm is preferable from the viewpoint of heat sealability and stability of vitamin E or its derivative. The thickness of the entire laminate layer is usually 200 to 450 μm. If the thickness of the entire laminate layer is less than 200 μm, sufficient cushioning properties cannot be obtained when heat-sealing the tube, so that the heat seal portion is wrinkled, adhesion is incomplete, and the contents may leak. Yes, if it exceeds 450 μm, the tube becomes hard and difficult to squeeze out. Such a container can be obtained as a toothpaste tube from a container packaging material manufacturer such as Dai Nippon Printing Co., Ltd. or Toppan Printing Co., Ltd.

  EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to a following example. In addition, all% in each example is the mass%. The fragrance | flavor used the thing of the composition shown to Tables 4-10. Ethylene oxide was abbreviated as EO.

[Examples and Comparative Examples]
Dentifrice compositions having the compositions shown in Tables 1 to 3 below were prepared by deaeration and mixing using a kneader. The amount of the dentifrice composition charged was 5 kg. In the following examples, polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil were weighed in a predetermined amount in a 200 mL glass beaker, heated to 80 ° C. using a water bath, and mixed and dispersed. It was prepared by a conventional method using a surfactant mixture and other components. However, in Comparative Example 13, polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil were weighed in predetermined amounts, and individually melted by heating to 80 ° C. using a water bath. The obtained dentifrice composition was filled into a tube A or B, which will be described later, and the residual rate, appearance stability, foamability, taste, and production suitability of vitamin E or its derivatives were evaluated by the following methods. The results are shown in Tables 1-3.

Tube A (Dai Nippon Printing Co., Ltd.):
From the outermost layer, LDPE55 / PET12 / LDPE20 / white LDPE60 / EMAA20 / AL10 / EMAA30 / LDPE20 / LLDPE30, thickness 257 μm, diameter 26 mm, filling amount 50 g
Tube B (Dai Nippon Printing Co., Ltd.):
Outermost from LDPE80 / LDPE25 / PET12 / LDPE25 / White _{LDPE100 / SiO x -PET12 / EMAA25 /} LLDPE80, thickness 359μm, diameter 37 mm, filling amount 100g
A numerical value shows thickness (micrometer).
The abbreviations are as follows.
LDPE: Low-density polyethylene white LDPE: White low-density polyethylene LLDPE: Linear low-density polyethylene AL: Aluminum PET: Polyethylene terephthalate EMAA: Copolymer resin of ethylene / methacrylic acid SiO _x -PET: Glass-deposited polyethylene terephthalate

Stability of vitamin E or its derivatives:
Vitamin E or its derivative in the composition immediately after preparation is determined as the initial value (mass%), and vitamin E contained in the composition after accelerated deterioration in a thermostatic bath at 50 ° C. for one month or its Using the concentration of the derivative as an evaluation sample value (mass%), the residual ratio of vitamin E or its derivative was calculated by the following formula. For the determination of vitamin E or its derivative, take 2g of dentifrice (use the first 2g extruded from the tube), extract vitamin E or its derivative with methanol, then 14th revised Japanese Pharmacopoeia First It was carried out by the method specified in the section of “Tocopherol”, “Tocopherol acetate” or “Tocopherol nicotinate” in each section of certain pharmaceuticals.
Residual rate of vitamin E or its derivatives (%)
= [Evaluation Sample Value (mass%) / Initial Value (mass%)] × 100
Evaluation criteria for vitamin E or its derivatives are as follows.
◎: Residual rate of vitamin E or its derivative 95% or more ○: Residual rate of vitamin E or its derivative 90% or more and less than 95% △: Residual rate of vitamin E or its derivative 80% or more and less than 90% ×: Vitamin E or Residual rate of the derivative is less than 80%

Appearance stability:
After denaturing the dentifrice composition filled in the tube in a 50 ° C thermostatic bath for one month, it was extruded onto paper and observed for the presence or absence of liquid components, the presence or absence of rough skin, and the presence or absence of discoloration. Samples stored in a constant temperature bath were comprehensively evaluated as standard products.
The evaluation criteria for appearance stability are as follows.
◎: Good with little change from the standard product ○: Good with little change from the standard product △: Slightly different from the standard product, not very good ×: Remarkably different from the standard product, poor The

Foam and taste:
Using expert panelists (10 persons), 1 g of the dentifrice composition was taken into a commercially available toothbrush (Dentist system marion, regular, hair hardness = usually, manufactured by Lion Corporation), brushed for 1 minute, and dentifrice composition The foaming property and taste of the product were evaluated according to the following criteria, and the average values were taken as the evaluation results of foaming property and taste, respectively.
Foaming property 5: Suddenly foamed immediately after starting brushing
4: Sufficient foam was generated in about 10 seconds after starting brushing.
3: Foamed in about 20 seconds after starting brushing
2: Foamed in about 30 seconds after starting brushing
1: Sufficient foaming was not obtained even at the end of brushing. Taste: The composition of Comparative Example 1 had a 40% aqueous solution of 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine (NIKKOL AM- 101, Nikko Chemicals Co., Ltd.) 5.0% was added, and a dentifrice balanced with the amount of purified water was prepared and evaluated as a standard product.
5: There was no oiliness compared to the standard product, and it had a very good taste.
4: Compared to the standard product, there was almost no oiliness and the taste was good
3: Compared to the standard product, it was not very oily and tasted slightly better
2: Slightly less oily than the standard product, but the taste was not very good
1: At the same level as the standard product, it was oily and tasted unbearable

Manufacturability:
In the preparation of the dentifrice composition, a predetermined amount of polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil was weighed in a 200 mL glass beaker, heated to 80 ° C. using a water bath, and mixed and dispersed in a water bath. After being taken out from the above, it was left at 25 ° C., the time until solidification was measured, and evaluated according to the following criteria.
◎: After taking out from the water bath, it did not solidify after 2 minutes to 5 minutes ○: After taking out from the water bath, it solidified in 1 minute or more and less than 2 minutes △: After taking out from the water bath, 20 seconds or more Solidified in less than 1 minute ×: immediately solidified after removal from the water bath

＊１、＊２は個別配合

* 1, * 2 are individually formulated

  From the results of Tables 1 to 3, the dentifrice compositions of the present invention all show a high residual ratio of vitamin E or a derivative thereof, excellent appearance stability, good foaming properties and taste, and suitability for production. It turned out to be good. Further, as is clear from the comparative examples, the average addition mole number of ethylene oxide of polyoxyethylene cetyl ether is 2, the average addition mole number of ethylene oxide of polyoxyethylene stearyl ether is 11, polyoxyethylene alkyl When ether has an alkyl group with 12 carbon atoms, polyoxyethylene hydrogenated castor oil has an average addition mole number of ethylene oxide of 5 or 100, and myristic acid diethanolamide, vitamin E or its derivatives The stability, foamability, appearance stability, good taste, and production suitability were not sufficiently ensured. Polyoxyethylene alkyl ether having an alkyl group having 14 to 18 carbon atoms and having an average addition mole number of ethylene oxide of 3 to 8 and polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 10 to 80 Even when blended, when each is used alone or when the mass ratio is outside the range of 1: 9 to 9: 1, the stability, foamability and appearance stability of vitamin E or its derivatives It did not satisfy all of the properties, taste, and production suitability. Also, when polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil are added separately, lumps are produced during production, and the stability, foamability, appearance stability, good taste, and production of vitamin E or its derivatives Aptitude was not sufficiently secured. Similar results were obtained even when the fragrances B, C, D, E, F, G, H, and I were used in place of the fragrance A.

  Furthermore, when a dentifrice composition having the following composition was prepared and evaluated, all of the dentifrice compositions were excellent in stability of vitamin E or its derivatives, excellent in appearance stability, good in foaming properties, and tasted. It was good and had good manufacturing aptitude. During production, polyoxyethylene alkyl ether and polyoxyethylene hydrogenated castor oil were weighed in predetermined amounts, heated to 80 ° C. using a water bath, and mixed and dispersed.

[Example 9] Toothpaste propylene glycol 5.0% by mass
70% sorbite solution 40.0
Xanthan gum 0.5
Carrageenan 0.5
Saccharin sodium 0.2
Sodium lauryl sulfate 1.2
(NIKKOL SLS, manufactured by Nikko Chemicals)
Polyoxyethylene stearyl ether (EO average addition mole number 5) 1.4
(BLAUNON SR-705, manufactured by Aoki Yushi Kogyo)
Polyoxyethylene hydrogenated castor oil (EO average added mole number 40) 1.4
(HC-40, manufactured by Nippon Emulsion)
Ascorbic acid-2-magnesium phosphate 0.2
Tocopherol nicotinate 0.1
(Vitamin E Nicotinate, made by BASF Takeda Vitamin)
Sodium hydroxide 0.1
Silicic anhydride 25.0
Titanium oxide 1.0
Cetylpyridinium chloride 0.05
Fragrance A 0.9
Purified water remaining
Total 100.0% by mass
Housed in tube A.

The evaluation results are as follows.
Stability of tocopherol nicotinate ◎
Appearance stability ◎
Foaming 5
Taste 5
Manufacturability ◎
Similar results were obtained even when the fragrances B, C, D, E, F, G, H, and I were used in place of the fragrance A. Similar results were obtained when tube B was used instead of tube A.

[Example 10] Toothpaste propylene glycol 3.0% by mass
70% sorbite solution 20.0
Dibasic calcium hydrogen phosphate dihydrate 40.0
Thickening silica 3.0
Sodium carboxymethylcellulose 1.2
Carrageenan 0.4
Sodium myristyl sulfate 1.5
(NIKKOL SMS, manufactured by Nikko Chemicals)
Polyoxyethylene stearyl ether (EO average addition mole number 3) 1.2
(EMALEX603, manufactured by Nippon Emulsion)
Polyoxyethylene hydrogenated castor oil (EO average added mole number 20) 1.2
(HC-20, manufactured by Nippon Emulsion)
Saccharin sodium 0.2
Titanium oxide 0.3
Fragrance B 1.0
Dl-α-tocopherol acetate 0.1
(Tocopherol acetate, manufactured by DSM Nutrition Japan)
Triclosan 0.1
ε-aminocaproic acid 0.03
Sodium monofluorophosphate 0.7
Isopropylmethylphenol 0.1
Methyl paraoxybenzoate 0.1
Purified water remaining
Total 100.0% by mass
Housed in tube A.

The evaluation results are as follows.
Stability of tocopherol acetate ○
Appearance stability ○
Foaming 5
Taste 5
Manufacturability ◎
Similar results were obtained even when the fragrances A, C, D, E, F, G, H, and I were used in place of the fragrance B. Similar results were obtained when tube B was used instead of tube A.

[Example 11] Toothpaste calcium carbonate 45.0% by mass
Thickening silica 3.0
Sodium polyacrylate 0.3
Xanthan gum 0.45
Carrageenan 0.5
70% sorbite solution 20.0
Lauroyl sarcosinate sodium 1.5
(Soipon SLP, manufactured by Kawaken Fine Chemicals)
Polyoxyethylene cetyl ether (EO average addition mole number 7) 1.2
(EMALEX107, manufactured by Nippon Emulsion)
Polyoxyethylene hydrogenated castor oil (EO average added mole number 80) 1.0
(BLAUNON RCW-80, Aoki Yushi Kogyo)
Saccharin sodium 0.2
Propylene glycol 4.0
Titanium oxide 0.3
Fragrance C 1.0
dl-α-tocopherol 0.1
(Dl-α-tocopherol, manufactured by BASF Takeda Vitamin)
Sodium monofluorophosphate 0.7
Triclosan 0.3
Tranexamic acid 0.05
Dipotassium glycyrrhizinate 0.1
Toki water extract 0.01
Purified water remaining
Total 100.0% by mass
Housed in tube A.

The evaluation results are as follows.
Stability of dl-α-tocopherol ○
Appearance stability ○
Foaming 5
Taste 4
Manufacturability ◎
Similar results were obtained even when the fragrances A, B, D, E, F, G, H, and I were used in place of the fragrance C. Similar results were obtained when tube B was used instead of tube A.

[Example 12] Toothpaste amorphous silicic acid 18.0 mass%
70% sorbite solution 40.0
Sodium lauryl sulfate 1.5
Sodium alginate 0.3
Xanthan gum 0.4
Sodium polyacrylate 0.3
Saccharin sodium 0.1
Xylitol 5.0
Propylene glycol 3.0
Fragrance D 1.1
Dl-α-tocopherol acetate 0.1
(Tocopherol acetate, manufactured by DSM Nutrition Japan)
Alanine 0.3
Polyoxyethylene myristyl ether (EO average addition mole number 8) 1.4
(EMALGEN 1108, manufactured by Kao)
Polyoxyethylene hydrogenated castor oil (EO average added mole number 20) 1.4
(NIKKOL HCO-20, manufactured by Nikko Chemicals)
Thickening silica 3.0
Titanium oxide 0.3
Dextranase (13000 units / g) 0.1
Mutanase (10000 units / g) 0.05
Sodium benzoate 0.5
Purified water remaining
Total 100.0% by mass
Housed in tube A.

The evaluation results are as follows.
Stability of tocopherol acetate ○
Appearance stability ◎
Foaming 4
Taste 4
Manufacturability ◎
Similar results were obtained even when the fragrances A, B, C, E, F, G, H, and I were used in place of the fragrance D. Similar results were obtained when tube B was used instead of tube A.

[Example 13] toothpaste acetic acid dl-α-tocopherol 0.1% by mass
(Tocopherol acetate, manufactured by DSM Nutrition Japan)
Sodium lauryl sulfate 1.0
(NIKKOL SLS, manufactured by Nikko Chemicals)
Amorphous silicic acid 15.0
Polyoxyethylene stearyl ether (EO average addition mole number 5) 1.2
Polyoxyethylene hydrogenated castor oil (EO average added mole number 20) 1.2
Oat extract 0.03
Tranexamic acid 0.05
Cetylpyridinium chloride 0.03
Sodium tripolyphosphate 1.0
Sodium fluoride 0.21
Propylene glycol 5.0
Polyethylene glycol # 4000 0.5
70% sorbite solution 50.0
Sodium carboxymethylcellulose 1.5
Thickening silica 5.0
Titanium oxide 0.5
Saccharin sodium 0.1
Fragrance E 1.2
Purified water remaining
Total 100.0% by mass
Housed in tube A.

The evaluation results are as follows.
Stability of tocopherol acetate ◎
Appearance stability ◎
Foaming 5
Taste 5
Manufacturability ◎
Similar results were obtained even when the fragrances A, B, C, D, F, G, H, and I were used in place of the fragrance E. Similar results were obtained when tube B was used instead of tube A.

Claims (4)

A dentifrice composition containing vitamin E or a derivative thereof, an anionic surfactant, and an abrasive, (A) having an alkyl group having 14 to 18 carbon atoms, and an average added mole number of ethylene oxide being 3 to 8 0.4 to 5.0% by mass of the polyoxyethylene alkyl ether and (B) 0.5 to 5% by mass of polyoxyethylene hydrogenated castor oil having an average added mole number of ethylene oxide of 10 to 80 , (a) component: (B) component at a mass ratio of 1: 9 to 9: dentifrice composition characterized in that formulated as surfactant mixture was mixed and dispersed in 1 scope. (A) The dentifrice composition of Claim 1 whose average addition mole number of the ethylene oxide of polyoxyethylene alkyl ether is 3-5. The dentifrice composition according to claim 1 or 2, wherein the content of the anionic surfactant is from 0.1 to 5.0% by mass. A dentifrice product in which the dentifrice composition according to claim 1 , 2 or 3 is filled in a container whose innermost layer is made of linear low density polyethylene.