HK1087016B - Base for oral composition and oral composition - Google Patents
Base for oral composition and oral composition Download PDFInfo
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- HK1087016B HK1087016B HK06107141.7A HK06107141A HK1087016B HK 1087016 B HK1087016 B HK 1087016B HK 06107141 A HK06107141 A HK 06107141A HK 1087016 B HK1087016 B HK 1087016B
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Description
Technical Field
The present invention relates to a base for an oral composition, and more particularly, to a base for an oral composition suitable for producing an oral composition containing no water or almost no water. The present invention further relates to an oral composition containing such a base for an oral composition.
Background
In general, a binder such as sodium carboxymethylcellulose, carrageenan, xanthan gum or the like is blended in an oral composition such as a dentifrice, and these components are dissolved in water to express viscosity, and a powder component such as an abrasive and a liquid component are combined to impart shape retention and appropriate viscosity.
Therefore, in an oral composition such as a dentifrice containing no water, it is difficult to maintain shape retention because viscosity is not expressed, and the oral composition separates a powder component and a liquid component with time.
On the other hand, in an oral composition such as a dentifrice, various active ingredients may be blended in a preparation for the purpose of imparting a function and an effect. Examples of the active ingredient include recalcification promoting ingredients, fluorides, bactericides, anti-inflammatory agents, hemostatic agents, various enzymes, and the like.
As the recalcification promoting component, calcium phosphate compounds such as hydroxyapatite are exemplified, and among them, α -tricalcium phosphate (abbreviated as α -TCP) is known to have a very high recalcification promoting effect in the oral cavity and to be effective for prevention and repair of dental caries. However, α -TCP has a property of being converted into an apatite compound in the presence of water, and this reaction is accelerated in the presence of fluoride or other water-soluble calcium phosphate to cause a self-setting reaction, and therefore, cannot be stably incorporated into an oral composition such as a dentifrice containing water in general.
Examples of the fluoride include sodium fluoride, potassium fluoride, sodium monofluorophosphate, and tin fluoride, and the fluoride has an effect of fluoridizing hydroxyapatite of teeth with fluoride ions to strengthen dentin. When fluoride is added to an oral composition such as a normal water-containing dentifrice, fluoride ions may be eluted into water in the oral composition, and other components such as an abrasive may be adsorbed, so that the original effect of fluoride ions cannot be exerted. For example, it is known that in an oral composition containing water and an abrasive such as sodium fluoride or tin fluoride and an abrasive such as calcium phosphate or calcium carbonate, fluorine ions are adsorbed on the abrasive and are deactivated.
Examples of the enzyme include lysomycetes, mutase (mutanase), proteolytic enzyme, amylase, dextrinase, and the like having a bacteriolytic action and a proteolytic action. Many of these enzymes have a problem of causing hydrolysis and lowering of enzyme activity when blended in a composition containing water. Therefore, when an enzyme is added to a composition containing water, it is necessary to select an enzyme that is less likely to cause hydrolysis or to search for a method for stably adding a different enzyme.
Further, although a natural bactericide, hinokitiol, or a hemostatic, epsilon-aminocaproic acid may be blended in an oral composition such as a dentifrice, the blending of these active ingredients in a composition containing water tends to decrease the quantitative value due to hydrolysis. Furthermore, ascorbic acid and salts thereof are known to be effective for bleeding caused by gingivitis, periodontal disease, and the like, but are likely to undergo decomposition reaction in the presence of water, resulting in a decrease in content and coloration.
The problem of stability of these active ingredients is caused by the water contained in oral compositions such as dentifrices. Therefore, an oral composition having a composition in which a powder component and a liquid component are not separated from each other with time and a shape retaining property are not required for an oral composition such as a dentifrice containing little water, which can stably contain α -TCP, fluoride, various enzymes, hinokitiol, ∈ -aminocaproic acid, ascorbic acid, and the like.
Heretofore, as a base for an oral composition suitable for an oral composition containing almost no water or a nonaqueous system, for example, a base containing agar or gelatin has been proposed in Japanese patent laid-open publication No. 2002-114656, a base containing polyethylene powder or polyethylene wax has been proposed in Japanese patent laid-open publication No. 2002-114657, and a base containing polyvinylpyrrolidone has been proposed in Japanese patent laid-open publication No. 2002-255772.
Disclosure of Invention
The purpose of the present invention is to provide a base for an oral composition, which is suitable for the production of an oral composition, particularly for the production of an oral composition containing no or almost no water. It is another object of the present invention to provide a base for an oral composition which is excellent in shape retention and stable over time without causing separation of components, and which is particularly suitable for production of an oral composition containing no water or almost no water. It is a further object of the present invention to provide a base for an oral composition, which can stably contain an unstable active ingredient in the presence of water. It is a further object of the present invention to provide an oral composition containing an unstable active ingredient, in particular, an oral composition containing no or substantially no water, which is generally stably blended in the presence of water.
The present inventors have made intensive studies to achieve the above object and as a result, have found that an oral composition having high stability can be provided by using an oral composition base having a specific composition, and have completed the present invention.
Accordingly, the present invention relates to a base for a nonaqueous oral composition, which is characterized by containing hydroxypropyl cellulose and at least one selected from the group consisting of concentrated glycerin, diglycerin, propylene glycol, 1, 3-butylene glycol and polyethylene glycol. In a preferred embodiment of the present invention, the base for a nonaqueous oral composition further contains at least one selected from the group consisting of anhydrous silicic acid and crystalline cellulose.
The present invention further relates to an oral composition containing the above-mentioned base for an oral composition. In an embodiment of the present invention, the oral composition is preferably a nonaqueous oral composition.
The nonaqueous oral composition in the present specification means an oral composition containing water in an amount of 0 to 3% by mass, preferably 0 to 1% by mass, and more preferably completely containing no water, based on the whole oral composition. In the present specification, such a base suitable for the production of a nonaqueous oral composition is referred to as a nonaqueous oral composition.
The present invention also relates to the above-mentioned base for an oral composition, and an oral composition containing an unstable active ingredient in the presence of water. Examples of the active ingredient unstable in the presence of water include α -tricalcium phosphate (α -TCP), fluorides, enzymes, hinokitiol, epsilon-aminocaproic acid, ascorbic acid, and ascorbate.
Accordingly, the oral composition of the present invention specifically contains at least one of the above-mentioned base for an oral composition and the above-mentioned active ingredient unstable in the presence of water.
Specifically, the oral composition of the present invention comprises the above-mentioned base for oral compositions and at least one selected from the group consisting of α -tricalcium phosphate (α -TCP), fluoride, enzymes, hinokitiol, epsilon-aminocaproic acid, ascorbic acid and ascorbate as an active ingredient unstable in the presence of water.
An embodiment of the present invention is an oral composition comprising the above-described base for an oral composition and α -tricalcium phosphate (α -TCP). In an embodiment of the present invention, there is also provided an oral composition comprising the above-mentioned base for an oral composition and at least one fluoride. In another embodiment of the present invention, an oral composition comprising the above-mentioned base for an oral composition and at least one enzyme is provided. An embodiment of the present invention is an oral composition comprising the above-mentioned base for an oral composition and hinokitiol. In another embodiment of the present invention, there is provided an oral composition comprising the above-mentioned base for an oral composition and epsilon-aminocaproic acid. In an embodiment of the present invention, the oral composition further comprises the above-mentioned base for an oral composition and at least one selected from ascorbic acid and salts thereof.
As a preferred embodiment of the oral composition of the present invention, there is an oral composition in which α -TCP and fluoride are combined with the matrix for an oral composition.
Detailed Description
The oral composition in the present specification includes dentifrices such as toothpaste, liquid dentifrice, wet dentifrice, etc., cream, ointment, patch, mouth freshener, mouthwash, chewing gum, mouthwash, etc. The oral composition of the present invention is preferably a nonaqueous oral composition.
The hydroxypropyl cellulose used in the base for an oral composition of the present invention is a nonionic cellulose derivative obtained by reacting propylene oxide with cellulose. There are grades that exhibit different viscosities depending on the degree of polymerization of the molecules. The low viscosity grade is about 1 to 4mPa/S, and the high viscosity grade is about 1000 to 5000 mPa/S. The viscosity was measured by using a rotational viscometer as a value (mPa/S) of a 2% aqueous solution of each hydroxypropylcellulose.
The present invention can use hydroxypropylcellulose of low to high viscosity grade, that is, it can be selected from hydroxypropylcellulose having a viscosity of 1 to 5000 mPa/S. Furthermore, hydroxypropyl cellulose of 2 or more types having different viscosities can be used. The invention preferably uses hydroxypropyl cellulose with the viscosity of 150-4000 mPa/S.
Such hydroxypropyl cellulose is widely used as a sintering agent for ceramics and fluorescent lamp tubes of building and motor parts, as typified by medicines and cosmetics, and commercially available products used for these are used in the present invention.
The content of 1 or more than 2 hydroxypropyl celluloses with different viscosities in the oral composition is 0.1-15 mass%, preferably 0.1-10 mass% of the total mass of the oral composition. The amount of the hydroxypropylcellulose in the above range is appropriate in view of the effect to be achieved by the present invention and the usability of the oral composition.
The base for an oral composition of the present invention further contains at least one of concentrated glycerin, diglycerin, propylene glycol, 1, 3-butylene glycol, and polyethylene glycol. Of these, propylene glycol and 1, 3-butanediol are particularly preferably used.
Concentrated glycerin, diglycerin, propylene glycol, 1, 3-butylene glycol, and polyethylene glycol, represented by drugs and cosmetics, are generally widely used in the food, miscellaneous goods, petrochemical industry, coating industry, and the like. Commercially available products can be used in the present invention.
The content of at least one of concentrated glycerin, diglycerin, propylene glycol, 1, 3-butylene glycol, and polyethylene glycol in the oral composition is preferably 10 to 85 mass%, and more preferably 20 to 60 mass%, based on the total mass of the oral composition. In view of exerting good usability of the oral composition, their content is suitably within the above range.
The base for the oral composition of the present invention may further contain anhydrous silicic acid and/or crystalline cellulose.
The anhydrous silicic acid is silicon dioxide, and the character is white powder. Sodium silicate is artificially treated with an acid to precipitate silica, and the silica is aged by gelation, dried and pulverized to obtain the silica gel. Further, it is preferable that the dry weight is reduced to 13% or less and the hot weight is reduced to 18% or less. Here, dry weight loss means the mass% of the evaporated components after heating 1g of anhydrous silicic acid at 105 ℃ for 2 hours, and intense heat weight loss means the mass% of the evaporated components after heating 1g of anhydrous silicic acid at 850 ℃ for 30 minutes.
Such anhydrous silicic acid is represented by food and cosmetics, and is widely used in general in pharmaceuticals, agricultural products, feeds, ink industry, rubber industry, plastic industry, and the like.
The content of the anhydrous silicic acid in the oral composition is preferably 0.5 to 30% by mass, more preferably 3 to 15% by mass, based on the total mass of the oral composition. The amount in the above range is appropriate in view of the effect to be achieved by the present invention and the usability of the oral composition.
Crystalline cellulose is a cellulose crystallite aggregate having substantially a certain degree of polymerization, which is obtained by acid hydrolysis or alkali hydrolysis of α -cellulose obtained from a fibrous plant as pulp.
Such crystalline cellulose is represented by foods and cosmetics, and is widely used in general for pharmaceuticals, agricultural products, feeds, and the like.
The content of the crystalline cellulose in the oral composition is preferably 0.5 to 30% by mass, more preferably 3 to 10% by mass, based on the total mass of the oral composition. The amount in the above range is appropriate in view of the effect to be achieved by the present invention and the usability of the oral composition.
In the present invention, the base for an oral composition may be combined with various components such as additives and active ingredients conventionally used in oral compositions to prepare an oral composition.
The matrix for oral compositions of the present invention is particularly advantageous in combination with active ingredients that are generally unstable in the presence of water. Examples of such components include α -TCP, fluorides, enzymes, hinokitiol, ε -aminocaproic acid, ascorbic acid and ascorbate.
The alpha-TCP used in the oral composition of the present invention is alpha-tricalcium phosphate (3 Ca)3(PO4)2·Ca(OH)2) In general, drugs and cosmetics are widely used in foods, miscellaneous goods, petrochemical products, and the like. In the present invention, can be usedAnd (5) selling the product.
The content of α -TCP in the oral composition of the present invention is preferably 0.1 to 50 mass%, and more preferably 1 to 30 mass%, based on the total mass of the oral composition. In order to exert the recalcification effect of α -TCP, the content of α -TCP is preferably 0.1 mass% or more, and if it exceeds 50 mass%, the usability of the oral composition may be impaired.
When α -TCP is blended, if fluoride is further used in combination, supply of fluorine ions increases recalcification, and thus a very excellent effect can be exhibited. Therefore, it is preferable to use α -TCP in combination with a fluoride described later.
Specific examples of the fluoride used in the present invention include sodium fluoride, potassium fluoride, sodium monofluorophosphate, and tin fluoride, and at least one of them can be used. These fluorides are generally widely used in pharmaceuticals, cosmetics, and the like. Commercially available products can be used in the present invention.
The content of the fluoride in the oral composition of the present invention is preferably 0.01 to 3% by mass based on the total mass of the oral composition, and the content of fluorine in the oral composition such as a dentifrice is preferably 100 to 1000 ppm.
The fluoride is preferably sodium fluoride and sodium monofluorophosphate.
Specific examples of enzymes used in the oral composition of the present invention include lysomycetes, mutase, proteolytic enzyme, amylase, dextrinase, and 1 or 2 or more thereof. These enzymes are widely used in general for pharmaceuticals, cosmetics, foods, and the like. Commercially available products can be used in the present invention.
The content of the enzyme in the oral composition of the present invention is preferably 0.01 to 5% by mass, more preferably 0.1 to 2% by mass, based on the total mass of the oral composition.
The enzyme is preferably lysomycete or amylase.
Hinokitiol used in the oral composition of the present invention is a specific component contained in a natural tree, hinokitious arborvitae, and is a crystalline acidic compound. Examples of other species of hinokitiol include hinoki Taiwan, western red pine of North America, and the like. Hinokitiol has strong antibacterial activity and broad antibacterial spectrum, and is one of few natural bactericides.
Such hinokitiol is represented by drugs and cosmetics, and is widely used in general for foods, agricultural products, building materials, feeds, and the like. Commercially available products used therein can be used in the present invention.
The content of hinokitiol in the oral composition of the present invention is preferably 0.005 to 0.5 mass%, more preferably 0.01 to 0.2 mass%, based on the total mass of the oral composition.
The epsilon-aminocaproic acid used in the oral composition of the present invention is a component having an anti-plasmin effect, a hemostatic effect, and an anti-inflammatory effect, and is widely used in general for foods, agricultural products, and the like, as typified by cosmetics and drugs. Commercially available products can be used in the present invention.
The content of epsilon-aminocaproic acid in the oral composition of the present invention is preferably 0.001 to 1 mass%, and more preferably 0.006 to 0.2 mass%, based on the total mass of the oral composition.
The ascorbic acid used in the oral composition of the present invention is so-called vitamin C, specifically L-ascorbic acid (C)6H8O6176) and salts thereof. Specific examples of the ascorbate used include sodium ascorbate, potassium ascorbate, calcium ascorbate, magnesium ascorbate, and the like. The oral composition of the present invention may contain 1 or 2 or more selected from ascorbic acid and salts thereof. Sodium ascorbate is preferably used in the ascorbate.
These ascorbic acids and salts thereof are components having anti-inflammatory action and collagen fiber synthesis promoting action, and are widely used in general in foods, agricultural products and the like, as typified by cosmetics and pharmaceuticals. Commercially available products can be used in the present invention.
The content of at least 1 selected from the group consisting of ascorbic acid and salts thereof in the oral composition of the present invention is preferably 0.001 to 20% by mass, more preferably 0.01 to 10% by mass, based on the total mass of the oral composition.
As described above, as the active ingredients used in combination in the base for an oral composition of the present invention, (1) α -TCP; (2) a fluoride compound; (3) enzymes; (4) hinokitiol; (5) epsilon-aminocaproic acid; and (6) ascorbic acid and salts thereof. The compound may contain 1 or 2 or more compounds selected from the groups (1) to (6) among them, and is not limited to the group 1, and the compounds selected from the group 2 or more may be used in combination. Among them, a-TCP and fluoride are preferably used in combination.
In the oral composition of the present invention, the following components may be added as required within the range of the usual usage amount, depending on the kind of the components.
< polishing slurry >
Examples thereof include silica abrasives such as silica gel, precipitated silica, pyrogenic silica, hydrous silicic acid, zeolite, aluminum silicate, and zirconium silicate, and 1 or 2 or more of them can be used in combination, calcium hydrogen phosphate dihydrate, calcium hydrogen phosphate anhydride, calcium pyrophosphate, trimagnesium phosphate, tricalcium phosphate, aluminum hydroxide, alumina, light calcium carbonate, heavy calcium carbonate, magnesium carbonate, zirconium silicate, and synthetic resin abrasives. The amount of the polishing agent is preferably 3 to 60% by mass, more preferably 10 to 45% by mass, based on the total composition.
< wetting agent >
1 or 2 or more kinds of polyhydric alcohols such as sorbitol and maltitol can be used.
< blowing agent >
Examples thereof include sodium lauryl sulfate, sodium lauryl sarcosinate, sodium alkyl sulfosuccinate, sodium coconut oil fatty acid monoglyceride sulfonate, sodium α -olefin sulfonate, N-acyl amino acid salts such as N-glutamic acid, 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazoline betaine, maltitol fatty acid esters, sucrose fatty acid esters, polyglycerol fatty acid esters, fatty acid diethanolamides, polyoxyethylene sorbitan monolaurate, polyoxyethylene hardened castor oil, and polyoxyethylene fatty acid esters, and 1 or 2 or more of them may be used in combination.
< sweetening agent >
Examples thereof include saccharin sodium, aspartame, trehalose, stevioside, stevia extract, p-methoxycinnamaldehyde, neohesperidin dihydrochalcone, perillatin, etc., and 1 or 2 or more of them may be used in combination.
< preservatives >
Examples thereof include parabens such as methyl paraben, ethyl paraben, propyl paraben and butyl paraben, sodium benzoate, phenoxyethanol and alkyldiaminoethylglycine hydrochloride, and 1 or 2 or more of them may be used in combination.
< fragrance component >
1 or 2 or more of the following substances may be used in combination: 1-menthol, anethole, menthone, eucalyptol, limonene, carvone, methyl salicylate, ethyl butyrate, eugenol, thymol, cinnamaldehyde, and trans-2-hexenal. These components may be blended in the form of a single product, or may be blended with essential oils containing them.
In addition to the above-mentioned perfume components, perfume components such as fatty alcohols or esters thereof, terpenoids, phenol ethers, aldehydes, ketones, lactones, and essential oils may be blended as long as the effects of the present invention are not impaired. The amount of the perfume is preferably 0.02 to 2% by mass based on the whole composition.
< effective ingredient >
Examples thereof include zeolite, chlorhexidine salts, cetylpyridinium chloride, benzalkonium chloride, benzethonium chloride, myrrh, triclosan, isopropylcresol, tocopherol acetate, tranexamic acid, dihydrocholesterol, polyvinylpyrrolidone, glycyrrhetinic acid salts, copper chlorophyllin salts, sodium chloride, and guaiacum salts, and 1 or 2 or more of them can be used in combination.
< others >
Pigments such as cyan No. 1, pigments such as titanium oxide, antioxidants such as dibutylhydroxytoluene, dry tea distillate, and flavoring agents such as sodium glutamate can be used.
When water is added to the oral composition of the present invention in an amount of 3% by mass or less depending on the type thereof, the following binder may be added as necessary in addition to the above components.
< Binder >
Examples thereof include alginates and derivatives thereof such as carrageenan (iota, lambda, kappa), alginic acid, sodium alginate, propylene glycol alginate, calcium-containing sodium alginate, potassium alginate, calcium alginate, ammonium alginate, xanthan gum, guar gum, gelatin, agar, sodium carboxymethylcellulose, sodium hydroxyethylcellulose, sodium polyacrylate, and the like, and 1 or more of them may be used in combination.
The oral composition comprising the above components in combination can be produced by a conventional method, and is not particularly limited.
The obtained composition such as dentifrice can be used by filling it in an aluminum tube, a laminate tube, a glass deposition tube, a plastic bottle, an aerosol container, etc.
(examples)
The present invention will be described in detail below with reference to examples and comparative examples, but the present invention is not limited to the following examples. Various toothpastes were prepared according to the compositions (unit: mass%) shown in tables 1 to 4 by a conventional method and used in the following tests. The results are summarized in tables 1 to 4.
1. Test of storage stability of toothpaste
After the toothpaste shown in Table 1 was prepared, it was stored under the following conditions in a severe environment. After the storage under severe environment was completed, the state of each toothpaste was subjected to sensory evaluation according to the following evaluation criteria.
[ storage conditions under severe Environment ]
Storing in a thermostatic bath at 1.60 deg.C for 1 month
Storing in a thermostatic bath at 2.50 deg.C for 2 months
[ evaluation standards ]
O: the state is unchanged compared with the state after modulation
X: the separation of solid and liquid components was confirmed
TABLE 1
| Component (%) | Examples | Comparative example | ||||
| 1 | 2 | 1 | 2 | 3 | 4 | |
| Hydroxypropyl cellulose (viscosity 150 ~ 400mPa/S) | 2.0 | 2.0 | - | - | - | - |
| 1, 3-butanediol | 61.8 | 49.8 | 63.8 | 51.8 | 48.8 | 48.8 |
| Anhydrous silicic acid | - | 12.0 | - | 12.0 | 12.0 | 12.0 |
| Carrageenan | - | - | - | - | 3.0 | - |
| Sodium carboxymethylcellulose | - | - | - | - | - | 3.0 |
| Aluminum hydroxide | 35.0 | 35.0 | 35.0 | 35.0 | 35.0 | 35.0 |
| Sodium lauryl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Saccharin sodium salt | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Nipagin ethyl ester | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| In total | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
| State stability storage at 60 ℃ for one month | ○ | ○ | × | × | × | × |
| State stability storage at 50 ℃ for two months | ○ | ○ | × | × | × | × |
2. Test for measurement of fluorine ion
After the toothpaste shown in Table 2 was prepared, it was stored under the following conditions in a severe environment. After preservation in a severe environment, a certain amount of toothpaste is measured, and the toothpaste is immediately centrifugally separated after being dispersed by water and separated into a liquid layer and a solid layer. For these liquid layer portions, the fluorine ion concentration was measured using a fluorine ion meter. Here, the detected fluoride ion is considered to be active fluoride ion which does not adsorb other components in the toothpaste. The remaining percentage of active fluorine ions was determined by the following formula (1).
[ storage conditions under severe Environment ]
Storing in a thermostatic bath at 1.60 deg.C for 1 week
Storing in a thermostatic bath at 2.60 deg.C for 2 weeks
[ formula (1) ]
The residual ratio (%) ([ (amount of fluorine ion after storage under the above-mentioned severe environment) ]/(amount of fluorine ion at the time of preparation of toothpaste) ] × 100
In addition, when the residual rate of fluorine ions, that is, the active fluorine ions, in the toothpaste storage product under severe conditions was 80% or more, it was judged that the fluoride was stable.
Also, the toothpastes shown in table 2 were subjected to the storage stability test in the same manner as in 1.
TABLE 2
| Component (%) | Examples | Comparative example | Reference example 1 | |||
| 3 | 4 | 5 | 6 | |||
| Hydroxypropyl cellulose (viscosity 150 ~ 400mPa/S) | 3.0 | 3.0 | - | - | 3.0 | |
| 1, 3-butanediol | 60.6 | 48.6 | - | 48.6 | 18.6 | |
| Anhydrous silicic acid | - | 12.0 | 12.0 | 12.0 | 12.0 | |
| Carrageenan | - | - | 2.0 | 3.0 | - | |
| Water (W) | - | - | 49.6 | - | 30.0 | |
| Sodium fluoride | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | |
| Calcium hydrogen phosphate | 35.0 | 35.0 | 35.0 | 35.0 | 35.0 | |
| Sodium lauryl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | |
| Saccharin sodium salt | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| Nipagin ethyl ester | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| In total | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | |
| State stability storage at 60 ℃ for one month | ○ | ○ | ○ | × | ○ | |
| State stability storage at 50 ℃ for two months | ○ | ○ | ○ | × | ○ | |
| Residual fluorine ion ratio (%) | Storing at 60 deg.C for 1 week | 95 | 94 | 45 | 94 | 41 |
| Storing at 60 deg.C for 2 weeks | 92 | 90 | 35 | 91 | 39 | |
3. Quantitative test for epsilon-aminocaproic acid
After the toothpaste shown in Table 3 was prepared, it was stored under the following conditions in a severe environment. After the storage under a severe environment, the epsilon-aminocaproic acid in each toothpaste was quantitatively tested by liquid chromatography under the following conditions.
[ storage conditions under severe Environment ]
Storing in a thermostatic bath at 1.60 deg.C for 1 month
Storing in a thermostatic bath at 2.50 deg.C for 2 months
[ test conditions ]
A detector: fluorescence detector (excitation wavelength: 390nm, fluorescence wavelength: 480nm)
Column: and (3) filling 5-10 mu m of octadecylsilane chemically bonded silica for high performance liquid chromatography into a stainless steel pipe with the inner diameter of 4.6mm and the length of 250 mm.
Column temperature: 40 deg.C
Mobile phase: phosphoric acid solution/acetonitrile mixed solution
Flow rate: 1.0ml per minute
The residual rate of epsilon-aminocaproic acid was determined by the following formula (2).
[ formula (2) ]
The remaining ratio (%) (amount of epsilon-aminocaproic acid after storage in the above-mentioned harsh environment) ]/(amount of epsilon-aminocaproic acid at the time of preparation of toothpaste) ] × 100
In addition, when the residual rate of epsilon-aminocaproic acid was 90% or more with respect to the toothpaste storage product under severe conditions, it was judged that epsilon-aminocaproic acid was stable.
Also, the toothpastes shown in table 3 were subjected to the storage stability test in the same manner as in 1.
TABLE 3
| Component (%) | Examples | Comparative example | Reference example 2 | |||
| 5 | 6 | 7 | 8 | |||
| Hydroxypropyl cellulose (viscosity 150 ~ 400mPa/S) | 3.0 | 3.0 | - | - | 3.0 | |
| 1, 3-butanediol | 56.7 | 44.7 | 15.7 | 44.7 | 14.7 | |
| Anhydrous silicic acid | - | 12.0 | 12.0 | 12.0 | 12.0 | |
| Carrageenan | - | - | 2.0 | 3.0 | - | |
| Water (W) | - | - | 30.0 | - | 30.0 | |
| Epsilon-aminocaproic acid | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| Aluminum hydroxide | 35.0 | 35.0 | 35.0 | 35.0 | 35.0 | |
| Polyoxyethylene hardened castor oil | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 | |
| Saccharin sodium salt | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| Nipagin ethyl ester | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| In total | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | |
| State stability storage at 60 ℃ for one month | ○ | ○ | ○ | × | ○ | |
| State stability storage at 50 ℃ for two months | ○ | ○ | ○ | × | ○ | |
| Residual rate of ε -aminocaproic acid (%) | Storing at 60 deg.C for one month | 100 | 100 | 82 | 99 | 81 |
| Storing at 50 deg.C for two months | 100 | 100 | 82 | 99 | 82 | |
4. Quantitative test for sodium ascorbate
After the toothpaste shown in Table 4 was prepared, it was stored under the following conditions in a severe environment. After the storage under a severe environment, quantitative tests were carried out on sodium ascorbate in each toothpaste by liquid chromatography under the following conditions.
[ storage conditions under severe Environment ]
Storing in a thermostatic bath at 1.60 deg.C for 1 month
Storing in a thermostatic bath at 2.50 deg.C for 2 months
[ test conditions ]
A detector: ultraviolet spectrophotometer (measuring wavelength: 245nm)
Column: a stainless steel tube having an inner diameter of 4.6mm and a length of 250mm was filled with a 5 μm-size octadecylsilane chemically bonded silica for high performance liquid chromatography.
Column temperature: 40 deg.C
Mobile phase: metaphosphoric acid solution
Flow rate: 1.0ml per minute
The remaining ratio of sodium ascorbate was obtained by the following formula (3).
[ formula (3) ]
Residual rate (%) ([ (amount of sodium ascorbate after storage in the above-mentioned severe environment) ]/(amount of sodium ascorbate at the time of preparation of toothpaste) ] × 100
In addition, when the residual ratio of sodium ascorbate was 90% or more with respect to the toothpaste storage product under severe conditions, it was judged that sodium ascorbate was stable.
Also, the toothpastes shown in table 4 were subjected to the storage stability test in the same manner as in 1.
TABLE 4
| Component (%) | Examples | Comparative example | Reference example 3 | |||
| 7 | 8 | 9 | 10 | |||
| Hydroxypropyl cellulose (viscosity 150 ~ 400mPa/S) | 3.0 | 3.0 | - | - | 3.0 | |
| 1, 3-butanediol | 58.9 | 46.9 | 17.9 | 46.9 | 16.9 | |
| Anhydrous silicic acid | - | 12.0 | 12.0 | 12.0 | 12.0 | |
| Carrageenan | - | - | 2.0 | 3.0 | - | |
| Water (W) | - | - | 30.0 | - | 30.0 | |
| Ascorbic acid sodium salt | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | |
| Aluminum hydroxide | 35.0 | 35.0 | 35.0 | 35.0 | 35.0 | |
| Sodium lauryl sulfate | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | |
| Saccharin sodium salt | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | |
| Nipagin ethyl ester | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| In total | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 | |
| State stability storage at 60 ℃ for one month | ○ | ○ | ○ | × | ○ | |
| State stability storage at 50 ℃ for two months | ○ | ○ | ○ | × | ○ | |
| Residual ratio of sodium ascorbate (%) | Storing at 60 deg.C for one month | 93 | 94 | 35 | 93 | 38 |
| Storing at 50 deg.C for two months | 97 | 96 | 38 | 96 | 37 | |
From the above experimental results, first of all, the results in table 1 show that the use of the base for an oral composition of the present invention results in no separation of toothpaste and excellent storage stability. The results in tables 2 to 4 show that the toothpaste composition of the present invention has good state stability and excellent storage stability of fluoride, epsilon-aminocaproic acid, ascorbic acid and salts thereof.
The above experiments were also conducted on the toothpastes of examples 9 to 22 described below, which were prepared in accordance with a conventional method, and the same results as described above were obtained.
[ example 9]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S) polyethylene glycol crystalline cellulose aluminum hydroxide sodium lauryl sulfate saccharin sodium nipagin perfume tocopherol acetate cetylpyridinium chloride | 3.0 mass% 49.6510.035.01.00.10.11.00.10.05 |
| In total | 100.0% by mass |
[ example 10]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 1000-4000 mPa/S) diglycerol propylene glycol anhydrous silicic acid crystalline cellulose sodium fluoride calcium carbonate sodium lauryl sulfate sodium dodecyl sarcosinate sodium stevia extract sodium benzoate perfume dipotassium glycyrrhizinate isopropyl cresol | 1.0 mass% 23.023.175.010.00.235.01.00.30.10.11.00.10.03 |
| In total | 100.0% by mass |
[ example 11]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 2-3 mPa/S) concentrated glycerol polyethylene glycol 1, 3-butanediol anhydrous silicic acid epsilon-aminocaproic acid stannic fluoride dentifriceDistilled water beta-glycyrrhetinic acid chlorhexidine hydrochloride perfume with calcium hydrogen phosphate sucrose fatty acid ester xylitol carrageenan nipagin perfume | 10.0 mass% 19.010.010.810.00.10.125.00.510.00.30.11.03.00.050.05 |
| In total | 100.0% by mass |
[ example 12]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 6-10 mPa/S) concentrated glycerol polyethylene glycol anhydrous silicic acid alpha-TCP sodium fluoride lauryl sodium sulfate polyoxyethylene hardened castor oil saccharin sodium nipagin spice tocopherol acetate glycyrrhizic acid | 10.0 mass% 34.4510.010.030.00.21.03.00.10.11.00.10.05 |
| In total | 100.0% by mass |
[ example 13]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S) concentrated glycerol anhydrous silicic acid crystalline cellulose chloride lysozyme sodium lauryl sulfate sodium dodecyl sarcosinate sodium stevia rebaudiana extract nipagin spice zeolite cetylpyridinium chloride | 3.0 mass% 54.9520.010.08.00.51.00.30.10.11.01.00.05 |
| In total | 100.0% by mass |
[ example 14]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 6-10 mPa/S), concentrated glycerol polyethylene glycol anhydrous silicic acid hinokitiol epsilon-aminocaproic acid dentifrice, calcium hydrogen phosphate polyoxyethylene hardened castor oil trehalose sorbitol alkyl diamino ethyl glycine hydrochloride solution, perfume sodium chloride tocopherol acetate | 5.0 mass% 23.720.010.00.050.115.05.05.05.00.051.010.00.1 |
| In total | 100.0% by mass |
[ example 15]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S) polyethylene glycol 1, 3-butylene glycol anhydrous silicic acid crystalline cellulose alpha-TCP sodium fluoride lauryl sodium sulfate sodium lauryl sarcosinate sodium stevia extract nipagin spice zeolite cetylpyridinium chloride | 3.0 mass% 20.030.2510.020.010.03.00.21.00.30.10.11.01.00.05 |
| In total | 100.0% by mass |
[ example 16]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S) polyethylene glycol 1, 3-butanediol anhydrous sodium lauryl silicate sulfate saccharin sodium parabenGold perfume sodium ascorbate tocopheryl acetate | 3.0 mass% 20.063.2510.01.00.50.11.01.01.0 |
| Cetylpyridinium chloride | 0.05 |
| In total | 100.0% by mass |
[ example 17]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 1000-4000 mPa/S) polyethyleneGlycol 1, 3-butanediol anhydrous silicic acid dentifrice containing calcium hydrogen phosphate glycerin fatty acid ester stevia rebaudiana extract sodium benzoate perfume, sodium ascorbate perfume, sodium fluoride dipotassium glycyrrhizinate isopropyl cresol | 1.0 mass% 20.046.575.020.03.00.11.01.02.00.20.10.03 |
| In total | 100.0% by mass |
[ example 18]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S), hydroxypropyl cellulose (viscosity 1000-4000 mPa/S), polyethylene glycol 1, 3-butanediol anhydrous silicic acid dentifrice, calcium hydrogen phosphate, sucrose fatty acid ester, polyoxyethylene hardened castor oil, xylitol, nipagin flavor, distilled water, ascorbic acid beta-glycyrrhetinic acid | 1.5% by mass and 0.5% by mass 10.037.210.025.00.53.010.00.11.01.00.10.05 |
| Chlorhexidine hydrochloride | 0.05 |
| In total | 100.0% by mass |
[ example 19]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 6-10 mPa/S) polyethylene glycol 1, 3-butanediol anhydrous sodium monofluorophosphate, sodium lauryl sulfate, polyoxyethylene hardened castor oil saccharin sodium nipagin spice, ascorbic acid zeolite, tocopherol acetate, glycyrrhizic acid | 10.0 mass% 15.052.5510.00.71.03.01.00.11.00.55.00.10.05 |
| In total | 100.0% by mass |
[ example 20]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S) concentrated glycerin propylene glycol anhydrous silicic acid dentifrice, and sodium ascorbate tocopherol acetate zeolite as nipagin flavor extracted from calcium hydrogen phosphate glycerin fatty acid ester polyoxyethylene hardened castor oil stevia rebaudiana Bertoni | 3.0 mass% 30.026.6510.020.01.02.00.10.11.05.00.11.0 |
| Cetylpyridinium chloride | 0.05 |
| In total | 100.0% by mass |
[ example 21]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S)1, 3-butanediol polyethylene glycol anhydrous calcium carbonate polyoxyethylene hardened castor oil saccharin sodium xylitol lauryl sodium sulfate nipagin perfume sodium ascorbate cetylpyridinium chloride beta-glycyrrhetinic acid sodium fluoride | 2.0 mass% 49.610.010.020.03.01.01.01.00.11.01.00.050.050.2 |
| In total | 100.0% by mass |
[ example 22]
| Preparation of toothpaste | |
| Hydroxypropyl cellulose (viscosity 150-400 mPa/S)1, 3-butanediol polyethylene glycol anhydrous silicic acid zeolite dentifrice is prepared from calcium hydrogen phosphate anhydrous ethanol titanium oxide sodium saccharin sodium lauryl sulfate dibutyl hydroxy toluene magnesium phosphate 1-menthol peppermint oil nipagin pigment sodium ascorbate tocopherol acetate | 3.0 mass% 45.110.06.05.017.05.53.01.81.00.50.30.30.20.10.11.00.1 |
| In total | 100.0% by mass |
Industrial applicability
The base for an oral composition of the present invention can provide a nonaqueous oral composition having good shape retention and high stability. By combining the base for an oral composition of the present invention with α -TCP, fluoride, various enzymes, hinokitiol, epsilon-aminocaproic acid, ascorbic acid, ascorbate, and the like, which are active ingredients that are generally unstable in the presence of water, a non-aqueous oral composition that is stable over time, has shape retention properties, can stably maintain the active ingredients, and does not cause separation of solid and liquid components, can be obtained.
Claims (4)
1. A nonaqueous oral composition having a water content of 0 to 3% by mass, characterized by containing ascorbic acid or a salt thereof, hydroxypropyl cellulose, and at least one selected from the group consisting of concentrated glycerin, diglycerin, propylene glycol, 1, 3-butylene glycol, and polyethylene glycol.
2. The nonaqueous oral composition according to claim 1, further comprising at least one of anhydrous silicic acid and crystalline cellulose.
3. The nonaqueous oral composition according to claim 1 or 2, wherein the ascorbic acid or a salt thereof is sodium ascorbate.
4. The non-aqueous oral composition according to claim 1 or 2, which is a dentifrice.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002323296 | 2002-11-07 | ||
| JP323296/2002 | 2002-11-07 | ||
| PCT/JP2003/014196 WO2004041230A1 (en) | 2002-11-07 | 2003-11-07 | Base for oral composition and oral composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| HK1087016A1 HK1087016A1 (en) | 2006-10-06 |
| HK1087016B true HK1087016B (en) | 2008-07-18 |
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