JP2012148998A - Dentifrice composition - Google Patents

Abstract

Disclosed is a dentifrice composition having excellent storage stability of β-glycyrrhetinic acid, high anti-inflammatory effect, little taste and irritation after use, moderate saltiness, and excellent brushing feeling.
SOLUTION: A dentifrice composition containing β-glycyrrhetinic acid is blended with sodium chloride and polyoxyethylene hydrogenated castor oil in a mass ratio of sodium chloride / polyoxyethylene hydrogenated castor oil in the range of 5-15. And a dentifrice composition comprising heavy calcium carbonate and agaric extract.
[Selection figure] None

Description

  The present invention relates to a dentifrice composition having excellent stability and anti-inflammatory effect of β-glycyrrhetinic acid, less nastyness and irritation after use, excellent salty taste and feeling of use at the time of use, and good usability. .

  Conventionally, it is known that glycyrrhetinic acid or a derivative thereof is added to a dentifrice composition as an anti-inflammatory agent (Patent Document 1: Japanese Patent Publication No. 45-22436, Patent Document 2: Japanese Patent Laid-Open No. 51-41447). Publication).

  However, when the dentifrice composition is stored for a long period of time, the residual amount of glycyrrhetinic acid or a derivative thereof is reduced, resulting in a problem that it is difficult to sufficiently exert its medicinal effect. Therefore, a dentifrice composition that has a high residual ratio of glycyrrhetic acid even when stored for a long period of time and that effectively maintains its medicinal effect has been desired.

  As a means for solving the above problem, there is a finding that when sodium chloride is added, the residual ratio of glycyrrhetinic acid and its derivatives is increased even when stored for a long period of time (Patent Document 3: Japanese Patent Laid-Open No. 63-35515). However, when sodium chloride is added, there is a problem that irritation occurs and the residual rate of glycyrrhetinic acid and its derivatives does not necessarily increase.

  On the other hand, as a means for solving the flavor when sodium chloride is blended, a technique has been proposed in which, when polyoxyethylene hydrogenated castor oil is added, the aftertaste is good and the feeling of use is excellent (Patent Document 4: JP-A-59-122417). Issue gazette). However, this technique alleviates the irritation caused by sodium chloride, but there is a problem that the flavor of the preparation does not necessarily improve even when polyoxyethylene hydrogenated castor oil is added. This technology improves the dispersion and solubilizing power and feel of use of oil-soluble components such as fragrances and pigments by using polyoxyethylene hydrogenated castor oil and an anionic surfactant in combination, and is suitable for a sodium chloride-containing system. It indicates that it can be used. From such a technique, it is not possible to predict a technique for improving the stability and feeling of use of glycyrrhetinic acid in a dentifrice composition containing glycyrrhetinic acid.

  Heavy calcium carbonate is widely used in dentifrice etc. as an abrasive with excellent brushing feeling, but generally the taste becomes mud when heavy calcium carbonate is blended as an abrasive in dentifrice compositions. There was a problem.

  Accordingly, an object of the present invention is to stably blend β-glycyrrhetinic acid in a dentifrice composition, have excellent anti-inflammatory effect with excellent storage stability of β-glycyrrhetinic acid, and good usability. It is providing the dentifrice composition containing this.

Japanese Patent Publication No. 45-22436 Japanese Patent Laid-Open No. 51-41447 JP 63-35515 A JP 59-122417 A

  The present invention has been made in view of the above circumstances, is excellent in stability of β-glycyrrhetinic acid, has a high anti-inflammatory effect, has little off-taste and irritation after use, has a moderate salty taste, and has an excellent feeling of brushing. It is an object of the present invention to provide a dentifrice composition.

  As a result of intensive studies to achieve the above object, the inventors of the present invention have added sodium chloride and polyoxyethylene hydrogenated castor oil to a dentifrice composition containing β-glycyrrhetinic acid, sodium chloride / polyoxyethylene. By blending the weight ratio of hydrogenated castor oil in the range of 5 to 15 and blending heavy calcium carbonate and agate extract, the stability of β-glycyrrhetinic acid is excellent and a high anti-inflammatory effect is exhibited. It has been found that a dentifrice composition having little off-taste and irritation after use, moderate salty taste and excellent brushing feeling can be obtained, leading to the invention.

When glycyrrhetinic acid is blended in the dentifrice composition, there are problems that the residual rate is lowered after storage or a nasty taste occurs. As described above, it is known that stability is increased when sodium chloride is used in combination with glycyrrhetinic acid. However, as a result of further studies by the present inventors, irritation may occur in this case, and after long-term storage, It is difficult to say that the stabilization of glycyrrhetinic acid can be satisfactorily improved, it is difficult to fully stabilize glycyrrhetinic acid under a good feeling of use, and it is difficult to exert a high anti-inflammatory effect, and further blended with polyoxyethylene hydrogenated castor oil However, it has been difficult to effectively prevent a decrease in the residual ratio of glycyrrhetinic acid and exhibit a high anti-inflammatory effect under a good feeling of use. On the other hand, according to the present invention, the dentifrice composition containing β-glycyrrhetinic acid is blended with sodium chloride and polyoxyethylene hydrogenated castor oil in an appropriate ratio, and heavy calcium carbonate is used as an abrasive. In addition, the above-mentioned problems can be solved unexpectedly, and the stability of β-glycyrrhetinic acid is improved satisfactorily, effectively reducing the residual rate after long-term storage. In addition to being able to effectively suppress gingivitis and exhibit high anti-inflammatory effects, mask off taste and irritation, moderate salty taste, maintain good flavor after storage, good wiping It is possible to obtain a preparation excellent in feeling in use. In the composition of the present invention, β-glycyrrhetinic acid is stabilized for a long period of time in the preparation. For example, even when stored at a high temperature of 60 ° C. for one month, the residual rate is suppressed and maintained stably, and has a high anti-inflammatory effect. In addition to playing, the feeling of use is also good.
In the dentifrice composition containing glycyrrhetinic acid, the mechanism by which the residual amount of glycyrrhetinic acid after long-term storage decreases is not clear, but β-glycyrrhetinic acid may be adsorbed to the polyethylene container when stored for a long period of time. Presumed to be a factor. According to the present invention, the solubilized state becomes appropriate by using polyoxyethylene hydrogenated castor oil in a specific ratio in combination with sodium chloride, and further by blending heavy calcium carbonate and a buckwheat extract, β-glycyrrhetinic acid Stability increases and can be sufficiently stabilized, and the anti-inflammatory effect is further enhanced, a good feeling of brushing is obtained, and the taste and irritation after use are masked, the salty taste is moderate and the taste after storage is good It is presumed that the above object can be achieved.

Accordingly, the present invention provides the following dentifrice composition.
Claim 1:
A dentifrice composition containing β-glycyrrhetinic acid is blended with sodium chloride and polyoxyethylene hydrogenated castor oil in a mass ratio of sodium chloride / polyoxyethylene hydrogenated castor oil in the range of 5 to 15, and heavy. A dentifrice composition comprising calcium carbonate and alum extract.
Claim 2:
The dentifrice composition of Claim 1 containing 5-20 mass% of sodium chloride.
Claim 3:
The dentifrice composition according to claim 1 or 2, comprising 0.8 to 2.5% by mass of polyoxyethylene hydrogenated castor oil.

  ADVANTAGE OF THE INVENTION According to this invention, the dentifrice composition which is excellent in stability of (beta) -glycyrrhetinic acid, has high anti-inflammatory effect, there are few tastes and irritation | stimulations after use, saltiness is moderate, and it is excellent in a brushing feeling. The composition of the present invention is suitable for the prevention or treatment of periodontal diseases such as gingivitis.

  The dentifrice composition of the present invention is formulated with an appropriate ratio of sodium chloride and polyoxyethylene hydrogenated castor oil to a dentifrice composition containing β-glycyrrhetinic acid, and a combination of heavy calcium carbonate and oat extract. (A) β-glycyrrhetinic acid, (b) sodium chloride, (c) polyoxyethylene hydrogenated castor oil, (d) heavy calcium carbonate, and (e) apricot extract essential contains.

(A) Component β-glycyrrhetinic acid may be blended as a derivative of β-glycyrrhetinic acid, specifically β-glycyrrhetinic acid, β-glycyrrhetinic acid stearyl, β-glycyrrhetinic acid pyridoxine, β-glycyrrhetinic acid glycerin. However, it is not limited to these.
Commercially available products can be used as the component (a) β-glycyrrhetinic acid, for example, Maruzen Pharmaceutical Co., Ltd. type β-glycyrrhetic acid can be used. The blending amount of β-glycyrrhetinic acid is preferably 0.001 to 1% (mass%, hereinafter the same) with respect to the total amount of the composition, and particularly 0.005 to 0.5% from the viewpoint of anti-inflammatory effect and flavor. If it is less than 0.001%, sufficient medicinal effects may not be expected, and if it exceeds 1%, a nasty taste may occur.

As the sodium chloride as the component (b), a commercially available product can be used. For example, Sanuki salt A manufactured by Nihonkaikai Co., Ltd. can be used.
The amount of sodium chloride is preferably 5 to 20% with respect to the total amount of the composition, particularly 7 to 20%, particularly 10 to 15% from the viewpoint of the stability and flavor of β-glycyrrhetinic acid. If it is less than 5%, the stability of β-glycyrrhetinic acid may not be improved satisfactorily or a moderate salty taste may not be obtained, and if it exceeds 20%, irritation to the oral mucosa may occur.

  (C) Although it does not restrict | limit especially as polyoxyethylene hydrogenated castor oil of a component, What the average addition mole number of ethylene oxide is 10-60 mol is preferable at the point of the storage stability of (beta) -glycyrrhetic acid, Especially A 20-mol thing can be used conveniently. When the number of added moles is less than 10 moles, the storage stability of β-glycyrrhetinic acid may not be sufficient, and when it exceeds 60 moles, the storage stability of β-glycyrrhetinic acid may be insufficient.

  A commercial item can be used for such polyoxyethylene hydrogenated castor oil. For example, NIKKOL HCO-10 (polyoxyethylene (10) hydrogenated castor oil, manufactured by Nikko Chemicals Corporation), NIKKOL HCO-20 (polyoxyethylene (20) hydrogenated castor oil, manufactured by Nikko Chemicals Corporation), NIKKOL HCO-30 (Polyoxyethylene (30) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-40 (Polyoxyethylene (40) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-60 (Polyoxyethylene (60 ) Hardened castor oil, manufactured by Nikko Chemicals Co., Ltd.).

  (C) The compounding quantity of the polyoxyethylene hydrogenated castor oil of a component is 0.8 to 2.5% with respect to the composition whole quantity, Especially 0.8 to 2.2%, Especially 1 to 2% is preferable. If it is less than 0.8%, the irritation mitigation effect may not be exerted on the oral mucosa, and the stability of β-glycyrrhetinic acid may be inferior. If it exceeds 2.5%, the salty taste may be impaired and a nasty taste may occur. There is.

  The compounding ratio ((b) / (c)) of the sodium chloride of the component (b) to the polyoxyethylene hydrogenated castor oil of the component (c) is 5 to 15, and preferably 7 to 13 by mass ratio. If it is less than 5, the salty taste is impaired and an unpleasant taste occurs. If it exceeds 15, the effect of improving the stability of β-glycyrrhetinic acid is not satisfactorily exhibited, and irritation occurs to the oral mucosa.

  (D) As a heavy calcium carbonate of a component, the heavy calcium carbonate marketed generally can be used, and a manufacturer, goods, and a grade are not restrict | limited to this. For example, heavy calcium carbonate (product name: Softon 1000, Softon 1200, Softon 1500, Softon 1800) manufactured by Bihoku Flour Industry Co., Ltd. can be used.

  The blending amount of heavy calcium carbonate is 10 to 50% with respect to the total amount of the composition, and preferably 20 to 40% from the viewpoint of brushing feeling. If it is less than 10%, there may be cases where sufficient brushing feeling cannot be expected, and if it exceeds 50%, a muddy odor may occur.

The buckwheat extract of component (e) used in the present invention can be blended as a solvent extract of buckwheat of citrus family plants. Oat extract has an anti-inflammatory effect and is an ingredient that improves gingival inflammation, and has a bitter taste based on berberine as an active ingredient, and can mask the taste of the base material in the dentifrice composition.
As the extract of buckwheat, as an extraction solvent, for example, water, a lower alcohol having 1 or 2 carbon atoms such as ethanol and the like can be mentioned, and an extract with water is particularly preferable.
A commercially available product can be used as the above-mentioned Aoba extract, for example, a powder type Aoba extract manufactured by Ogi Pharmaceutical Co., Ltd. can be used.

  The compounding amount of the Aoba extract can be 0.005 to 0.5% with respect to the total amount of the composition, but the content of berberine is 0.0003 to 0.03 with respect to the total amount of the composition in terms of solid content. % Is desirable. In particular, in terms of anti-inflammatory effect and off-flavor masking, the compounding amount of Aoba extract is 0.02 to 0.2%, and the content of berberine is 0.0012 to 0.012% in terms of solid content. It is more preferable. If the extract is less than 0.005% or berberine is less than 0.0003%, sufficient anti-inflammatory effect and unpleasant masking effect may not be exhibited. If the extract is more than 0.5%, berberine If the content exceeds 0.03%, an unpleasant taste based on bitterness may develop.

  The dentifrice composition of the present invention can be prepared and applied as a toothpaste, liquid dentifrice, etc., in particular, as a toothpaste, and other appropriate known components in addition to the above components depending on the dosage form. It can mix | blend as needed. Optional components include, for example, wetting agents, (d) abrasives other than heavy calcium carbonate, (a) active ingredients other than (beta) -glycyrrhetinic acid and (e) buckwheat extract, (c) interfaces other than polyoxyethylene hydrogenated castor oil An activator, a binder, a fragrance, a pH adjuster, an antiseptic, a sweetener, a colorant, and the like can be mentioned, and they can be blended as long as the effects of the present invention are not hindered. The composition of the present invention can be produced by mixing these components and water by an ordinary method.

  As a wetting agent, glycerin, polyethylene glycol, propylene glycol, ethylene glycol, 1,3-butylene glycol, sugar alcohols such as reduced starch saccharified products, or one or more of polyhydric alcohols can be blended. In the case of a toothpaste, the blending amount of the wetting agent is preferably 5 to 50% with respect to the entire composition.

  As abrasives, silica-based abrasives such as silica gel, aluminosilicate, zirconosilicate, etc., dibasic calcium phosphate dihydrate, dibasic calcium phosphate anhydrous, phosphoric acid-based abrasives such as calcium pyrophosphate, aluminum hydroxide, alumina Titanium dioxide, crystalline zirconium silicate, polymethyl methacrylate, insoluble calcium metaphosphate, magnesium carbonate, tertiary magnesium phosphate, zeolite, zirconium silicate, hydroxyapatite, fluoroapatite, calcium deficient apatite, tertiary calcium phosphate, fourth One type or two or more types of calcium phosphate, eighth calcium phosphate, light calcium carbonate, synthetic resin-based abrasive and the like can be used. The blending amount of these abrasives is desirably in the range where the total blending amount including the component (d) is usually 10 to 50%, particularly 20 to 40% with respect to the total amount of the toothpaste.

  Examples of various active ingredients include fluorine compounds such as sodium fluoride, sodium monofluorophosphate and tin fluoride, enzymes such as dextranase and mutanase, and water-soluble phosphate compounds such as potassium phosphate and sodium salt of orthophosphate. , Tranexamic acid, epsilon-aminocaproic acid, allantoin, allantoinchlorohydroxyaluminum, hinokitiol, sodium lauroylsarcosine, ascorbic acid and its salts, dl-α-tocopherol acetate, dl-α-tocopherol nicotinate, dihydrocholesterol, α-bisabolol, Chlorhexidine salts, azulene, azulene sulfonate, glycyrrhizic acid and salts thereof, chelating phosphate compounds such as copper chlorophyllin sodium, chlorophyll, glycerophosphate, gluco Copper compounds such as copper acid, hydroxamic acid and its derivatives, sodium tripolyphosphate, zeolite, methoxyethylene maleic anhydride copolymer, polyvinylpyrrolidone, epidihydrocholesterin, cetylpyridinium chloride, benzethonium chloride, benzalkonium chloride, dihydro Examples include cholesterol, trichlorocarbanilide, zinc citrate, soft sugar beet extract, chamomile, clove, rosemary, ougon, safflower and the like. In addition, the compounding quantity of these active ingredients can be made into an effective quantity in the range which does not prevent the effect of this invention.

As the surfactant, a surfactant usually used in a dentifrice composition can be blended. Examples of anionic surfactants include sodium alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate, acyl sarcosine salts such as sodium lauroyl sarcosine and sodium myristoyl sarcosine, sodium dodecylbenzenesulfonate, hydrogenated coconut fatty acid sodium monoglyceride monosulfate, lauryl Examples include sodium 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, and the like.
Nonionic surfactants include those other than (c) component polyoxyethylene hydrogenated castor oil, such as polyoxyethylene alkyl ether, sucrose fatty acid ester, alkylol amide, polyoxyethylene sorbitan monostearate, polyoxyethylene Polyoxypropylene glycol, alkyl glucoside, polyglycerin fatty acid ester and the like are used.
Examples of the amphoteric surfactant include lauryl dimethylaminoacetic acid betaine, N-coconut oil fatty acid acyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, coconut oil fatty acid amidopropyldimethylaminoacetic acid betaine, and coconut oil fatty acid. Amidopropyl betaine or the like is used.
The blending amount of these surfactants can be in a range where the total blending amount including the component (c) is 0.8 to 5%.

  As binder, cellulose binder such as sodium carboxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxymethylethylcellulose, methylcellulose, xanthan gum, carrageenan, guar gum, sodium alginate, cationized cellulose, montmorillonite, gelatin , Sodium polyacrylate, and the like, and one or more of these can be blended. A compounding quantity is 0.1 to 5% normally with respect to the composition whole quantity.

  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, grapefruit oil, coconut oil, sweetie oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil , Patchouli oil, iris concrete, absolute peppermint, rose absolute, orange flower absolute, vanilla absolute, mango absolute, patchouli absolute, ginger oleoresin, pepper oleoresin, capsicum ole Natural fragrances such as resin and pepper extract, and fragrances and menthols processed by these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder fragrance, etc.) , Carboxyl, Anethole, Cineol, Methyl salicylate, Ethyl salicylate, Cynamic aldehyde, Eugenol, 3-l-Mentoxypropane-1,2-diol, Thymol, Linalol, Linaryl acetate, Limonene, Menthone, Menthyl acetate, Menthyl lactate , Phenoxyethyl isobutyrate, methyl jasmonate, N-substituted paramentane-3-carboxamide, pinene, octylaldehyde, pregon, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, ethyl lactate, hexyl Rubacetate, isoamyl acetate, allyl hexanoate, allyl cyclohexane propionate, methyl cinnamate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, gamma and delta lactones having 4 to 12 carbon atoms, yonon, caron, propyl Alcohol, butanol, benzyl alcohol, maltol, phenylethyl alcohol, isoamyl alcohol, n-hexenol, cis-3-hexenol, cis-6-nonenol, α-terpineol, ambretolide, dimethyl sulfide, cycloten, furaneol, ethylcyclopente Nolon, furfural, trimethylpyrazine, 2-methylbutyric acid, propionic acid, ethylthioacetate, monomenthyl succinate , Linalool oxide, vanillyl butyl ether, isopulegol, spirantol and other single flavors, strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, ume flavor, orange flavor, lemon flavor Used in combination with known perfume materials used in dentifrice compositions such as blended perfumes such as fruit mix flavors, tropical fruit flavors and tea flavors, and perfume solvents such as ethyl alcohol, propylene glycol, triacetin and glycerin fatty acid esters can do. Although the compounding quantity of these fragrance | flavor raw materials is not specifically limited, It is preferable to use 0.000001 to 1% in a composition. Moreover, as a fragrance | flavor for perfume using the said fragrance | flavor raw material, it is preferable to use 0.1 to 2.0% in a composition.

  Examples of pH adjusters include phthalic acid, phosphoric acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid, pyrophosphoric acid, glycerophosphoric acid and carbonic acid, and potassium salts, sodium salts and ammonium salts thereof, ribonucleic acid and salts thereof. Furthermore, 1 type (s) or 2 or more types, such as sodium hydroxide, can be normally added in the range which does not prevent the effect of this invention.

  Examples of the preservative include paraoxybenzoic acid esters such as butylparaben, propylparaben, ethylparaben and methylparaben, benzoic acid such as sodium benzoate or a salt thereof, potassium sorbate and the like.

  Examples of sweeteners include saccharin sodium, xylitol, erythritol, maltitol, lactitol, aspartame, neotame, stevioside, sucralose, monelin, neohesperidin, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, etc.

As colorants, in addition to dyes defined by legal dyes such as Blue No. 1, Yellow No. 4 and Red No. 106, Spirulina Blue Dye, Gardenia Blue, Casamas Yellow, Crotin, Casa Mashed, Beat Red, Cochineal Dye Natural pigments such as ultramarine, natural pigments such as ultramarine, bitumen, and bengara can be used.
In addition, the compounding quantity of these components can be made into a normal quantity in the range which does not prevent the effect of this invention.

  As a container, the material of the container to accommodate is not restrict | limited in particular, Usually, containers, such as polyethylene used for a toothpaste composition and a liquid dentifrice composition, can be used.

  Hereinafter, although the example and comparative example which correspond to the dentifrice composition of this invention are shown and the characteristic and effect of this invention are demonstrated concretely, this invention is not restrict | limited to a following example. In the following examples,% is mass% unless otherwise specified.

Examples and comparative examples
Toothpaste compositions having the compositions shown in Tables 1 to 3 were prepared by the following production method. In addition, the comparative example was prepared according to the following method.
Manufacturing method:
(1) A phase was prepared by mixing and dissolving water-soluble components (excluding the binder and propylene glycol) such as saccharin and sorbite in purified water at room temperature.
(2) A phase B was prepared in which a buckwheat extract and a binder were dispersed at room temperature in propylene glycol.
(3) B phase was added and mixed in A phase under stirring, and C phase was prepared.
(4) In phase C, ingredients other than water-soluble ingredients such as fragrances, abrasives, surfactants and β-glycyrrhetinic acid are mixed at room temperature using a 1.5 L kneader (manufactured by Ishiyama Shoten), and removed by decompression. Foaming (pressure 4 kPa) was performed to obtain 1.5 kg of a dentifrice composition.

  For the preparation of these dentifrice compositions, the Aoba extract is manufactured by Oshiro Pharmaceutical Co., Ltd., β-glycyrrhetinic acid is manufactured by Maruzen Pharmaceutical Co., Ltd., sodium chloride is Sanuki salt A manufactured by Nihonkaisui Co., Ltd., and heavy calcium carbonate is Bihoku. NIKKOL HCO-20 manufactured by Nikko Chemicals Co., Ltd. was used as Softon 1000 manufactured by Powdered Industries Co., Ltd. and polyoxyethylene hydrogenated castor oil. In addition, the outside standard (standard product quasi-drug) standard product was used for sodium lauryl sulfate, silicic anhydride, sodium carboxymethylcellulose, propylene glycol, sodium saccharin, and purified water. The pure sorbitol was 70%. About the fragrance | flavor, it mix | blended using the fragrance | flavor composition AI shown in Table 4 (using the flavor composition shown in Tables 5-10).

The prepared dentifrice composition was a laminated tube (LDPE55 / PET12 / LDPE20 / white LDPE60 / EMAA20 / AL10 / EMAA30 / LDPE20 / LLDPE30, thickness 257 μm) whose innermost layer was made of linear low-density polyethylene and had a diameter of 26 mm and an inner diameter of 8 mm. (Dai Nippon Printing Co., Ltd.)) was filled with 50 g.
The abbreviations and names in the layer structure of the laminated tube used are as follows, and the numbers following the abbreviations indicate the thickness (μm) of each layer.
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

  About the obtained dentifrice composition, (1) stability of β-glycyrrhetinic acid, (2) anti-inflammatory effect, (3) no taste after use, (4) no irritation after use, (5) Saltiness and (6) brushing feeling were evaluated by the following methods. The results are shown in Tables 1-3.

(1) Stability of β-glycyrrhetinic acid Immediately after preparation of the dentifrice composition (initial) and after storage at 60 ° C. for 1 month, 5 g is extruded from the laminated tube, and the content of β-glycyrrhetinic acid in the preparation in each tube is determined. The residual ratio was calculated by the following method.
An internal standard solution (fluoranthene in methanol) and a methanol / water / acetic acid (100) mixture (900: 100: 1) were added to the dentifrice composition, and the mixture was uniformly dispersed, and then a liquid chromatography filter (0.45 μm). ) To prepare a sample solution. If necessary, it may be centrifuged after uniform dispersion. Separately, β-glycyrrhetinic acid for quantification was diluted with a methanol / water / acetic acid (100) mixture (900: 100: 1), and then the internal standard solution was accurately added to obtain a standard solution. The sample solution and 20 μL of the standard solution were tested by liquid chromatography under the following conditions. QT (the ratio of the peak area of β-glycyrrhetinic acid of the sample solution to the peak area of the internal standard substance) and QS (peak of the internal standard substance) The ratio of the peak area of β-glycyrrhetinic acid of the standard solution to the area was determined. The β-glycyrrhetinic acid content was determined according to the following formula, and the β-glycyrrhetinic acid residual rate was calculated.

β-glycyrrhetinic acid content (%) = WS × QT / QS × 1 / WT
WS: Amount of β-glycyrrhetinic acid for quantification (g)
WT: Sample amount (g)
Operation conditions of internal standard substance fluoranthene in methanol Detector: UV absorption photometer (measurement wavelength: 250 nm)
Column: ODS column Column temperature: Room temperature Mobile phase: Methanol / water / acetic acid (100) mixture = 28/11/1
Flow rate: Adjusted so that the retention time of β-glycyrrhetinic acid is about 25 minutes

β-glycyrrhetinic acid residual rate (%) =
[(Β-glycyrrhetinic acid content at the tube mouth after 1 month storage at 60 ° C.) / (Initial β-glycyrrhetinic acid content)] × 100

The stability of β-glycyrrhetinic acid was evaluated according to the following criteria.
(Evaluation criteria)
◎: β-glycyrrhetinic acid residual rate of 95% or more ○: β-glycyrrhetic acid residual rate of 90% or more and less than 95% Δ: β-glycyrrhetinic acid residual rate of 85% or more and less than 90% ×: β-glycyrrhetinic acid residual rate of less than 85%

(2) Anti-inflammatory effect The following method is used to administer a diluted solution obtained by diluting a dentifrice composition 4 times with purified water against incisor gingivitis in ODU rats (plaque adherent rats) to improve gingivitis. A verification experiment was performed to evaluate the anti-inflammatory effect.

  Ten ODU rats were grouped, weaned at 5 weeks of age, and MF powdered feed (Oriental Yeast Co., Ltd.) was freely ingested for 3 months to induce gingivitis in the incisor gingiva. The diluted solution was administered to the gingivitis part of these rats twice a day for 2 weeks. The gingiva before and 2 weeks after administration of the diluent was observed under a microscope. The improvement effect was evaluated in the following four stages, and the average score of 10 animals was shown in the table as ◎, ○, Δ, × according to the following criteria.

(Score)
4 points: remarkable improvement effect 3 points: improvement effect is seen 2 points: slight improvement effect is seen 1 point: no improvement effect is seen (evaluation criteria)
◎: 3.5 points to 4.0 points ○: 3.0 points to less than 3.5 points △: 2.0 points to less than 3.0 points ×: Less than 2.0 points

(3) No taste after use It evaluated by the sensory test using 10 expert panelists. About 1 g of the sample dentifrice composition was placed on a commercially available toothbrush and brushed for 3 minutes. The tastes felt after use were evaluated in the following 4 levels, and the average score of 10 people was evaluated according to the following criteria: ◎, ○, The results are shown in the table with Δ and ×.

(Score)
4 points: Does not feel any nasty taste 3 points: Feels slightly tasty 2 points: Feels tasty 1 point: Feels the nasty taste very strongly (Evaluation criteria)
◎: 3.5 points to 4.0 points ○: 3.0 points to less than 3.5 points △: 2.0 points to less than 3.0 points ×: Less than 2.0 points

(4) No irritation after use The sensory test using 10 expert panelists was used for evaluation. About 1 g of the dentifrice composition of the sample was placed on a commercial toothbrush and brushed for 3 minutes. The irritation felt after use was evaluated in the following four stages, and the average score of 10 people was evaluated according to the following criteria: ◎, ○, The results are shown in the table with Δ and ×.

(Score)
4 points: No stimulation at all 3 points: Slight stimulation but no problem in use 2 points: Feeling stimulation 1 point: Feeling stimulation very strongly (Evaluation criteria)
◎: 3.5 points to 4.0 points ○: 3.0 points to less than 3.5 points △: 2.0 points to less than 3.0 points ×: Less than 2.0 points

(5) Salty taste in use It evaluated by the sensory test using ten expert panelists. About 1 g of the sample dentifrice composition was placed on a commercially available toothbrush and brushed for 3 minutes. The saltiness felt during use was evaluated in the following four stages, and the average score of 10 persons was evaluated according to the following criteria. , Δ, × are shown in the table.

(Score)
4 points: feels moderately salty while brushing teeth, good feeling of use 3 points: feels slightly salty while brushing teeth, no problem in use 2 points: while brushing teeth , Almost no salty taste, poor usability 1 point: While brushing teeth, no salty feel at all, very bad usability (evaluation criteria)
◎: 3.5 points to 4.0 points ○: 3.0 points to less than 3.5 points △: 2.0 points to less than 3.0 points ×: Less than 2.0 points

(6) Cleaning feeling during use Evaluation was made by a sensory test using 10 expert panelists. About 1 g of the sample dentifrice composition was placed on a commercial toothbrush and brushed for 3 minutes. The brushing feeling felt during use was evaluated in the following four stages, and the average score of 10 people was evaluated according to the following criteria: , ○, Δ, × are shown in the table.

(Score)
4 points: Feeling of brushing very strongly while brushing teeth 3 points: Feeling of brushing while brushing teeth 2 points: Feeling of brushing slightly while brushing teeth 1 point: No brushing feeling while brushing teeth (Evaluation criteria)
◎: 3.5 points to 4.0 points ○: 3.0 points to less than 3.5 points △: 2.0 points to less than 3.0 points ×: Less than 2.0 points

From the results of Tables 1 to 3, when either (b) sodium chloride, (c) polyoxyethylene hydrogenated castor oil, (d) heavy calcium carbonate, or (e) buckwheat extract is missing, When the ratio of the component (c) is inappropriate (Comparative Example), the storage stability and anti-inflammatory effect of β-glycyrrhetinic acid are inferior, and the toothpaste of the present invention is inferior to taste and brushing feeling. Compositions (Examples) are excellent in stability and anti-inflammatory effect of β-glycyrrhetinic acid, and have an unpleasant taste and no irritation after use, a moderate salty taste during use, an excellent feeling of brushing, and a good feeling in use. As a result, it was found that these excellent characteristics were combined.
In addition, the same effect was acquired also when the fragrance | flavor composition BI was used instead of the fragrance | flavor composition A. FIG.

表中、部は質量部である（以下同様。）。

In the table, parts are parts by mass (the same applies hereinafter).

Claims (3)

  A dentifrice composition containing β-glycyrrhetinic acid is blended with sodium chloride and polyoxyethylene hydrogenated castor oil in a mass ratio of sodium chloride / polyoxyethylene hydrogenated castor oil in the range of 5 to 15, and heavy. A dentifrice composition comprising calcium carbonate and alum extract.   The dentifrice composition of Claim 1 containing 5-20 mass% of sodium chloride.   The dentifrice composition according to claim 1 or 2, comprising 0.8 to 2.5% by mass of polyoxyethylene hydrogenated castor oil.