JP2012158559A - Berberine-containing dentifrice composition, and stabilization method thereof - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a dentifrice composition excellent in stability of berberine, suppressing fading of a pigment, and holding stably a formulation color tone, concerning a dentifrice composition containing berberine and calcium carbonate, and to provide a method for improving stability of berberine in the dentifrice composition, and suppressing fading of the pigment.SOLUTION: This invention relates: to a dentifrice composition formed by blending (C) polyoxyethylene-hardened castor oil and (E) Blue No.1 and/or Red No.106 as pigments with a dentifrice composition containing (A) berberine and (B) calcium carbonate; and to a stabilization method thereof. The invention also relates: to a dentifrice composition formed by blending (D) sorbitol containing the amount of <0.045 mass% direct reducing sugar and the (E) component with a dentifrice composition containing (A) and (B) components; and to a stabilization method thereof.

Description

  The present invention relates to a dentifrice composition comprising berberine and calcium carbonate, and more specifically, a dentifrice composition having excellent berberine stability and suppressing discoloration of pigments and maintaining a stable color tone of the preparation. And a method for improving the stability of berberine and suppressing the fading of the pigment.

  Berberine is a kind of alkaloid having a unique astringent feeling, and is known to have an astringent anti-inflammatory effect and an antibacterial effect against oral bacteria. Conventionally, in order to effectively exhibit or improve the effects of periodontal disease prevention effect, caries prevention effect, tooth floss formation prevention effect in the oral cavity, etc., for dentifrice compositions, such as amber containing berberine It is known that a citrus family plant extract or a buttercup family plant extract such as auren is blended as an active ingredient (Patent Documents 1 to 6: JP-A-57-56415, 58-39615, 58). -57320, 61-36215, 62-155209, JP-A-2001-97837).

  Calcium carbonate is an abrasive widely used for dentifrices, and generally the appearance of a kneaded preparation can be maintained well by incorporating calcium carbonate. However, when berberine is used with calcium carbonate, which is widely used as an abrasive, it has been difficult to maintain berberine sufficiently stably.

Examples of the technique relating to the problem of decreasing the residual rate of berberine include the following.
First, the berberine residual rate decreases due to the presence of aldehyde fragrance blended in the fragrance composition blended in the oral composition for the purpose of fragrance. It is disclosed that a product and / or a buttercup family plant extract can be stabilized and blended (Patent Document 7: JP-A-63-63608).
In general, natural fragrances such as peppermint oil and spearmint oil contain a small amount of aldehyde-based fragrance that causes deterioration, and it has been found that the residual rate of berberine gradually decreases. As a means for solving deterioration due to such a cause, a method of blending modified mint oil (Patent Document 8: Japanese Patent Laid-Open No. 2000-72617) has been proposed.
Furthermore, it is disclosed that polyoxyethylene hydrogenated castor oil is effective for stabilizing berberine in a calcium carbonate-containing berberine-containing oral composition (Patent Document 9: JP 08-175941 A).

JP-A-57-56415 JP 58-39615 A JP 58-57320 A JP-A-61-36215 JP 62-155209 A JP 2001-97837 A JP 63-63608 A JP 2000-72617 A Japanese Patent Application Laid-Open No. 08-175941 JP 09-136844 A Japanese Patent Laid-Open No. 08-81344 International Publication No. 2005/108503 Pamphlet

  The present invention has been made in view of the above circumstances. In a dentifrice composition containing berberine and calcium carbonate, the dentifrice is excellent in berberine stability, the discoloration of the pigment is suppressed, and the color tone of the preparation is stably maintained. An object of the present invention is to provide a method for improving the stability of berberine in an agent composition and a dentifrice composition and suppressing the fading of a pigment.

  As a result of intensive studies to achieve the above object, the inventors of the present invention have developed a dentifrice composition containing berberine and calcium carbonate, polyoxyethylene hydrogenated castor oil, and blue No. 1 and / or red 106 as a pigment. It was found that, by blending with No. 1, the berberine is excellent in stability, and the color fading of the pigment is suppressed and the color tone of the preparation can be stably maintained.

  That is, as shown in Patent Document 9 above, it is known that berberine can be stabilized by adding polyoxyethylene hydrogenated castor oil to a dentifrice composition containing berberine and calcium carbonate. It is. The dentifrice composition containing berberine, calcium carbonate, and polyoxyethylene hydrogenated castor oil is colored yellow based on the blending of berberine, but it does not cause a significant problem in appearance. However, in order to give a better appearance to the berberine-containing dentifrice composition, when a pigment is blended to color other than yellow, for example, when green No. 3 is blended to color green, a stabilizer As a result, the stability of berberine is greatly reduced despite the incorporation of an effective polyoxyethylene hydrogenated castor oil.As a result, the incorporation of a pigment has a very adverse effect on the berberine stability of a berberine-containing dentifrice composition. Furthermore, it was found that the dye fades with time depending on the dye. Therefore, as a result of further investigation to improve this point, as a result of using a specific dye among various dyes, that is, blue No. 1 or red No. 106, surprisingly, a berberine-containing dentifrice composition The berberine stabilizing effect of polyoxyethylene hydrogenated castor oil is not adversely affected, and a good berberine-containing dentifrice composition is provided, and the above blue No. 1 or red No. 106 contains berberine. It has been found that the dentifrice composition has almost no fading even at high temperature and long-term storage, and the color tone of the berberine-containing dentifrice composition can be stably maintained over a long period of time.

  In addition, the applicant of the present invention can improve the stability of berberine in the same manner by previously blending a dentifrice composition containing berberine and calcium carbonate with sorbitol having a reducing sugar amount of less than 0.045% by mass. Although an improved dentifrice composition was proposed (Japanese Patent Application No. 2010-240538), when such a dentifrice composition is blended with a pigment such as Green No. 3, the stability of berberine is similarly deteriorated. When blue No. 1 or red No. 106 is used as a pigment, the berberine stabilizing effect by the sorbit is not inhibited, and a good berberine stabilizing effect is obtained, and blue No. 1 or red No. 106 is also faded. It has been found that there is no.

The green No. 3 has a chemical name of 2- [α- [4- (N-ethyl-3-sulfobenzyliminio) -2,5-cyclohexadienylidene] -4- (N-ethyl-3- Sulfobenzylamino) benzyl] -5-hydroxybenzenesulfonate disodium salt, while Blue No. 1 has the chemical name 2- [α- [4- (N-ethyl-3-sulfobenzyliminio) -2,5-Cyclohexadienylidene] -4- (N-ethyl-3-sulfobenzylamino) benzyl] benzenesulfonate, both of which are very similar in structure. Nevertheless, when Green No. 3 is used as described above, the stability of berberine is significantly impaired, whereas Blue No. 1 does not hinder the stability of berberine, which is unexpected. This is the effect of this.
Red 106 is similar to Red 3 and Red 104 (1) in its main skeleton, but Red 106 is similar to Blue 1 in the group bonded to the benzene ring. In that case, it seems that the group bonded to the benzene ring affects the stability and discoloration of berberine, but the reason why Green No. 3 and Red No. 106 give the above-mentioned effects still remains. It is unknown.

  Accordingly, Patent Documents 10 to 12 (Japanese Patent Laid-Open Nos. 09-136844, 08-81344, and WO 2005/108503 pamphlets) have been proposed as techniques relating to dye stabilization. It is difficult to expect that berberine can be stabilized by technology and the discoloration of blue No. 1 and red No. 106 is suppressed.

Accordingly, the present invention provides a dentifrice composition and a dentifrice composition described below and a method for suppressing the fading of a pigment while improving the stability of berberine.
Claim 1:
To a dentifrice composition containing (A) berberine and (B) calcium carbonate, (C) polyoxyethylene hydrogenated castor oil, and (E) blue No. 1 and / or red No. 106 as a pigment. A dentifrice composition characterized by being formulated.
Claim 2:
A dentifrice composition containing (A) berberine and (B) calcium carbonate; (D) a sorbite having a direct reducing sugar content of less than 0.045% by mass; A dentifrice composition containing Red 106.
Claim 3:
Furthermore, the dentifrice composition of Claim 2 which mix | blended (C) polyoxyethylene hydrogenated castor oil.
Claim 4:
A dentifrice composition containing (A) berberine and (B) calcium carbonate is blended with (C) polyoxyethylene hydrogenated castor oil, and (E) blue No. 1 and / or red 106 as a pigment. A method for improving the stability of berberine in the dentifrice composition and suppressing the fading of the pigment, characterized in that No. is used.
Claim 5:
A dentifrice composition containing (A) berberine and (B) calcium carbonate is blended with (D) a sorbit having a direct reducing sugar content of less than 0.045% by mass, and (E) blue as a pigment. A method for improving the stability of berberine in the dentifrice composition and suppressing the fading of the pigment, characterized by using No. 1 and / or Red No. 106.

  ADVANTAGE OF THE INVENTION According to this invention, in the dentifrice composition which mix | blended berberine and calcium carbonate, the dentifrice which is excellent in the stability of berberine, does not produce the discoloration of blue No. 1 and red No. 106, and can maintain the color tone of a formulation stably. An agent composition can be provided.

Hereinafter, the present invention will be described in more detail. In the present invention, the first invention includes (A) berberine and (B) a dentifrice composition containing calcium carbonate, (C) polyoxyethylene hydrogenated castor oil, (E) blue No. 1 and / or as a pigment. Red No. 106 is blended, and the second invention includes (D) a sorbite having a direct reducing sugar amount of less than 0.045% by mass, and (E) a blue No. 1 and a dye as a pigment. / Or red 106.
That is, the dentifrice composition of the present invention comprises (A) berberine, (B) calcium carbonate, (C) polyoxyethylene hydrogenated castor oil and / or (D) a direct reducing sugar content of less than 0.045% by mass. (E) Blue No. 1 and / or Red No. 106 are contained.

  The berberine as the component (A) used in the present invention can be formulated as a solvent extract of a plant containing berberine, in particular, a solvent extract of a citrus family plant such as a buckwheat or a buttercup family plant such as abalone. In addition, well-known things can be used as these plant extracts. As such a berberine-containing plant extract, a commercially available product may be used, and for example, it can be obtained under the product names of “Obaku extract” manufactured by Ogi Seiyaku Co., Ltd. and “Ouren extract” manufactured by Alps Pharmaceutical Co., Ltd. Moreover, these plant extracts may be used individually by 1 type, and may use 2 or more types together.

  The blending amount of the berberine-containing plant extract is preferably 0.0005 to 0.05% (mass%, the same applies hereinafter) of the whole composition in terms of pure content as berberine, and in particular, the astringent effect and the storage stability of berberine. 0.001% or more is preferable from the aspect of the above, and 0.02% or less is preferable from the viewpoint of the taste after storage and the appearance of the kneaded skin during storage. If it is less than 0.0005%, the storage stability of berberine may be inferior. If it exceeds 0.05%, discoloration of the pigment may not be suppressed, and in particular, discoloration may not be sufficiently suppressed when a berberine-containing plant extract is blended.

The calcium carbonate as the component (B) is blended as an abrasive or an extender pigment and is not particularly limited as long as it is used in a dentifrice composition, but heavy calcium carbonate is preferred.
As such calcium carbonate, commercially available products can be used, and examples thereof include heavy calcium carbonate (product names: Softon 1000, Softon 1200, Softon 1500, Softon 1800) manufactured by Bihoku Powder Chemical Co., Ltd.

  The blending amount of calcium carbonate is preferably 1 to 50%, particularly 10 to 40%, especially 15 to 35% of the whole composition. If it exceeds 50%, the storage stability of berberine may be inferior, and the fading of the pigment may not be suppressed.

  In the present invention, (C) polyoxyethylene hydrogenated castor oil and / or (D) sorbitol having a direct reducing sugar content of less than 0.045% is used as the berberine stabilizer.

  (C) As polyoxyethylene hydrogenated castor oil, an average added mole number of ethylene oxide is preferably 5 to 80 mol, particularly 10 to 80 mol, particularly 20 to 60 mol, from the viewpoint of storage stability of berberine. . If the amount is less than 5 mol, the storage stability of berberine may not be sufficiently improved, and if it exceeds 80 mol, the storage stability of berberine may not be sufficiently improved.

  A commercial item can be used for such polyoxyethylene hydrogenated castor oil, for example, NIKKOL HCO-5 (polyoxyethylene (5) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-20 (polyoxy). Ethylene (20) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd., NIKKOL HCO-10 (polyoxyethylene (10) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-20 (polyoxyethylene (20) hydrogenated castor Oil, manufactured by Nikko Chemicals Co., Ltd., NIKKOL HCO-30 (polyoxyethylene (30) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-40 (polyoxyethylene (40) hydrogenated castor oil, Nikko Chemicals Co., Ltd.) Made), NIKKOL HCO 60 (polyoxyethylene (60) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.) NIKKOL HCO-80 (polyoxyethylene (80) hydrogenated castor oil, manufactured by Nikko Chemicals Co., Ltd.).

  (C) The compounding quantity of polyoxyethylene hydrogenated castor oil is 0.3 to 5% of the whole composition, and 0.8 to 3% is especially suitable. If the blending amount is less than 0.3%, the storage stability of berberine may not be sufficiently improved. If it exceeds 5%, the suppression of fading of the pigment may be insufficient due to the influence of impurities contained in the polyoxyethylene hydrogenated castor oil.

The component (D) is a sorbite having a direct reducing sugar content of less than 0.045%, preferably less than 0.030% with respect to pure sorbitol.
The above-mentioned direct reducing sugar content can be measured according to the method for measuring the amount of sorbite direct reducing sugar in JIS K1509.
Sorbit is usually used as an aqueous solution containing 60 to 70% of pure sorbitol from the viewpoint of usability. In the present invention, sorbit indicates an aqueous solution containing sorbitol.
As such a sorbit, what is marketed by the product name of NEOSORB70 / 02SB made from Rocket Japan, etc. can be used, for example.

(D) The compounding quantity of the sorbitol of a component is 10-45% of the whole composition as a pure sorbitol, Especially 15-35% is preferable. If it is less than 10%, the dry resistance of the dentifrice composition may be reduced, and the appearance of the kneaded skin after storage may be deteriorated. If it exceeds 45%, the amount of direct reducing sugar in the entire composition increases, and berberine May have poor storage stability and convergence effect.
It should be noted that only the sorbitol having the above-mentioned direct reducing sugar amount is blended as the sorbite, and the other sorbits may not be blended.

  The blending ratio of the pure sorbitol (D) component / berberine (A) component is preferably 350 to 70,000, particularly 700 to 40,000, especially 2,000 to 30,000, in terms of mass ratio. 000 to 25,000 is most preferable. When the blending ratio is less than 350, the appearance of the kneaded skin after storage may be inferior, and when it exceeds 70,000, the stability of berberine, and further, the discoloration suppressing effect of the pigment may not be sufficiently improved.

The component (E) used in the present invention is Blue No. 1 and / or Red No. 106, which is a pigment that does not reduce the storage stability of berberine in a dentifrice containing calcium carbonate, and is a fading color in this dentifrice composition. It is a pigment with a small amount. This pigment is formulated to make the color tone of a normally yellow berberine-containing dentifrice composition green or orange.
Blue No. 1 is also known as brilliant blue FCF, chemical name 2- [α- [4- (N-ethyl-3-sulfobenzyliminio) -2,5-cyclohexadienylidene] -4- (N- It is known as the disodium salt of ethyl-3-sulfobenzylamino) benzyl] benzenesulfonate, and can be obtained from Sakai Kasei Co., Ltd., Koyo Chemical Co., Ltd., and Saneigen FFI Co., Ltd.
Red 106 is also known as Acid Red, chemical name 9- (2′-sulfonium-4′-sulfophenyl) -6-diethylamino-3- (N, N-diethylimino) -3-isoxanthene-sodium. It can be obtained from Sakai Kasei Co., Ltd., Koyo Chemical Co., Ltd., and Saneigen FFI Co., Ltd.

  (E) The compounding quantity of the pigment | dye of a component is 0.00005 to 0.005% of the whole composition, It is preferable to set it as 0.0001 to 0.0002% especially. If it is less than 0.00005%, the colorability may be inferior or fading may occur. Conversely, if it exceeds 0.005%, the storage stability of berberine may be deteriorated.

  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 ingredients in addition to the above ingredients depending on the dosage form. Can be blended. For example, (D) wetting agents other than sorbit, (B) abrasives other than calcium carbonate, (A) active ingredients other than berberine, (C) surfactants other than ingredients, binders, fragrances, pH adjusters, Examples include preservatives, sweeteners, colorants other than the component (E), and the like. 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. (D) The blending amount of the wetting agent including sorbit is preferably 10 to 70% in the case of a toothpaste and 20 to 90% in the case of a liquid dentifrice with respect to the entire composition.
In the first invention, there is no problem in the stability of berberine because (C) polyoxyethylene hydrogenated castor oil is blended even if a normal sorbite is used as the sorbite, but in the case of the first invention, A specific sorbit (a sorbit having a direct reducing sugar content of less than 0.045%) can be used.

  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, tribasic magnesium phosphate, zeolite, zirconium silicate, tribasic calcium phosphate, hydroxyapatite, fluoroapatite, calcium deficient apatite, tribasic calcium phosphate 1 type (s) or 2 or more types can be used for 4th calcium phosphate, 8th calcium phosphate, a synthetic resin type abrasive | polishing agent, etc. The blending amount of the abrasive including calcium carbonate as the component (B) is usually 0 to 50%, particularly 5 to 50% with respect to the total amount of the composition in the case of the toothpaste, and the composition in the case of the liquid dentifrice. It is 0 to 30%, particularly 5 to 30%, based on the total amount.

  As various active ingredients, in addition to the berberine of the component (A), other active ingredients such as fluorine compounds such as sodium fluoride, sodium monofluorophosphate and tin fluoride, enzymes such as dextranase and mutanase, Water-soluble phosphate compounds such as potassium salt and sodium salt of phosphate, tranexamic acid, epsilon-aminocaproic acid, allantoin, allantochlorohydroxyaluminum, hinokitiol, sodium lauroylsarcosine, ascorbic acid and its salt, dl-α-tocopherol acetate, Nicotinic acid dl-α-tocopherol, dihydrocholesterol, α-bisabolol, chlorhexidine salts, azulene, azulene sulfonate, glycyrrhizic acid and its salts, glycyrrhetinic acid, copper chlorophyllin sodium, chloro , Chelating phosphate compounds such as glycerophosphate, copper compounds such as copper gluconate, hydroxamic acid and its derivatives, sodium tripolyphosphate, zeolite, methoxyethylene maleic anhydride copolymer, polyvinylpyrrolidone, epidihydrocholesterin, Examples thereof include extracts of cetylpyridinium chloride, benzethonium chloride, benzalkonium chloride, dihydrocholesterol, trichlorocarbanilide, zinc citrate, sugar beet extract, chamomile, clove, rosemary, oxon, 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, in addition to the polyoxyethylene hydrogenated castor oil as component (C), other surfactants usually used in dentifrice compositions 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, for example, polyoxyethylene alkyl ether, sucrose fatty acid ester, alkylol amide, polyoxyethylene sorbitan monostearate, polyoxyethylene polyoxypropylene glycol, alkyl glucoside, polyglycerin fatty acid ester, etc. It is done. 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 is such that the total blending amount including the component (C) is usually in the range of 0.3 to 5%.
In the case of the second invention, polyoxyethylene hydrogenated castor oil is not essential, but may be blended.

  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 can be mentioned, and these can be used alone or in combination of two or more. 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 processed with these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder fragrance, etc.), and menthol , 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 Acetate, isoamyl acetate, allyl hexanoate, allyl cyclohexane propionate, methyl cinnamate, methyl anthranilate, ethyl methyl phenyl glycidate, linalyl acetate, 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, ethyl Cyclopentenolone, furfural, trimethylpyrazine, 2-methylbutyric acid, propionic acid, ethylthioacetate, mono Single fragrances such as ntil succinate, linalool oxide, vanillyl butyl ether, isopulegol, spirantol, strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, ume flavor, orange Known perfume materials used in dentifrice compositions such as flavors, lemon flavors, fruit mix flavors, tropical fruit flavors, tea flavors, and other flavoring solvents such as ethyl alcohol, propylene glycol, triacetin, and glycerin fatty acid esters Can be used in combination. 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, sodium hydroxide etc. are mentioned, These 1 type (s) or 2 or more types can be normally added in the range which does not interfere with 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 the sweetener include saccharin sodium, xylitol, erythritol, maltitol, lactitol, aspartame, neotame, stevioside, sucralose, monelin, neohesperidin, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone and the like.

  As the colorant, it is not necessary to add other than the dye of the component (E), but in addition to the dye specified by the legal dye such as Yellow No. 4 within the range not hindering the effect of the present invention, the spirulina blue dye, Natural pigments such as gardenia blue, casamas yellow, crottin, cassama red, beet red, cochineal pigments, natural pigments such as ultramarine blue, bitumen, bengara and the like may be added.

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

  Hereinafter, although an example and a comparative example are shown and the feature and effect of the present invention are explained concretely, the present invention is not restricted to the following examples. In the following examples,% is mass% unless otherwise specified.

Examples and comparative examples
Dentifrice compositions having the compositions shown in Tables 4 to 8 were prepared by the following production methods and evaluated by the following methods. The results are shown in Tables 4-8.
(Production method)
(I) A phase was prepared by mixing and dissolving water-soluble components (excluding binder and propylene glycol) such as saccharin and sorbite in purified water at room temperature.
(Ii) A phase B in which a plant extract containing berberine in propylene glycol and a binder was dispersed at room temperature was prepared.
(Iii) B phase was added and mixed in A phase under stirring, and C phase was prepared.
(Iv) In the C phase, ingredients other than water-soluble components such as fragrances, abrasives and anionic surfactants are mixed at room temperature using a 1.5 L kneader (manufactured by Ishiyama Shoten), and degassed by depressurization (pressure) 4 kPa) to obtain 1.5 kg of a dentifrice composition.

For the preparation of these dentifrice compositions, amber extract (water-dried extract, berberine content 6.0%, manufactured by Koshiro Pharmaceutical Co., Ltd.), calcium carbonate (Softon 1500 manufactured by Bihoku Flour Industry Co., Ltd.), polyoxyethylene Hardened castor oil (NIKKOL HCO-5 (manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-20 (manufactured by Nikko Chemicals Co., Ltd.), NIKOL HCO-40 (manufactured by Nikko Chemicals Co., Ltd.), NIKKOL HCO-80 (manufactured by Nikko Chemicals Co., Ltd.) In addition, the standard product of the original genus (quasi-drug raw material standard) was used for sodium lauryl sulfate, silicic anhydride, sodium carboxymethylcellulose, propylene glycol, sodium saccharin, and purified water. (All manufactured by Tsubaki Kasei Co., Ltd.) The sorbite was as shown in Table 2, and the sorbite solution used was a pure sorbate of 70% .The direct reducing sugar content was determined by the method for measuring the amount of sorbite directly reducing sugar in JIS K1509. Is a value measured according to
About the fragrance | flavor, what is shown in below-mentioned Tables 9-15 was used.

The dentifrice composition thus obtained was a laminate tube (LDPE55 / PET12 / LDPE20 / white LDPE60 / EMAA20 / AL10 / EMAA30 / LDPE20 / LLDPE30, thickness 26 mm, inner diameter layer made of linear low-density polyethylene and having an inner diameter of 8 mm. 257 μm (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

The storage stability of berberine in the dentifrice composition and the discoloration after storage were evaluated by the following methods.
(1) Storage stability of berberine Immediately after preparing the dentifrice composition and storing it in a container, and after storing at 50 ° C. for 3 months, the berberine content was determined and evaluated by the following method.
An internal standard solution (quinoline yellow SS in methanol) and a mobile phase were added to the dentifrice composition and dispersed uniformly, and then filtered using a liquid chromatography filter (0.45 μm) to obtain a sample solution. Centrifugation was performed after uniform dispersion as necessary. Separately, standard berberine chloride was dissolved in methanol, diluted with the mobile phase according to the berberine concentration of the composition, and then the internal standard solution was accurately added to obtain a standard solution. A 20 μL sample solution and a standard solution were tested by liquid chromatography under the following conditions. QT (ratio of the peak area of berberine of the sample solution to the peak area of the internal standard substance) and QS (standard with respect to the peak area of the internal standard substance) The ratio of the peak area of berberine in the solution) was determined, the berberine content was determined by the following formula, and the berberine residual ratio was calculated.

Berberine content (ppm) =
WS × (100-D) × (353.37 / 371.81) × (QT / QS) ×
(K / WT)
WS: Standard amount of berberine chloride (g)
WT: Sample amount (g)
D: Moisture content of standard berberine chloride (%)
K: Constant (set by dilution concentration, etc.)
353.37: Molecular weight of berberine 371.81: Molecular weight of berberine chloride

Internal standard substance Quinoline Yellow SS methanol solution operating conditions Detector: UV absorption photometer (measurement wavelength: 345 nm)
Column: ODS column Column temperature: Room temperature Mobile phase: Water / acetonitrile / methanol = 2/2/1
(Add appropriate amount of sodium lauryl sulfate and tartaric acid)
Flow rate: Adjusted so that the retention time of berberine is about 20 minutes

Berberine remaining rate (%) =
[(Berberine content at the tube mouth after storage at 50 ° C. for 3 months) / (initial berberine content)] × 100

The storage stability of berberine was evaluated according to the following criteria.
(Evaluation criteria)
◎: Berberine remaining rate of 96% or more ○ to ◎: Berberine remaining rate of 93% or more and less than 96% ○: Berberine remaining rate of 90% or more and less than 93% Δ: Berberine remaining rate of 85% or more and less than 90% ×: Berberine remaining rate of 85% Less than

(2) Amber after storage Immediately after preparing the dentifrice composition and storing it in a container, and for the dentifrice composition after storage at 50 ° C. for 3 months, the absorbance of the dye was determined and evaluated by the following method.
60 vol% ethanol was added to the dentifrice composition and dispersed uniformly, and then centrifuged to obtain a sample solution. The absorbance at the maximum absorption wavelength of each dye was measured and evaluated by the residual ratio (%) when the absorbance immediately after preparing the dentifrice composition was taken as 100%. The measurement wavelength of the absorbance of each dye is as shown in Table 3.

  In addition, in order to remove the influence of absorbance derived from the components of the dentifrice composition, a dentifrice composition excluding Blue No. 1 was prepared from the dentifrice composition of Example 1, and stored immediately after preparation and at 50 ° C. for 3 months. Later, the absorbance was measured at the same wavelength to obtain a blank.

The discoloration after storage was evaluated according to the following criteria.
(Evaluation criteria)
A: Absorbance remaining rate of 85% or more ○ to ◎: Absorbance remaining rate of 80% or more and less than 85% ○: Absorbance remaining rate of 70% or more and less than 80% Δ: Absorbance remaining rate of 50% or more and less than 70% ×: Absorbance Residual rate of less than 50%

表中、部はいずれも質量部である（以下、同様。）。

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

Claims (5)

  To a dentifrice composition containing (A) berberine and (B) calcium carbonate, (C) polyoxyethylene hydrogenated castor oil, and (E) blue No. 1 and / or red No. 106 as a pigment. A dentifrice composition characterized by being formulated.   A dentifrice composition containing (A) berberine and (B) calcium carbonate; (D) a sorbite having a direct reducing sugar content of less than 0.045% by mass; A dentifrice composition containing Red 106.   Furthermore, the dentifrice composition of Claim 2 which mix | blended (C) polyoxyethylene hydrogenated castor oil.   A dentifrice composition containing (A) berberine and (B) calcium carbonate is blended with (C) polyoxyethylene hydrogenated castor oil, and (E) blue No. 1 and / or red 106 as a pigment. A method for improving the stability of berberine in the dentifrice composition and suppressing the fading of the pigment, characterized in that No. is used.   A dentifrice composition containing (A) berberine and (B) calcium carbonate is blended with (D) a sorbit having a direct reducing sugar content of less than 0.045% by mass, and (E) blue as a pigment. A method for improving the stability of berberine in the dentifrice composition and suppressing the fading of the pigment, characterized by using No. 1 and / or Red No. 106.