JP5720416B2 - Gel oral composition and method for producing the same - Google Patents

Description

  The present invention is excellent in shape retention and phase-liquid separation stability, and has good oral cavity composition that prevents the oral composition from dripping from the mouth when brushed in the oral cavity. The present invention relates to a gel-like composition for oral cavity and a method for producing the same, which are compatible with contradictory functions such as good spread of the composition for oral cavity and exhibit a satisfactory cleaning effect in the oral cavity.

  It is known that oral compositions such as dentifrices are useful not only for daily oral care hygiene products but also for the prevention of dental caries and periodontal diseases. Further, in the composition for oral cavity, when applying to a cleaning tool such as a toothbrush when performing oral cleaning, it is an essential condition that it has shape retention as a dentifrice or the like and does not cause phase separation. In order to exert a sufficient cleaning effect in the oral cavity, it has a good retention to prevent liquid dripping from the oral cavity, and the oral composition in the oral cavity in a short act of oral cleaning It is said that it is useful to have a spread in the oral cavity that the object spreads.

  As means for improving the shape-retaining property when applied to cleaning tools such as toothbrushes, conventional clay agents such as synthetic layered sodium silicate / magnesium and synthetic hectorite, carboxyvinyl polymer and sodium polyacrylate are used. It is an effective means to mix a synthetic water-soluble polymer substance into an oral composition, and among these components blended into the oral composition, the clay agent has a higher shape retention. It has been known.

  As means for improving the activity of the preparation by utilizing the high shape retention of the clay agent, a toothpaste composition containing a peroxydiphosphate containing synthetic hectorite, silica, hydrated alumina, and a humectant (see Patent Document 1) A casein composition for transporting a bioactive ingredient containing a clay agent and casein protein (see Patent Document 2), a dentifrice composition containing no abrasive containing a hydrophilic clay agent and a phytic acid compound ( Patent Document 3), and a dentifrice composition (see Patent Document 4) in which a hydrophilic clay agent, a modified cellulose polymer, a carboxyvinyl polymer, and natural rubber-derived anionic polymers are blended has been proposed.

Japanese Patent Publication No. 3-36803 JP-T-2002-521415 Special table 2009-513695 gazette Special table 2009-519235 gazette

  However, in any of the techniques, it is difficult to ensure the shape retention over time, or it may hang down from the mouth during use and cannot be satisfactorily maintained in the oral cavity. It was difficult to satisfy the contradictory function of goodness at the same time. In addition, these techniques have problems such as phase-liquid separation over time, and it is difficult to say that the cleaning effect in the oral cavity is sufficient, and there is still room for improvement. In the composition for oral cavity, it is desired to improve the cleaning effect in the oral cavity. However, in the prior art, the shape retention with time and the phase separation stability are excellent, and the retention in the oral cavity and the spread in the oral cavity are excellent. It has been difficult to obtain a composition for oral cavity that balances goodness and satisfies all these characteristics.

  The present invention has been made in view of the above circumstances, and is excellent in aging shape retention and phase-liquid separation stability, and has both good retention in the oral cavity and good spread in the oral cavity. It aims at providing a composition and its manufacturing method.

As a result of intensive studies to achieve the above object, the inventors of the present invention have found that at least one selected from synthetic layered sodium silicate / magnesium (a), sodium carboxymethylcellulose, hydroxyethylcellulose, sodium alginate, xanthan gum, and carrageenan. The water-soluble polymer substance (b) is used in combination at a water content of 15 to 50% by mass, and in particular, the ratio (b) / (a) in the above components (a) and (b) is 0.4 to 7 and the inclusion of an anionic surfactant (c) satisfies the shape retention property and phase-liquid separation stability, and the oral composition droops from the mouth when brushed in the oral cavity. Usability that balances good retention in the oral cavity with no spread and good spread in the oral cavity where the oral composition spreads well in the oral cavity It was found that good gel oral composition.

That is, the components (a), (b), and (c) have been conventionally known as components for oral compositions, and when a clay agent is added to oral compositions such as toothpastes, the shape retention and the like are improved. It is known that it can be done. However, a paste-like oral composition such as a toothpaste generally containing a water-soluble polymer substance is a pseudoplastic fluid having a yield value, and has a certain solid-like property in a state where no external force is applied. However, when a large external force is applied, the bond due to internal stress is broken and changes to liquid properties.For this reason, when the yield value is increased by improving the shape retention and retention in the oral cavity, As a result, it was difficult to make these conflicting characteristics compatible. Furthermore, in a gel-form preparation with a large amount of water, it is more difficult to maintain the shape-retaining property although it tends to spread into the oral cavity, and it is more difficult to achieve both of these properties.
In contrast, the present inventors have provided an aqueous solution of one or more water-soluble polymer substances selected from sodium carboxymethyl cellulose, hydroxyethyl cellulose, sodium alginate, xanthan gum, and carrageenan, and an aqueous solution of synthetic layered sodium silicate / magnesium silicate. In particular, in this case, by adjusting the ratio of the water-soluble polymer substance and the synthetic layered sodium silicate / magnesium, an organic-inorganic composite thickener having high thixotropy is provided, and the water content is 15 It was found that a gel-like composition giving the above-mentioned effect can be obtained by adding an anionic surfactant (c) in addition to this at ˜50% by mass, which is determined by the present inventors. This is a new finding.

  More specifically, as shown in the experimental examples described later, the synthetic layered sodium silicate / magnesium does not substantially exhibit thixotropic properties in a low-concentration aqueous solution, while the aqueous solution of the water-soluble polymer substance has a certain amount. Although thixotropy is shown, the thixotropy of an aqueous solution in which an aqueous solution of the above water-soluble polymer substance and an aqueous solution of a synthetic layered sodium silicate / magnesium solution are used in combination with both of these components, although the value is small. Synergistically with each other, and at least 1.1 times the thixotropy of the above water-soluble polymer substance aqueous solution, especially about 2 times or more thixotropic properties in the case of a sodium carboxymethyl cellulose aqueous solution, a hydroxyethyl cellulose aqueous solution, and a xanthan gum aqueous solution. And thus the organic-inorganic composite obtained in this way Increasing viscous is effective as increasing Nebamoto material of the gel oral compositions was found that acts effectively in providing the above effects. In this case, the thixotropic improvement effect is obtained by using and mixing an aqueous solution of the water-soluble polymer substance and an aqueous solution of synthetic layered sodium silicate / magnesium, and these components are not in an aqueous solution state. Even if they are mixed together, or the mixture is dissolved in water and an aqueous solution, the above-described thixotropy improving effect cannot be obtained.

Accordingly, the present invention provides the following gel oral composition and method for producing the same.
Claim 1:
An aqueous solution of case stratified like sodium silicate, magnesium (a), sodium carboxymethyl cellulose, hydroxyethyl cellulose, sodium alginate, xanthan gum, and an aqueous solution of one or more water-soluble polymer selected from carrageenan (b), (a ) Component and (b) component (b) / (a) an organic-inorganic composite thickener formed by mixing such that the mass ratio is 0.4 to 7 (c) anionic surfactant Is added, the water content in the composition is adjusted to 15 to 50% by mass, and the blending amount of the component (a) is 0.1 to 1.5% by mass of the total composition, (b) A gel-like composition for oral cavity , wherein the compounding amount of the component is 0.5 to 2% by mass of the whole composition, and the compounding amount of the component (c) is 0.2 to 2% by mass of the whole composition. .
Claim 2:
Furthermore, the gel-like composition for oral cavity of Claim 1 with which 12-52 mass% abrasive | polishing agent was mix | blended .
Claim 3:
The concentration of the aqueous solution of the component (a) is 0.1 to 10% by mass, and the concentration of the aqueous solution of the component (b) is 0.3 to 10% by mass . .
Claim 4:
An aqueous solution of synthetic layered sodium silicate / magnesium (a) and an aqueous solution of one or more water-soluble polymer substances (b) selected from sodium carboxymethylcellulose, hydroxyethylcellulose, sodium alginate, xanthan gum and carrageenan (a) After mixing so that ratio (b) / (a) of a component and (b) component may be 0.4-7 as a mass ratio, and preparing an organic inorganic composite thickener, water content is 15-50 mass%. And (c) a method for producing a gel-type oral cavity composition in which an anionic surfactant is added , and the blending amount of the component (a) is 0.1 to 1.5 mass of the whole composition. %, The blending amount of the component (b) is 0.5 to 2% by weight of the whole composition, and the blending amount of the component (c) is 0.2 to 2% by weight of the whole composition. the gel-like mouth Method of manufacturing a formed product.
Claim 5:
Furthermore, the manufacturing method of the composition for gelled oral cavity of Claim 4 which adds 12-52 mass% of abrasive | polishing agents .
Claim 6:
The concentration of the aqueous solution of component (a) is 0.1 to 10% by mass, and the concentration of the aqueous solution of component (b) is 0.3 to 10% by mass. Manufacturing method .

  The gel composition for oral cavity of the present invention is excellent in temporal shape retention and phase-liquid separation stability, and has good retainability that prevents the oral composition from dripping from the mouth when brushed in the oral cavity. The composition for oral cavity that spreads well in the oral cavity has good spreadability in the oral cavity, has little stringiness and good usability, and a sufficient cleaning effect with a short act of applying the preparation in the oral cavity It is possible to play.

It is a graph which shows the hysteresis loop curve of the thickening body (blank) obtained using only the carboxymethylcellulose sodium aqueous solution in an experiment example. It is a graph which shows the hysteresis loop curve of the thickened body of sodium carboxymethylcellulose / synthetic layered sodium silicate and magnesium = 5/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickened body of sodium carboxymethylcellulose / synthetic layered sodium silicate.magnesium = 4/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickening body of sodium carboxymethylcellulose / synthetic layered sodium silicate and magnesium = 3/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickener (blank) obtained using only the hydroxyethylcellulose aqueous solution in an experiment example. It is a graph which shows the hysteresis loop curve of the thickened body of hydroxyethyl cellulose / synthetic layered sodium silicate / magnesium = 5/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickening body of hydroxyethylcellulose / synthetic layered sodium silicate magnesium * 4/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickening body of hydroxyethylcellulose / synthetic layered sodium silicate magnesium * 3/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickening body (blank) obtained using only the sodium alginate aqueous solution in an experiment example. It is a graph which shows the hysteresis loop curve of the thickener of sodium alginate / synthetic layered sodium silicate.magnesium = 5/1 in the experimental example. It is a graph which shows the hysteresis loop curve of the thickener of sodium alginate / synthetic layered sodium silicate.magnesium = 4/1 in the experimental example. It is a graph which shows the hysteresis loop curve of the thickened body of sodium alginate / synthetic layered sodium silicate.magnesium = 3/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickening body (blank) obtained using only the xanthan gum aqueous solution in an experiment example. It is a graph which shows the measurement result by the said viscoelasticity measuring apparatus of the thickened body of xanthan gum / synthetic layered sodium silicate * magnesium = 5/1 in an experiment example. It is a graph which shows the hysteresis loop curve of the thickened body of xanthan gum / synthetic layered sodium silicate * magnesium = 4/1 in an experiment example. It is a graph which shows the hysteresis loop curve of the thickened body of xanthan gum / synthetic layered sodium silicate and magnesium = 3/1 in an experimental example. It is a graph which shows the hysteresis loop curve of the thickening body (blank) obtained using only the carrageenan aqueous solution in an experiment example. It is a graph which shows the hysteresis loop curve of the thickening body of the carrageenan / synthetic | combination layered sodium silicate and magnesium = 5/1 in an experiment example. It is a graph which shows the hysteresis loop curve of the thickening body of the carrageenan / synthetic | combination layered sodium silicate and magnesium = 4/1 in an experiment example. It is a graph which shows the hysteresis loop curve of the thickened body of carrageenan / synthetic layered sodium silicate and magnesium = 3/1 in an experimental example.

Hereinafter, the present invention will be described in more detail.
The present invention relates to a gel-like oral composition, which has a high thixotropic property, that is, a high yielding property, and a low yield value when compared with a normal toothpaste. It has both good retention and good spread.
In general, toothpaste containing a water-soluble polymer substance is a pseudoplastic fluid having a yield value among non-Newtonian fluids, and in a stationary state, a strong binding action due to intermolecular stress and interparticle stress acts and is a liquid. It also exhibits certain solid-like properties. If the external force is less than the stress acting inside the material, the material will only undergo elastic deformation. When the external force becomes greater than the stress acting inside the substance, the bond due to the internal stress is broken, and the molecules and particles in the substance begin to move and move irregularly, changing to the properties of the liquid. That is, the yield value is a value of external stress when a substance having both solid and liquid properties changes from solid to liquid, that is, when external force and internal stress are equal. In such oral compositions such as toothpaste, when the yield value is increased in order to improve the shape retention and the like, it is difficult to spread in the oral cavity and the cleaning effect is not sufficiently exhibited. On the other hand, the gel-like composition of the present invention usually has a higher yield value in order to improve shape retention over time and retention in the oral cavity, that is, results in a loss of good spread in the oral cavity. The thixotropy is enhanced, so that they can be compatible with each other, and have an exceptional effect.

The composition for oral cavity of the present invention is
(A) Synthetic layered sodium silicate / magnesium,
(B) a water-soluble polymer substance selected from sodium carboxymethylcellulose, hydroxyethylcellulose, sodium alginate, xanthan gum, carrageenan,
(C) An anionic surfactant is an essential component.

Here, as the component (a), synthetic layered sodium silicate / magnesium is used, and commercially available products such as Laponite (manufactured by Rockwood) can be used. The synthetic layered sodium silicate / magnesium has an approximate mass% of SiO ₂ : 58.0%, MgO: 25.4%, Na ₂ O: 3.1%, Li ₂ O: 1.0%. Other components are synthetic clay agents containing some water and trace metals. It is a completely synthetic product and is produced by mixing sodium silicate with sodium salt, magnesium salt and lithium salt and reacting them. Natural clay agents such as bentonite and hectorite are similar in crystal structure, but synthetic layered sodium and magnesium silicates have a much smaller primary particle size than those of natural clay agents. It has a feature of having a structure.

  (A) Although the compounding quantity of a component is not restrict | limited in particular, 0.05-2% (% of the whole composition) from the point of the preservability provision effect with time, the ease of mounting to a toothbrush etc., and the point of the spreading | diffusion in an oral cavity ( % By mass, the same shall apply hereinafter). If the content is less than 0.05%, sufficient effect of imparting shape retention with time may not be exhibited. If the content exceeds 2%, phase-liquid separation may occur or the spread in the oral cavity may be impaired. More preferably, it is 0.1 to 1.5% from the viewpoint of shape retention with time, phase separation, and good spread in the oral cavity.

  The water-soluble polymer substance of component (b) is selected from sodium carboxymethyl cellulose, hydroxyethyl cellulose, sodium alginate, xanthan gum, and carrageenan, and these can be used alone or in combination of two or more. . In particular, sodium carboxymethyl cellulose, hydroxyethyl cellulose, and xanthan gum can be suitably used.

  These water-soluble polymer substances may be those usually used in oral compositions, and commercially available products can be used. Examples of sodium carboxymethyl cellulose include CMC Daicel (manufactured by Daicel Chemical Industries, Ltd.), examples of hydroxyethyl cellulose include, for example, HEC Daicel (manufactured by Daicel Chemical Industries, Ltd.), and examples of sodium alginate include, for example, Duck Algin (Kibun Food Chemifa ( Co., Ltd.), xanthan gum, for example, Keldent (CP Kelco), and carrageenan, for example, carrageenan (CP Kelco) can be used.

  The blending amount of the water-soluble polymer substance (b) is preferably 0.2 to 3% of the entire composition, and if it is less than 0.2%, a sufficient effect of suppressing separation of phase liquid may not be exhibited. Exceeding this may impair the ease of placement on the toothbrush. More preferably, it is 0.5 to 2% from the viewpoint of phase liquid separation and ease of placement on a toothbrush.

  In this case, the component (a) and the component (b) have a ratio (mass ratio) of (b) / (a) of 0.2 to 20, more preferably 0.3 to 15, and still more preferably 0.4. From 10 to 10 and particularly preferably from 0.4 to 7, it is preferable from the viewpoints of temporal shape retention, liquid separation, ease of placement on a toothbrush and the like, and oral retention.

(C) As an anionic surfactant of component, higher alkyl sulfate ester salt having 8 to 18 carbon atoms of alkyl group such as sodium lauryl sulfate and sodium myristyl sulfate, polyoxyethylene alkyl sulfate ester salt, α-olefin N-acyl sarcosine salts such as sulfonate, sodium lauroyl sarcosine, and myristoyl sarcosine sodium, N-lauroyl taurine salts, and the like can be used, and one or more of these can be blended. An anionic surfactant is an alkali metal salt of an alkyl sulfate ester or an alkali metal salt of an N-acyl sarcosine acid, especially a lauryl sulfate (sodium salt) or an N-lauroyl sarcosine, particularly from the viewpoint of good spread in the oral cavity. Acid salts (sodium salts) are preferred.
Commercially available products can be used as the anionic surfactant, and specific examples include sodium lauryl sulfate (Toho Chemical Industry Co., Ltd.) and sodium N-lauroyl sarcosine (Kawaken Fine Chemical Co., Ltd.).

  (C) The amount of the anionic surfactant is preferably 0.1 to 3%, more preferably 0.2 to 2% of the whole composition from the viewpoint of oral retention and good spread in the oral cavity. It is. If the content is less than 0.1%, sufficient oral retentive effect is not exhibited, the spread in the oral cavity is poor, and if it exceeds 3%, phase-liquid separation tends to occur, or the oral mucosa is stimulated. May occur.

The oral composition of the present invention can be blended with known components depending on the type.
For example, a dentifrice can be blended with an abrasive, and examples of the abrasive include abrasive anhydrous silicic acid, aluminum hydroxide, calcium carbonate, dibasic calcium phosphate dihydrate, dibasic calcium phosphate anhydrate, etc. Silica anhydride and calcium carbonate are particularly preferred from the viewpoint of good spread in the oral cavity.
Specific examples of the abrasive silicic anhydride include precipitated silica, silica gel, aluminosilicate, zirconosilicate and the like, and precipitated silica is particularly preferable. The precipitated silica is more preferably precipitated silica having a median diameter (d50) of 5 to 50 μm, particularly 10 to 30 μm. If the median diameter is less than 5 μm, sufficient polishing properties cannot be obtained, and if it exceeds 50 μm, a feeling of strangeness may occur during use. The median diameter is a value obtained by measuring a cumulative distribution of 50% on a volume basis using a particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., Microtrac particle size distribution meter, dispersant: water).
A commercially available product can be used as the abrasive, and examples thereof include silicic anhydride (precipitated silica (median diameter 18 μm), Taki Chemical Co., Ltd.), calcium carbonate (Calfine Co., Ltd.), and the like.

  The blending amount of the abrasive is preferably 12 to 52%, particularly preferably 12 to 45%, and more preferably 15 to 40% from the viewpoint of the effect of imparting shape retention with time and the phase liquid separation. If it is less than 12%, sufficient effect of imparting shape retention with time may not be exhibited, or phase-liquid separation may occur, and if it exceeds 52%, the spreadability in the oral cavity may be impaired.

  In the composition for oral cavity of the present invention, if necessary, it is within a range not hindering the effects of the present invention, for example, a thickener, a binder, a surfactant, and optionally a sweetener, preservative, and effective. Ingredients, pigments (colorants), fragrances and the like can be blended.

  As the thickener, glycerin, sorbit, propylene glycol, polyethylene glycol having an average molecular weight of 200 to 6,000, ethylene glycol, sugar alcohols such as reduced starch saccharified products, or one or more of polyhydric alcohols can be used. (Usually, the blending amount is 5 to 50%).

  As the binder, the above components (a) and (b) are used, but in addition, organic binders such as sodium polyacrylate, propylene glycol alginate, carbopol, guar gum, gelatin, and Avicel as desired. You may mix | blend inorganic binders, such as a montmorillonite, a kaolin, a bentonite, etc. in the range which does not inhibit the effect of this invention.

As the surfactant, in addition to the anionic surfactant, an amphoteric surfactant and a nonionic surfactant can be blended if necessary. Examples of amphoteric surfactants include N-acyl glutamate and 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine. Nonionic surfactants include, for example, alkyl glycosides, sucrose fatty acid esters, alkylol amides. , Polyoxyethylene sorbitan monostearate, polyoxyethylene polyoxypropylene glycol, polyoxyethylene alkyl ether, decaglyceryl laurate and the like.
The composition of these surfactants is usually 0 to 3%, particularly 0 to 2%.

  Sweeteners include saccharin sodium, aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, perilartin, etc., and preservatives include parabens (paraoxybenzoate) such as butylparaben and ethylparaben. And sodium benzoate.

  Various active ingredients include, for example, fluorides such as sodium fluoride, potassium fluoride, stannous fluoride, strontium fluoride, sodium monofluorophosphate, condensed phosphate, potassium salt of normal phosphate, sodium salt, etc. Water-soluble phosphate compound, tranexamic acid, epsilon-aminocaproic acid, allantochlorohydroxyaluminum, ascorbic acid or a salt thereof, dl-tocopherol acetate, dihydrocholesterol, α-bisabolol, chlorhexidine salts, azulene, dipotassium glycyrrhizin, sodium chloride, Glycyrrhetinic acid, copper chlorophyllin sodium, chlorophyll, copper compounds such as copper gluconate, aluminum lactate, strontium chloride, potassium nitrate, hydroxamic acid and its derivatives, zeolite, methoxyethylene, Pi dihydro cholesterol, benzethonium chloride, dihydrocholesterol, trichlorocarbanilide, zinc citrate, Japanese angelica root soft extract, Phellodendron bark extract, camomile, clove, rosemary, scutellaria root and a plant extract of safflower 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.

  Perfumes are peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime Oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, iris concrete, absolute peppermint Natural fragrances such as absolute rose and orange flower, and fragrances that have been processed (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder fragrance, etc.), and Menthol, Carvone, Anethole, Cineol, Methyl salicylate , Synamic aldehyde, eugenol, 3-l-menthoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone, menthyl acetate, N-substituted-paramentane-3-carboxamide, pinene, octylaldehyde , Citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, hexanal, propyl alcohol, butanol, isoamyl Alcohol, hexenol, dimethyl sulfide, cycloten, furfural, trimethylpyrazine, ethyl lactate, methyl lactate, ethylthioacete For peroral compositions such as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mix flavor, tropical fruit flavor, etc. The well-known perfume material used can be used.

  The blending amount of the fragrance is not particularly limited, however, the above fragrance material is preferably used in a composition of 0.000001 to 1%. Moreover, it is preferable to use 0.1-2.0% of the fragrance | flavor for perfume using the said fragrance | flavor raw material in a formulation composition.

  Examples of the colorant include Blue No. 1, Yellow No. 4, Green No. 3, and the like.

  In the composition of the present invention, the water content is 15 to 50%, preferably 20 to 45%, more preferably 25 to 45%. It is important for the amount of water to be in the above-mentioned range to effectively express the above-described effect. If the amount of water is too small, the spread in the oral cavity may be impaired, and if the amount of water is too large, the shape retention property, phase-liquid separation stability, and oral retention may be impaired. Outside the amount range, the object of the present invention cannot be achieved.

  The composition for gelled oral cavity of the present invention comprises an aqueous solution of synthetic layered sodium silicate / magnesium (a) and one or more water-soluble polymer substances selected from sodium carboxymethylcellulose, hydroxyethylcellulose, sodium alginate, xanthan gum, and carrageenan. After mixing with the aqueous solution of (b) and preparing an organic-inorganic composite thickened body, it can be manufactured by adjusting the water content to 15 to 50% by mass and adding (c) an anionic surfactant. . In this case, the ratio (b) / (a) of the component (a) to the component (b) is 0.2 to 20, more preferably 0.3 to 15, more preferably 0.4 to 10, It is more preferable to mix so that it may become 0.4-7 especially preferably.

The thickener according to the present invention is produced by separately preparing the aqueous solution of the component (a) and the aqueous solution of the component (b) and mixing them. In this case, the aqueous solution of the component (a) With the aqueous solution of component b), the aqueous solution of component (b) may be added to the aqueous solution of component (a), or the aqueous solution of component (a) may be added to the aqueous solution of component (b).
Furthermore, the anionic surfactant of component (c) is added after preparing the above thickened body, but other compounding components can be added as appropriate, and even if added to the aqueous solution of component (a) (b ) Component may be added to the aqueous solution, or may be added together with component (c). In addition, it is desirable to add an abrasive | polishing agent and a fragrance | flavor after mixing (a) and (b) component.

  In this case, the concentration of the aqueous solution of component (a) is preferably 0.1 to 10%, particularly preferably 0.2 to 6%, and the concentration of the aqueous solution of component (b) is 0.3 to 10%, particularly 0.4. ~ 6% is preferred. Such an aqueous solution of component (a) and an aqueous solution of component (b) are mixed at a mass ratio of 5: 1 to 1: 5, particularly 1: 1, and the ratio of (b) / (a) is in the above range. It is desirable to obtain a thickened body.

In the present invention, by mixing the aqueous solutions of the components (a) and (b) as described above, good thixotropy is given, and the mass ratio of the components (a) and (b) is (b) / (a ) = Thickened body formed using a ratio of 3/1 is a cone plate type rotational viscometer, specifically, a cone plate type viscoelasticity measuring device, Rheo Stress RS50 (manufactured by HAAKE), and sensor C35 / Viscosity measurement using only the water-soluble polymer substance and the area S ₁ surrounded by the hysteresis loop curve when measured at 4 degrees, γ = 0 to 50 (1 / s), 120 s, and 25 ° C. The ratio <thixotropic property> ((S ₁ / S ₀ ) × 100) with the area S ₀ surrounded by the hysteresis loop curve is 130 to 1,000, particularly 150 to 1,000, especially 200 to 800. Increase A viscous body is obtained.

  In addition, when mixing the aqueous solution of (a) component and the aqueous solution of (b) component, the mixing conditions are not specifically limited, Although a normal method can be employ | adopted, Room temperature, specifically about 15-30 degreeC It is preferable to stir for 3 to 20 minutes under the following temperature conditions.

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

  EXAMPLES Hereinafter, although an Example, a comparative example, and an experiment example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples,% is mass% unless otherwise specified.

Examples and comparative examples
Gel-like dentifrice compositions having the compositions shown in Tables 1 and 2 were prepared by the following method and evaluated as follows. The results are shown in Tables 1 and 2.

Preparation of test gel dentifrice composition Prepare 5% aqueous solution of synthetic layered sodium silicate and magnesium silicate, and other components in the composition excluding the anionic surfactant, abrasive and fragrance of component (c) A solution obtained by dissolving the required component in the residual water was mixed with an aqueous solution in which the water-soluble polymer substance (b) was dissolved at room temperature, and stirred for 10 minutes to prepare a thickened body, and then the component (c). A gel dentifrice composition was prepared by kneading an anionic surfactant, an abrasive, and a fragrance, and the innermost layer was a linear low-density polyethylene 26 mm diameter and 8 mm diameter laminated tube (low-density polyethylene 72 μm / Ethylene / acrylic acid copolymer resin 90 μm / Aluminum 10 μm / Ethylene / acrylic acid copolymer resin 35 μm / Linear low density polyethylene 50 μm, thickness 257 μm (Dai Nippon Printing Co., Ltd.) )))) Was filled with 50 g.

The components used for the preparation of the gel dentifrice composition are as follows, and for the other components, standard products of quasi-drug raw material standards were used.
Synthetic layered sodium silicate / magnesium; Laponite D, Rockwood sodium carboxymethylcellulose; CMC Daicel, Daicel Chemical Industries'hydroxyethylcellulose; HEC Daicel, Daicel Chemical Industries, Ltd. sodium alginate; Duck Algin, Kibun Food Chemifa Corporation Xanthan Gum; Keldent, CP Kerco Carrageenan; Carrageenan, CP Kerco Sodium Lauryl Sulfate; Toho Chemical Industries, Ltd. Silicic Anhydride (Abrasive Silica);
Precipitating silica with a median diameter of about 20 μm, manufactured by Taki Chemical Co., Ltd.

  About the obtained gel dentifrice composition, temporal retention, phase separation stability, ease of placement on a toothbrush, oral retention, good spread in the oral cavity, and further remineralization effect The method was evaluated.

(1) Method for evaluating shape retention over time The dentifrice composition was extruded 10 mm onto a toothbrush having a brush head width of 10 mm and a length of 20 mm, and the shape after 3 minutes was visually evaluated according to the following criteria.
Evaluation criteria:
◎: No change in shape and does not hang from toothbrush ○: Some change in shape, but does not hang from toothbrush △: Some change in shape, slightly hangs from toothbrush ×: Change in shape, hangs from toothbrush

(2) Evaluation method of phase-liquid separation stability After storing the composition at 60 ° C. for 1 month, the composition was extruded 5 cm onto the paper, and the width (mm) from which the water soaked into the paper or the paper oozed was visually observed. And evaluated according to the following criteria.
Evaluation criteria:
◎: No phase-liquid separation ○: Little phase-liquid separation (less than 1 mm)
Δ: Slightly phase-liquid separation (1 mm or more and less than 5 mm)
X: There is phase-liquid separation (5 mm or more)

(3) Evaluation method of ease of placement on toothbrush Using about 10 subjects, about 1 g of the composition is placed on a toothbrush having a brush head width of 10 mm and a length of 20 mm, and the ease of placement on the toothbrush is “very easy to place”. , “Easy to place”, “Slightly difficult to place” and “Difficult to place” were obtained. Of these answers, 4 points were “Very easy to place”, 3 points were “Easy to place”, 2 points were “Slightly difficult to place”, and 1 point was “Difficult to place”. The ease of placement on the toothbrush was evaluated.
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 1.0 points More than 2.0 points

(4) Method for evaluating intraoral retainability Using about 10 subjects, about 1 g of the composition was placed on a toothbrush having a brush head width of 10 mm and a length of 20 mm and brushed for 3 minutes. Answers were obtained in four stages: "Cannot hang from the mouth", "Can hardly hang from the mouth", "Slightly hangs from the mouth", "Sags from the mouth". Of these answers, 10 points were given as follows: 4 points “No dripping from the mouth”, 3 points “No dripping from the mouth”, 2 points “Drawing slightly from the mouth”, 1 point “Dropping from the mouth” Intraoral retention was evaluated from the average score according to the following criteria.
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 1.0 points More than 2.0 points

(5) Evaluation method of good spread in the oral cavity Using about 10 subjects, about 1 g of the dentifrice composition was placed on a toothbrush having a brush head width of 10 mm and a length of 20 mm, followed by brushing for 3 minutes. Responses were obtained in four levels: “very good”, “good”, “somewhat bad”, and “bad”. Among these answers, 4 points “very good”, 3 points “good”, 2 points “slightly bad” and 1 point “bad”, the average score of 10 people in the oral cavity according to the following criteria The goodness of the spread was evaluated.
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 1.0 points More than 2.0 points

＊；水分量はソルビット液（７０％）中の水分と精製水との合計を示す（以下、同様。）。

*: The amount of water indicates the total amount of water in the sorbite liquid (70%) and purified water (the same applies hereinafter).

[Experimental example]
10% aqueous solution of the water-soluble polymer substance (b), and (b) / (a) = 5/1, 4/1, 3/1 synthetic layered sodium silicate / magnesium (laponite) (a) aqueous solution. Prepare 2% aqueous solution, 2.5% aqueous solution and 3.3% aqueous solution, respectively, add 50 ml of aqueous solution of laponite (a) to 50 ml of aqueous solution of water-soluble polymer substance (b), and stir for 10 minutes. Then, each thickener was obtained at a mass ratio of (b) / (a) shown in Table 3.
The thickened body was measured using a cone plate viscoelasticity measuring device (RheoStress RS50 (manufactured by HAAKE)) at a sensor C of 35/4 degrees, a shear rate of 0 to 50 (1 / s), a measurement time of 120 seconds, and 25 ° C. did.
The results are shown in Tables 3 and 4. Moreover, the hysteresis loop curve obtained by the measurement by the cone plate type viscoelasticity measuring apparatus of each thickened body is shown in FIGS.
The absolute value (Pa · s) in Table 3 indicates an area surrounded by a hysteresis loop curve obtained by measurement with a cone plate type rotational viscometer. The blank (%) in Table 4 shows the area S ₁ surrounded by the hysteresis loop curve of each thickened body and the area surrounded by the hysteresis loop curve when the viscosity is measured similarly using only the water-soluble polymer substance. is a value indicating a ratio _{((S 1 / S 0 ×} 100)) and S _0.
In the figure, Laponite is abbreviated as LAPONITE, carboxymethylcellulose sodium as CMC, hydroxyethylcellulose as HEC, sodium alginate as AR, xanthan gum as XG, and carrageenan as KG.

なお、ラポナイト単独では、チキソトロピー性はなく絶対値が０になった。

Note that laponite alone had no thixotropic property and the absolute value was zero.

From the above results, an organic / inorganic composite having a high thixotropic property by mixing the aqueous solution of the component (a) and the aqueous solution of the component (b) to form a thickened body composed of the components (a) and (b) and water. A thickened body is obtained. Further, this thickened body is obtained by measuring a thickened body formed using a mass ratio of (b) / (a) = 3/1 with a cone plate type rotational viscometer. the area S ₁ surrounded by the hysteresis loop curve, a ratio (S ₁ / S ₀₎ and the area S ₀ enclosed by the hysteresis loop curve when the viscosity measured in the same manner by using only the water-soluble polymer × 100 was found to be 130-1,000.

Claims (6)

An aqueous solution of case stratified like sodium silicate, magnesium (a), sodium carboxymethyl cellulose, hydroxyethyl cellulose, sodium alginate, xanthan gum, and an aqueous solution of one or more water-soluble polymer selected from carrageenan (b), (a ) Component and (b) component (b) / (a) an organic-inorganic composite thickener formed by mixing such that the mass ratio is 0.4 to 7 (c) anionic surfactant Is added, the water content in the composition is adjusted to 15 to 50% by mass, and the blending amount of the component (a) is 0.1 to 1.5% by mass of the total composition, (b) A gel-like composition for oral cavity , wherein the compounding amount of the component is 0.5 to 2% by mass of the whole composition, and the compounding amount of the component (c) is 0.2 to 2% by mass of the whole composition. . Furthermore, the gel-like composition for oral cavity of Claim 1 with which 12-52 mass% abrasive | polishing agent was mix | blended . The concentration of the aqueous solution of the component (a) is 0.1 to 10% by mass, and the concentration of the aqueous solution of the component (b) is 0.3 to 10% by mass . . An aqueous solution of synthetic layered sodium silicate / magnesium (a) and an aqueous solution of one or more water-soluble polymer substances (b) selected from sodium carboxymethylcellulose, hydroxyethylcellulose, sodium alginate, xanthan gum and carrageenan (a) After mixing so that ratio (b) / (a) of a component and (b) component may be 0.4-7 as a mass ratio, and preparing an organic inorganic composite thickener, water content is 15-50 mass%. And (c) a method for producing a gel-type oral cavity composition in which an anionic surfactant is added , and the blending amount of the component (a) is 0.1 to 1.5 mass of the whole composition. %, The blending amount of the component (b) is 0.5 to 2% by weight of the whole composition, and the blending amount of the component (c) is 0.2 to 2% by weight of the whole composition. the gel-like mouth Method of manufacturing a formed product. Furthermore, the manufacturing method of the composition for gelled oral cavity of Claim 4 which adds 12-52 mass% of abrasive | polishing agents . The concentration of the aqueous solution of component (a) is 0.1 to 10% by mass, and the concentration of the aqueous solution of component (b) is 0.3 to 10% by mass. Manufacturing method .

Images