JPH0796490B2 - Toothpaste composition - Google Patents

Description

FIELD OF THE INVENTION The present invention relates to dentifrice compositions that inhibit tartar formation.

BACKGROUND OF THE INVENTION Tartar is a dental deposit that is a major cause of gingivitis, periodontitis, etc., and suppressing or eliminating the formation thereof is necessary for prevention and treatment of periodontal disease. However, while the tartar is soft, it can be removed by brushing, but once it is deposited on the tooth, it is difficult to completely remove it. It is believed that such deposition occurs because the amorphous or microcrystalline calcium phosphate present in dental plaque gradually changes into dense hydroxyapatite crystals. Therefore, if the formation of dense hydroxyapatite crystals is suppressed, the formation of tartar can be effectively suppressed.

It has been conventionally known that the combined use of a polyphosphate salt and a polyvalent metal salt effectively suppresses the change from calcium phosphate to hydroxyapatite (Japanese Patent Laid-Open No. Sho 61-206).
52-108029). However, in a dentifrice composition containing a polyvalent metal salt and a polyphosphate together, the polyphosphate in the composition is significantly hydrolyzed (Japanese Patent Application Laid-Open No. 61-36211).
No.), there is a problem that the dentifrice composition loses the effect of inhibiting tartar formation over time. Then, in order to stabilize the polyphosphate, a polyphosphate root, one or more kinds of polyvalent metal roots selected from magnesium, barium and strontium, and a carboxylic acid composition characterized by containing a carboxylic acid root Have been proposed (JP-A-61-36211).
issue). However, when polyphosphate is mixed in a high concentration to suppress tartar formation, the salting-out effect or the like affects the viscous agent and the foaming agent in the dentifrice composition, and the shape retention and foaming properties of the dentifrice composition. However, there is a problem in that the product quality deteriorates, the usability deteriorates, and the commercial value deteriorates.

The present inventors have solved these problems, by suppressing the formation of hydroxyapatite, as a result of various studies to obtain a dentifrice composition that is stable for a long period of time and prevents tartar formation and has a good feeling of use, It was found that the stability of the polyphosphate in the dentifrice composition is remarkably increased by using the polyphosphate in combination with magnesium aluminometasilicate, and the change over time in the tartar formation inhibitory effect of the polyphosphate is extremely small. A mixture containing the above polyphosphate and magnesium aluminometasilicate as an essential component does not disintegrate due to the shear share during the production of a dentifrice composition by spray drying, etc., and easily becomes particles of a strength that disintegrates during brushing with a toothbrush. It is possible to mold into a toothpaste composition by formulating a high concentration of polyphosphate in such particles and blending it into the toothpaste composition. The shape retention and foaming properties of the product do not deteriorate and the feeling of use is not impaired, and the particles disintegrate due to brushing during tooth brushing and the polyphosphate is dispersed in the mouth to exert the effect of inhibiting tartar formation. The present invention has been completed and the present invention has been completed.

DISCLOSURE OF THE INVENTION The present invention provides a dentifrice composition characterized by containing particles containing magnesium aluminometasilicate and polyphosphate as essential components. According to the dentifrice composition of the present invention, the polyphosphate can be blended stably and in a high concentration, so that the formation of tartar can be effectively suppressed, and the presence of the polyphosphate in a high concentration allows the dentifrice to be brushed. The shape retention and foamability of the composition do not deteriorate.

Next, the results of testing the change over time in the tartar formation inhibitory effect of the dentifrice composition containing particles of magnesium aluminometasilicate and polyphosphate and the shape retention and foaming properties are shown.

The particles and the dentifrice base used were manufactured according to the following manufacturing method according to the formulation shown below.

Preparation of particles All the numerical values in the table mean% by weight.

Purified water was added to each of magnesium aluminometasilicate and the polyphosphate of Table 1 in a separate container to form a slurry. Then, the above-mentioned two kinds of slurries were uniformly mixed, and this was spray-dried by a spray-drying apparatus having an inlet temperature of 250 ° C. to prepare particles.

Preparation of dentifrice base Ingredients% by weight Silica 20.0 Sorbit (70% aqueous solution) 60.0 Sodium carboxymethylcellulose 1.4 Sodium lauryl sulfate 1.4 Sodium saccharin 0.2 Fragrance 0.9 Prepared in 100 purified water Separately powder and liquid ingredients in the above formulation Mix evenly in a container. Then, the liquid component was added to the powder component and uniformly mixed, and defoamed to obtain a dentifrice base.

Changes over time in tartar formation inhibitory effect (1) Preparation of test toothpaste 95 g of the above-mentioned toothbrush base was uniformly blended with the components shown in Table 2 below, and then filled in a laminate tube to prepare a test toothpaste.

The numbers in the table mean grams.

(2) Preparation of test solution Immediately after the preparation and after the preparation, the temperature should be 40 ° C and the humidity should be 75%.
10 g of each test toothpaste shown in Table 2 left for a month was placed in a beaker, and the toothpaste was ground with a glass rod. Then water
30 ml was added, and the mixture was stirred with a magnetic stirrer for 30 minutes and then centrifuged at 17,000 rpm for 10 minutes, and the obtained supernatant was used as a test solution.

(3) Measurement of Tartar Formation Inhibitory Effect The tartar formation inhibitory effect of the test toothpaste was examined by measuring the production time of hydroxyapatite in each of the above test solutions by the pH stat method. Specifically, each test solution 1m
1 and 0.1 M aqueous sodium dihydrogen phosphate solution (1 ml) in a reaction flask with continuous stirring under a nitrogen atmosphere.
added to ml. Then, 1 ml of 0.1 M potassium chloride aqueous solution was added, and the pH was adjusted to 7.4 ± 0.05 with sodium hydroxide.
During this period, sodium dihydrogen phosphate and calcium chloride react with each other to produce dicalcium phosphate, and OH ⁻ ions are consumed during the conversion to hydroxyapatite, which lowers the pH. The pH was maintained at 7.4. The amount of 0.1N sodium hydroxide aqueous solution consumed at this time was changed to Toa Denpa's pH Stat HSS.
It was automatically recorded with a -10A type and the time for producing hydroxyapatite was measured. The results are shown in Table 3.

The pH stat method is widely used as a method for screening an active ingredient that suppresses tartar formation, and the ability to suppress hydroxyapatite crystal growth in vitro and the ability to suppress calcification in vivo of the ingredient. It has been found that there is a good correlation between them.

In the case of the control test, the hydroxyapatite formation reaction proceeded in two stages. First, the base was rapidly consumed when a precipitate of amorphous calcium phosphate was formed (after 1 to 4 minutes),
Subsequent rapid consumption of base was observed as the amorphous calcium phosphate transformed into hydroxyapatite crystals for 15-20 minutes after which base consumption decreased.

Therefore, the delay or disappearance of the second rapid consumption of the base means that the production of hydroxyapatite crystals was suppressed.

As is clear from Table 3, in the case of the test dentifrices 2 and 4 in which only sodium pyrophosphate or sodium tripolyphosphate was mixed in the dentifrice base, a good calculus formation inhibiting effect was shown immediately after the preparation, but the temperature was 40 ° C and the humidity was 75%. After being left for 3 months under the condition of 1, the effect was remarkably reduced. On the other hand, in the case of test toothpaste 1 and 3 in which sodium pyrophosphate or sodium tripolyphosphate was used in combination with magnesium aluminometasilicate and blended into the toothpaste base, it was highly effective in inhibiting tartar formation immediately after preparation and after leaving for 3 months. showed that.

Shape retention The test toothpaste prepared in the same manner as above according to the formulation of Table 4 was left for 3 months under the conditions of a temperature of 40 ° C and a humidity of 75%, and the external shape of the toothpaste paste when extruded from the tube was as follows. It was evaluated by visual observation according to the evaluation criteria of 1.

Evaluation Criteria: The upper portion of the extruded paste retains the circular shape of the tube mouth with almost no loss of shape, while the lower portion is flat and is in a preferable state for use on a toothbrush for stable use.

△: The upper part of the extruded paste is slightly out of shape, but it is not such that the usability is impaired.

×: The extruded paste was soft and could not maintain the circular shape of the tube mouth and lost its shape.

The results are shown in Table 4. Foamability According to the formulation of Table 4, the temperature after production was 40 ° C in the same manner as above,
Using a test toothpaste left for 3 months under the condition of a humidity of 75%, 5 professional panelists brushed the tooth as usual, and the amount of foaming was sensory evaluated according to the following evaluation criteria.

Evaluation Criteria ○: There is sufficient foaming.

B: Foaming is normal.

X: Little foaming.

The results are shown in Table 4.

The numbers in the table mean grams.

As is clear from Table 4, when sodium pyrophosphate is blended in a dentifrice base at a high concentration, the use of sodium pyrophosphate in the form of particles does not deteriorate the shape retention and foaming property, and it seems that the feeling of use deteriorates. There is no such thing.

Thus, the magnesium aluminometasilicate used in the particles incorporated into the dentifrice composition of the present invention is Al ₂ O ₃ .MgO
・ 2SiO ₂・ XH ₂ O is a white inorganic powder represented by the chemical formula, which is commercially available and is based on the total amount of particles from the viewpoint of the particle strength required to exert the effect of the dentifrice composition of the present invention. 20% by weight or more. The polyphosphate used for the particles is not particularly limited, but preferably chain polyphosphate, for example, sodium pyrophosphate, potassium pyrophosphate, disodium dihydrogen pyrophosphate, potassium tripolyphosphate, sodium tetrapolyphosphate, pentapolyline. Sodium acid salts and the like are particularly preferable, and sodium pyrophosphate, potassium pyrophosphate and sodium dihydrogen pyrophosphate can be mentioned, and one kind or two or more kinds thereof can be used in combination. The blending amount of the polyphosphate salt is not particularly limited, but 0.01 to 10% by weight, preferably 0.1 to 5% by weight, based on the total amount of the dentifrice composition, and 0.05 to 80% by weight, preferably, the total amount of particles, 0.5 to 60% by weight. If the blending amount is less than 0.01 wt% with respect to the total amount of the composition and less than 0.05 wt% with respect to the total amount of particles, the tartar formation inhibitory effect is not exhibited, while on the other hand, 10 wt% with respect to the total amount of the toothpaste composition
If it is more than 80% by weight based on the total amount of particles, the physical properties of the dentifrice composition are adversely affected.

Further, to the particles, if necessary, an inorganic powder, a water-soluble polymer, a water-insoluble pigment or the like usually used in a dentifrice composition can be added within a range that does not impair the effects of the present invention.

As a method for producing particles using the above components, inorganic powder, water-soluble polymer, polyphosphoric acid prepared in a separate container in a slurry solution of magnesium aluminometasilicate mixed with a water-insoluble pigment and the like as desired. A salt slurry solution is added and mixed, treated with an emulsifier, and then spray-dried by a conventional method. The temperature required for spray drying may be a temperature at which the stability of the components is not impaired, but is preferably about 250 ° C., and the desired particle size can be obtained by appropriately adjusting the spray speed, the shape of the spray nozzle, and the like. It can be a particle of a diameter. The particles can be produced by a dry granulation method, a tumbling granulation method or the like other than the above powder drying method, but the spray drying method is most preferable because of the convenience of the manufacturing process and the like.

The particles thus obtained do not disintegrate with the stirring shear during the production of a dentifrice composition containing the particles, but completely disintegrate during brushing using the composition so that the polyphosphate is uniformly dispersed in the mouth. Has strong strength. The particle size of the particles is not particularly limited, but usually from 0.05 to 1 m from the viewpoint of usability.
It has an average particle size of m, preferably 0.1-0.5 mm.

The components used as the base of the dentifrice composition of the present invention differ depending on the type and purpose of the composition, but the following components are usually used.

For example, as abrasives, dibasic calcium phosphate dihydrate and anhydride, monobasic calcium phosphate, tribasic calcium phosphate, calcium carbonate, calcium pyrophosphate, titanium oxide, alumina, hydrated alumina, silica gel, colloidal silica, anhydrous alkali Silica-based abrasives such as metal silicate complex salts, aluminum silicate, water-soluble sodium metaphosphate, insoluble potassium metaphosphate, magnesium triphosphate, magnesium carbonate, calcium sulfate, polymethylmethacrylate, bentonite, zirconium silicate, Synthetic resins and the like are mentioned, and one kind or two or more kinds thereof is usually added in an amount of 5 to 60% by weight based on the total amount of the dentifrice composition.

As the binder, carrageenan, sodium carboxymethyl cellulose, methyl cellulose, hydroxyethyl cellulose, cellulose derivatives such as sodium carboxymethyl hydroxyethyl cellulose, alkali metal alginates such as sodium alginate, propylene glycol alginate ester, xanthan gum, tragacanth gum, karaya gum, gum arabic, etc. Examples include gums, polyvinyl alcohol, sodium polyacrylate, carboxyvinyl polymers, binding binders such as polyvinylpyrrolidone, and inorganic binders such as silica gel, aluminum silica gel, bee gum, and laponite, and one or more of them may be used. Is usually added in an amount of 0.5 to 5% by weight based on the total amount of the dentifrice composition.

Examples of the thickening agent include sorbit, glycerin, ethylene glycol, propylene glycol, 1,3-butylene glycol, polyethylene glycol, polypropylene glycol, xylit, maltite, lactit and the like, and one or more of them may be used as a dentifrice composition. Usually, 10 to 70% by weight is blended with respect to the total amount.

Examples of the surfactant include water-soluble salts of higher alkyl sulfates having an alkyl group with 8 to 18 carbon atoms such as sodium lauryl sulfate and sodium myristyl sulfate, and water-soluble higher salts such as hydrogenated coconut oil fatty acid monoglyceride sodium monosulfate. Fatty acid monoglyceride monosulfate, alkylaryl sulfonate such as sodium dodecylbenzene sulfonate, higher alkyl sulfonate, higher fatty acid ester of 1,2-dihydroxypropane sulfonate, N-lauroyl, N-myristoyl or N-palmitoyl An anionic activator such as a substantially saturated higher aliphatic acylamide of a lower aliphatic aminocarboxylic acid compound such as sodium, potassium or ethanolamine salt of sarcosine,
The number of carbon atoms in fatty acid groups such as sucrose mono and dilaurate
12-18 sucrose fatty acid ester, lactose fatty acid ester, lactitol fatty acid ester, maltitol fatty acid ester, stearic acid monoglyceride, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monostearate, polyoxyethylene (10,20 , 40,60,80,100 mol) Hydrogenated castor oil, polymer of ethylene oxide and propylene oxide, and condensation of polyethylene oxide such as polyoxyethylene polyoxypropylene monolauryl ester with fatty acid, fatty alcohol, polyhydric alcohol and polypropylene oxide And nonionic activators such as betaine-type and amino acid-type amphoteric activators, and one or two of them.
0 to 5% by weight, based on the total amount of the dentifrice composition
Compound.

As the active ingredient, allantoins, epsilon aminocaproic acid, tranexamic acid, dextranase, amylase, protease, mutanase, lysozyme, lytic enzymes, enzymes such as liter enzyme, sodium monofluorophosphate, alkali monofluorophosphate, etc. Metal monofluorophosphate, sodium fluoride,
Ammonium fluoride, fluorides such as stannous fluoride, dihydrocholesterol, glycyrrhetin salts, glycyrrhetinic acid, glycerophosphate, chlorophyll, caropeptide, water-soluble inorganic phosphate compounds, vitamins, other anticalculus agents, etc., One kind or two or more kinds can be blended.

Further, sweeteners such as sodium saccharin, stevioside, neohesperidyl dihydrochalcone, glycyrrhizin, perillartine, thaumatin, asparatyl phenylalanine methyl ester, p-methoxycinnamic aldehyde, sucrose, lactose, fructose and sodium cyclamate are added to the total amount of the dentifrice composition. 0 to 1% by weight, preferably 0.01 to 0.5% by weight, and if necessary, p-hydroxymethylbenzoic acid, p-hydroxyethylbenzoic acid, p-hydroxypropylbenzoic acid, p-
Preservatives such as hydroxybutylbenzoic acid, sodium benzoate, lower fatty acid monoglyceride, fragrances such as wintergreen oil, spearmint oil, peppermint oil, sassafras oil, clove oil, eucalyptus oil, gelatin, peptone, arginine hydrochloride, albumin, casein , Whitening agents such as titanium dioxide, silicones, pigments, and other components may be added.

The dentifrice composition of the present invention contains the above-mentioned particles in a conventional dentifrice base, for example, in the case of toothpaste, an abrasive, a binder, a thickener,
It is manufactured by an ordinary method by uniformly blending it with a mixture of a surfactant, a medicinal agent, a flavoring agent, a flavoring agent and the like. The blending amount of the particles is
0.1 to 20% by weight of the total amount of the dentifrice composition, preferably,
1 to 10% by weight. If the amount is less than 0.1% by weight, the effect of inhibiting tartar formation is not sufficiently exerted, while if it is more than 20% by weight, the physical properties of the dentifrice composition are impaired.

EXAMPLES Next, the present invention will be described in more detail with reference to Examples.

Example 1 Component wt% Precipitable silica (ZEODENT113 ) 20. Sodium carboxymethylcellulose 1.4 Titanium oxide 0.5 Sorbit (70% aqueous solution) 60.0 Sodium lauryl sulfate 1.5 Sodium saccharin 0.2 Purified water Remainder From the above ingredients, apply to a toothpaste base prepared according to a conventional method.
20% sodium lophosphate and alumina metasilicate
Particles produced by a conventional method from 80% by weight of magnesium acid salt
Blended uniformly with 5.0% by weight to the total amount of toothpaste composition
Toothpaste manufactured.

Example 2 Particles prepared according to a conventional method from 20% by weight of sodium pyrophosphate, 50% by weight of magnesium aluminometasilicate and 30% by weight of magnesium carbonate based on the dentifrice base of Example 1 were used in an amount of 5.0% by weight based on the total amount of the dentifrice composition. A toothpaste was manufactured by uniformly blending.

Example 3 To the dentifrice base of Example 1 above, 20% by weight of sodium pyrophosphate, 75% by weight of magnesium aluminometasilicate and 5% by weight of Ultramarine Blue were used, and 5.0% by weight based on the total amount of the dentifrice composition of particles prepared by a conventional method. % To prepare a toothpaste.

Example 4 To the dentifrice base of Example 1 above, 60% by weight of sodium pyrophosphate, 39% by weight of magnesium aluminometasilicate and 1% by weight of hydroxyethyl cellulose were used to prepare particles prepared by a conventional method in an amount of 5.0% by weight based on the total amount of the dentifrice composition. A toothpaste was manufactured by uniformly blending.

Example 5 Sodium tripolyphosphate was added to the toothpaste base of Example 1 above.
Toothpaste was prepared by uniformly blending 50% by weight and 50% by weight of magnesium aluminometasilicate according to a conventional method with 5.0% by weight of the particles prepared by a conventional method.

Example 6 Sodium tripolyphosphate was added to the toothpaste base of Example 1 above.
20% by weight, magnesium aluminometasilicate 75% by weight
A toothpaste was prepared by uniformly blending 5% by weight of titanium mica and 5.0% by weight of the particles prepared by a conventional method with respect to the total amount of the toothpaste composition.

Example 7 To the dentifrice base of Example 1, particles prepared by a conventional method from 20% by weight of sodium tetrapolyphosphate, 20% by weight of potassium pyrophosphate and 60% by weight of magnesium aluminometasilicate were used in an amount of 5.0% based on the total amount of the dentifrice composition. A toothpaste was prepared by uniformly blending it in a weight percentage.

Claims (2)

[Claims] 1. A dentifrice composition comprising particles of magnesium aluminometasilicate and polyphosphate as essential components. 2. The dentifrice composition according to item (1), wherein the polyphosphate is a chain polyphosphate.