WO2005000260A1

WO2005000260A1 - Dentifrice composition

Info

Publication number: WO2005000260A1
Application number: PCT/JP2004/009377
Authority: WO
Inventors: Kouichi Sugawara; Hiroyuki Shimizu
Original assignee: Lion Corporation
Priority date: 2003-06-27
Filing date: 2004-06-25
Publication date: 2005-01-06
Also published as: KR20060023547A; JPWO2005000260A1; JP4482767B2; CN1812760A; CN100393297C; KR101181379B1

Abstract

A dentifrice composition, characterized in that it comprises a zeolite, aluminum oxide and silicic acid anhydride, in the form of granules having an average particle diameter of 150 to 800 μm and an average decay strength of 15 to 100 g/piece.

Description

Specification

Technical field of dentifrice composition

TECHNICAL FIELD The present invention relates to a dentifrice composition containing zeolite, which has an appropriate abrasiveness that does not damage teeth and has an excellent calculus formation inhibiting effect. Background art

Conventionally, zeolite has been known to have an effect of preventing tartar formation and bad breath, and oral compositions containing the same have been proposed (Japanese Patent Application Laid-Open No. Hei 11-38017, 6 3—1 4 6 8 0 9 Publication). Also, due to the nature of zeolite, it is known that a smaller particle size adsorbs the causes of tartar and bad breath better and is more effective. However, zeolite has higher powder abrasive properties as its particle size is smaller due to its powder properties, and its abrasive properties against teeth are higher than inorganic powders generally used as toothpaste abrasives. It is easily damaged and cannot be blended in large amounts.

In other words, zeolite is effective in preventing tartar formation and bad breath when incorporated into a dentifrice composition.The greater the amount of zeolite, the higher the effect, but the higher the abrasiveness, the higher the abrasiveness and may damage teeth. For this reason, the compounding amount is currently limited, and for this reason, there has been a demand for the development of a technique that exerts its effectiveness while controlling its abrasiveness. Heretofore, a dentifrice has been proposed in which an inorganic abrasive is granulated and granules having a controlled particle size and disintegration strength are blended (Japanese Patent Publication No. 6-21053, Japanese Patent Application Laid-open No. Japanese Patent Application Laid-Open No. 2-2266347, Japanese Patent Application Laid-Open No. 10-36632). However, each of these aims only to efficiently remove dirt such as plaque by controlling the abrasiveness of the inorganic abrasive, and causes calcium and bad breath that cause tartar. No consideration was given to the effect of adsorbing and removing sulfur compounds and the like. Disclosure of the invention

An object of the present invention is to provide a dentifrice composition that has appropriate tooth polishing properties that do not damage teeth, and that exerts zeolite-derived efficacy satisfactorily and has an excellent tartar formation preventing effect. I do.

The present inventors have conducted studies to achieve the above object.As a result, zeolite was made to contain silica anhydride as a binder, the average particle size was 150 to 800 ^ m, and the average disintegration strength was 15 to 15. By increasing the particle size to 100 gZ, the increase in abrasiveness due to zeolite is suppressed, and surprisingly, when aluminum oxide is mixed and granulated into the granules, the abrasiveness due to zeolite blending is increased. Was found to be further suppressed, to have an appropriate polishing property, and to exhibit sufficient zeolite-derived efficacy (tartar prevention effect). This makes it possible to incorporate a large amount of zeolite into the dentifrice composition. By blending the above granules in the dentifrice composition as an active ingredient for preventing calculus formation, it has an appropriate tooth polishing property that does not damage the teeth, It has been found that the dentifrice composition having an excellent calculus formation inhibiting effect can be obtained by sufficiently exhibiting the effectiveness of the calculus formation inhibiting effect derived therefrom.

Therefore, the present invention

[1] Granules containing zeolite, aluminum oxide, and silicic anhydride, with an average particle size of 150 to 800 ^ m and an average disintegration strength of 15 to 100 g / piece A dentifrice composition characterized by this,

[2] The content of zeolite in the granules is 50 to 99% by mass, the content of aluminum oxide is 0.5 to 25% by mass, and the content of gay anhydride is 0.5 to 25% by mass. The dentifrice composition according to claim 1, wherein

[3] The dentifrice composition according to claim 1 or 2, wherein the blending amount of the granules is 1 to 50% by mass of the whole composition.

I will provide a. Brief Description of Drawings

FIG. 1 is a schematic diagram of a pH change amount measuring device used for evaluating calcium capturing ability in an example of the present invention. BEST MODE FOR CARRYING OUT THE INVENTION

The dentifrice composition of the present invention is characterized by containing zeolite, aluminum oxide, and silicic anhydride, and containing granules having a specific average particle size and average disintegration strength (hereinafter, referred to as zeolite granules).

Here, zeolite used in the present invention _{_{_{compositions, W m Z n 0 2 n}}} 's H 2 0 (W is N a, C a, K, with B a or S r, Z is S i + A 1 (S i: A 1> 1 s is not fixed), and there are both natural and synthetic aluminosilicates, about 40 of which are natural and those which are synthetic. In the present invention, any of these zeolites can be used In the present invention, natural zeolites and synthetic zeolites are exemplified as useful zeolites as natural zeolites. , Clinopti-mouth lite, mordenite, anal sim, shabasite, erionite, romontite, philipsite, ferrierite, ilakite, etc. The synthetic zeolites are A (3A, 4A, 5A, etc.) type zeolites. , L There are zeolites, faujasites (X-type zeolites, Y-type zeolites), offaleites, erionites, mordenites, etc. However, natural zeolites contain contaminants and lack homogeneity, so synthetic zeolites are preferred. Among the synthetic zeolites, A (3A, 4A, 5A) type zeolites, X type zeolites, Y type zeolites, and L type zeolites are preferable, and the effect when blended in an oral composition is preferable. A-type zeolite is more preferable in view of the above point.Among the A-type zeolites, 4A-type zeolite is superior to other A-type zeolites in calcium-capturing power and is particularly preferable in terms of tartar-preventing effect. A-type zeolites are commercially available, for example, Sasil (Degussa), Toyobuilder, Zeolam (Tohoku Soichi Co., Ltd.), Shilton (Mizusawa Chemical Industries) Co., Ltd.), and the like.

The average particle size of zeolite used as a raw material for zeolite granules is not particularly limited, but is preferably from 1 to 100 m.If the particle size is smaller than 1, the granule strength may be low, and appropriate abrasiveness may not be maintained. In addition, if it is larger than 100 m, the effectiveness of zeolite in zeolite granules may be reduced. The average particle size was measured using a Microtrac particle size analyzer (manufactured by Nikkiso Co., Ltd.). It is a fixed value (the same applies hereinafter).

The content of this zeolite in zeolite granules is preferably from 50 to 99% (mass%, the same applies hereinafter), particularly preferably from 70 to 90%.

Aluminum oxide is produced by the Pier method and has a sintering temperature of 1,000 to 1,200. By controlling to about C, it is preferable that the degree of pregelatinization is 50 to 70% .If the degree of pregelatinization is high, the polishing power may not be able to be maintained properly and the polishing power may be too high. On the other hand, if it is too low, the effectiveness of the zeolite granules may be reduced. The average particle size (average particle size according to the same measuring method as for the above zeolite) is preferably from 0.1 to 106 m, more preferably from 0.5 to 3 m. If the particle size is larger than 10 ^ m, the polishing power may be too high, and if it is smaller than 0.1 m, the zeolite effectiveness of the zeolite granules may be reduced.

The content of aluminum oxide is preferably 0.5 to 25%, particularly preferably 1 to 20% of the whole raw material used for zeolite granulation, and if it exceeds 25%, the amount of zeolite becomes relatively small, Zeolite may be less effective. Also,

If it is less than 0.5%, the expression of zeolite effectiveness may decrease.

In addition, there are two types of industrial methods for producing silicic anhydride, a dry method and a wet method. In the present invention, it is particularly preferable to use precipitated silica by a wet method. The average particle size (average particle size according to the same measuring method as for the above zeolite) is preferably 0.1 to 50 °, more preferably 1 to 20 m. If the dry acid method is used, or if the particle size is larger than 50 m or smaller than 0.1 m, the disintegration strength of the granules may be weak and the abrasiveness may be too large. .

The content of the silicic acid anhydride in the zeolite granules is preferably 0.5 to 25%, and particularly preferably 1 to 20% .If the content is less than 0.5%, the disintegration strength of the granules will be low, and the abrasiveness will be low. May be too large, and if it exceeds 25%, the amount of zeolite is relatively small, and the effectiveness of zeolite may be reduced.

Further, in the present invention, in addition to the aluminum oxide and the caustic anhydride as the zeolite granule raw material, various insoluble materials may be used as long as the performance of the zeolite granules is not hindered. It is possible to add optional components such as Specifically, dibasic calcium phosphate (dihydrate or anhydride), dibasic calcium phosphate, tribasic calcium phosphate, calcium pyrophosphate, calcium carbonate, aluminum hydroxide, magnesium carbonate, tribasic magnesium phosphate, insoluble sodium metaphosphate And insoluble potassium metaphosphate, titanium oxide, zirconium silicate and the like. The amount of the insoluble material is preferably 20% or less.

Further, in addition to the insoluble material, a medicinal ingredient, a coloring agent, a fragrance ingredient, and other excipients generally used for dentifrices can be blended. Among them, the coloring agent is preferably a water-insoluble one such as titanium oxide, gunjiyou, konjiyo, bengalara, mica titanium, and lake dye.

The zeolite granules according to the present invention can be obtained by adding aluminum oxide and citric anhydride, and if necessary, the above-mentioned optional components to the above-mentioned zeolite, and granulating the zeolite so as to have a specific average particle size and average disintegration strength. Obtainable.

In this case, the average particle size of the zeolite granules is determined by sieving with a JIS sieve and calculating the 50% particle size from the particle size distribution, where the average particle size is 150 to 800 m, preferably 2%. It is in the range of 0 to 500 jm. If the average particle size is smaller than 150 m, the polishing ability cannot be controlled and the polishing power becomes too large. If the average particle size exceeds 800 m, the feeling of use of the compounded toothpaste is impaired.

In addition, the average disintegration strength of zeolite granules was determined by measuring the automatic breaking strength of 30 granules with a rheometer (Sun Rheometer CR-200D) manufactured by Sun Science Co., Ltd. The measured value of the load when the zeolite granules collapse when compressed at a pressure in the range of 15 to 100 gZ, preferably 20 to 50 g / piece, as the average value of Use If the average disintegration strength is less than 15, the abrasiveness cannot be controlled, and the abrasive power becomes too large. If the average disintegration strength exceeds 100 g, the feeling of use of the toothpaste deteriorates.

Examples of a method for forming zeolite granules include a compression molding method, an extrusion molding method, and a spray drying method. A sintering method is preferable because granules having the above strength range can be easily obtained.

In the dentifrice composition of the present invention, one or more zeolite granules are arranged. The compounding amount is preferably 1 to 50%, particularly preferably 2 to 30% of the whole composition. If the amount is less than 1%, the effectiveness of the zeolite granule may not be sufficiently exhibited, and if it exceeds 50%, the feeling of use of the toothpaste may be deteriorated. The dentifrice composition of the present invention can be prepared into various types of dentifrices such as toothpaste, moist dentifrice, and liquid dentifrice in which the above zeolite granules are dispersed, and preferably a dentifrice having thixotropic properties to a liquid dentifrice. . In that case, various optional components other than the above-mentioned zeolite granules usually used for a dentifrice composition can be blended. Other ingredients that can be included include abrasives, thickeners (humectants), binders, surfactants, sweeteners, flavors, preservatives, and the like. Since the required components and the amounts of these other components differ depending on the dosage form, the selection of the components and the amounts of the components are carried out in the same manner as in the previous case, and within the range that does not impair the effects of the present invention. It is necessary.

As abrasives, dibasic calcium phosphate (dihydrate or anhydrous), dibasic calcium phosphate, tribasic calcium phosphate, calcium pyrophosphate, calcium carbonate, aluminum hydroxide, alumina, magnesium carbonate, magnesium phosphate tribasic Water, insoluble sodium metaphosphate, insoluble potassium metaphosphate, titanium oxide, anhydrous caic acid, hydrated caic acid, titanium gayate, zirconium silicate, and synthetic resin-based abrasives. In the case of toothpaste, which is a typical dosage form, the amount of the abrasive is preferably 5 to 80%, more preferably 10 to 50% of the whole composition.

As cleaning aids, polyphosphates such as pyrophosphate and tripolyphosphate, alkaline agents such as sodium bicarbonate and sodium carbonate, organic acids such as citric acid, malic acid, tartaric acid, ascorbic acid, lactic acid, and acetic acid; The salts can also be incorporated in effective amounts.

Binders include carrageenan, sodium carboxymethylcellulose, methylcellulose, ethylcellulose, cellulose acetate, sodium hydroxyethylcellulose, sodium alginate, xanthan gum, tragacanth gum, karaja gum, arabia gum, locust bean gum, polyvinyl alcohol, Examples thereof include sodium polyacrylate, lipoxyvinyl polymer, polyvinylpyrrolidone, carbopol, silica gel, aluminum silica gel, thickening silica, veegum, laponite and the like (the blending amount is usually 0.1 to 5.0%). Examples of the thickener include glycerin, sorbitol, ethylene glycol, propylene glycol, polyethylene glycol, polypropylene glycol, xylitol, maltitol, lactol, and the like (the compounding amount is usually 1 to 80%).

Surfactants can include anionic surfactants, cationic surfactants, nonionic surfactants, and zwitterionic surfactants. Examples of anionic surfactants include sodium lauryl sulfate, sodium myristyl sulfate, Sodium N-lauroylzalucosinate, sodium N-myristoylsarcosinate, sodium dodecylbenzenesulfonate, sodium hydrogenated coconut fatty acid monodaliceride monosulfate, sodium lauryl sulfoacetate, sodium olefinesulfonate, Examples thereof include N-acyl daltamate such as sodium N-palmitoyl glutamate, and N-acyl taurate such as N-methyl-N-acyl sodium phosphate. Nonionic surfactants include sucrose fatty acid esters such as sucrose fatty acid esters and maltose fatty acid esters, sugar alcohol fatty acid esters such as maltitol fatty acid esters and lactol fatty acid esters, alkylol amide, and polyoxetylene sorbitan. Polyoxyethylene sorbitan fatty acid esters such as monostearate, polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil, fatty acid ethanolamides such as lauric mono- or diethanolamide, sorbitan fatty acid esters, and polyoxyethylene higher alcohol esters Ter, polyoxyethylene polyoxypropylene copolymer, polyoxyethylene polyoxypropylene fatty acid ester, polyglycerin fatty acid ester, pull mouth nick, etc. It is done. Examples of the amphoteric surfactant include N-alkyl-N-potassium oxymethyl-N-hydroxyethylimidazolymbetaine, N-radiaryldiaminoethyldaricin, and N-myristyldiaminoethyldaricin. Examples thereof include alkyldiaminoethyldaricin and sodium N-alkyl-1-hydroxyethylimidazoline betaine. These surfactants may be used alone or in combination of two or more.

The amount of the surfactant to be incorporated is preferably from 0.001 to 10%, more preferably from 0.01 to 5%, particularly preferably from 0.1 to 2% of the whole composition.

Sweeteners include saccharin sodium, stepioside, stevia extract, Examples include paramethoxycinnamic aldehyde, neohesperidyl hydrochalcone, perillartin, glycyrrhizin, thaumatin, and asparatyl phenylalanine methyl ester, which can be added in an effective amount.

As fragrances, menthol, anethole, carvone, eugenol, limonene, n-decyl alcohol, citronellol, (-one tvneol, citronellilla acetate, cineole, linalool, etil linalool, peniline, thymol, spearmint oil, peppermint oil, lemon Examples include oil, orange oil, sage oil, rosemary oil, cinnamon oil, pimento oil, laurel oil, perilla oil, winter green oil, clove oil, and yurikuri oil, which can be incorporated in effective amounts.

As preservatives, in addition to various parabens, nonionic antibacterial agents such as sodium benzoate and triclosan, cationic antibacterial agents such as benzethonium chloride and cetylpyridinium chloride, and essential oil components can be formulated in effective amounts. .

The active ingredients include enzymes such as dextranase, amylase, proteinase, and mutanase; alkaline metal monofluorophosphates such as sodium monofluorophosphate; fluorides such as sodium fluoride and stannous fluoride; Tranexamic acid, epsilon aminocaproic acid, aluminum chlorohydroxy allantoin, azulene, glycyrrhizinate, glycyrrhetinic acid, sodium chloride, vitamin (:,

Anti-inflammatory agents such as E, copper chlorophyll, copper dalconate, cetyl pyridium chloride, benzalkonium chloride, triclosan, hinokitiol, lysozyme chloride, and other bactericides; anticalculus agents such as polyphosphates; polyethylene glycol, polyvinyl pyridone And other hypersensitivity preventive agents such as aluminum lactate and potassium nitrate. The amount of the active ingredient can be an effective amount. The dentifrice composition of the present invention can be prepared by a conventional method according to the dosage form by mixing the above components. In addition, the material of the container for containing the dentifrice composition is not particularly limited, and the container used for the dentifrice composition can be used. Specifically, plastics such as polyethylene, polypropylene, polyethylene terephthalate, and nylon can be used. Container, lamine

— G (AL (aluminum) — plastic) Containers, metal containers, etc. can be used. The dentifrice composition of the present invention suppresses an increase in abrasiveness due to zeolite blending, has an appropriate tooth abrasiveness that does not damage teeth, and has an effect of preventing calculus formation derived from zeolite. It is effective for preventing tartar formation.

Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples. In the following examples,% is% by mass.

(Example Comparative Examples 1 to 5)

Granules containing the components shown in Table 1 and zeolite in the compounding ratio were prepared by a sintering method to obtain granules having the following average disintegration strength and average particle size. The average crushing strength and average particle size of the granules were measured by the following methods. The results are shown in Table 1.

Measurement of average disintegration strength of granules:

Using a Rheometer (Sun Rheometer CR-200D) manufactured by Sun Kagaku Co., Ltd., the load when the granules collapsed when one condyle was compressed at a speed of 1 O mmZ was measured 30 times repeatedly. The average value at the time was obtained and defined as the average strength of the granules.

Measurement of average particle size:

100 g of the powder was sieved with a JIS sieve to obtain a particle size distribution, and a 50% particle size was calculated, which was defined as an average particle size.

Using the obtained granules containing the following zeolite, a dentifrice composition having the composition shown in Table 2 was prepared by a conventional method, and calcium scavenging ability was measured by the following method to evaluate the abrasiveness and the tartar prevention effect. did. Table 2 shows the results.

Test method 1 (Abrasiveness):

5 g of the prepared dentifrice was dispersed in 2 OmL of water, and the copper plate whose weight was measured in advance with the dispersion was polished 200,000 times with an inclined polishing tester (manufactured by Tokyo Ishiyama Shoten). After the completion, the copper plate was taken out and dried, the weight was measured again, and the polishing property was evaluated from the difference in weight before and after polishing.

Test method 2 (calcium capturing ability):

0.02 g of the prepared toothpaste was dispersed in 20 OmL of a saturated solution of calcium ions and phosphate ions, and the pH was adjusted to 7.41 with 0.1 ml of sodium hydroxide. The test solution was transferred to an apparatus as shown in FIG. 1, and the time-dependent change in pH after adding the hydroxyapatite powder was measured. During the measurement of pH over time, the air in the container was replaced with nitrogen, and the solution was stirred with a stirrer. That is, in the apparatus shown in FIG. 1, a test solution 2 is put in a container 1, a pH electrode 3 is inserted, and a nitrogen introduction tube 4 Nitrogen is introduced into the container, and in this container 1, the time-dependent change in pH is measured while stirring the test solution 2 with a stirrer 6 in a thermostat 5 at 37 ° C. At this time, since the change in pH becomes smaller as the calcium-capturing ability becomes higher, the amount of pH change after 3 hours was calculated, and the calcium-capturing ability was evaluated.

[table 1]

* 1: Zeolite (4 A zeolite, average particle size 25 m)

* 2: Caic anhydride (precipitated silica, average particle size 20 m)

* 3: Aluminum oxide (average particle size l

(α degree 60%)

[Table 2]

From the results in Table 2, when zeolite granules having an average particle size of 150 800 βΐη and an average disintegration strength of 15 100 gZ granules obtained by adding aluminum oxide and citric anhydride were added (Example), polishing was performed. In comparison with the case where zeolite granules were not blended (Comparative Example 5), there was almost no change, and the polishing property of zeolite was suppressed, and it had excellent calcium-capturing ability and was derived from zeolite. It can be understood that the tartar prevention effect was exhibited, and the object of the present invention could be achieved. (Examples 2 to 9)

A dentifrice composition having the composition shown in Table 3 was prepared by a conventional method, and the calcium capturing ability was evaluated in the same manner as described above. Table 3 shows the results. As the zeolite granules, those shown in Table 4 were used.

From the results in Table 3, it was confirmed that the dentifrice composition of the present invention (Example) had a small pH change amount, had an excellent calcium capturing ability, and satisfactorily exhibited the effectiveness of zeolite. In addition, as a result of evaluating the polishing properties in the same manner as described above, all the dentifrice compositions showed almost the same polishing properties as the case of Example 1 as compared with the dentifrice composition containing no zeolite granules. No change was observed, confirming that the polishing property was suppressed.

[Table 3]

〇:

1 or more and less than 0.2

X: pH change is 0, 2 or more Ho 4]

* 4: Zeolite (4 A type zeolite, average particle size 25)

* 5: Caic anhydride (precipitated silica, average particle size 25 ^ m)

* 6: Aluminum oxide (average particle diameter lm, degree of a conversion 60%)

Claims

The scope of the claims

1. A dentifrice composition comprising zeolite, aluminum oxide, and silicic acid, granules having an average particle size of 150 to 800 [im, and an average disintegration strength of 15 to 100 gZ.

2. The content of zeolite in the granules is 50 to 99% by mass, the content of aluminum oxide is 0.5 to 25% by mass, and the content of gay anhydride is 0.5 to 25% by mass. The dentifrice composition according to claim 1.

3. The dentifrice composition according to claim 1, wherein the blending amount of the granules is 1 to 50% by mass of the whole composition.