KR19980081637A - Oral composition - Google Patents

Abstract

It relates to an oral composition containing a water-insoluble noncationic fungicide which exhibits improved stability and improved rheological properties over time and which is excellent in removing tooth plaque, preventing bad breath and removing tooth-colored substances.

The addition of porous calcium carbonate to the oral composition prevents the lowering of the bactericidal activity of water-insoluble noncationic fungicides such as triclosan, and has excellent effects on the removal of tooth plaque, prevention of bad breath and removal of tooth-colored substances. Stability is improved. In addition, the addition of sodium carboxymethyl cellulose to the oral composition can improve rheological properties and stability over time.

Description

Oral composition

The present invention relates to an oral composition exhibiting stabilized bactericidal activity of a water-insoluble noncationic fungicide when filled into a container having an innermost layer made of synthetic resin. More specifically, the present invention exhibits an excellent effect of inhibiting viscosity change and thixotropy properties at high temperatures, preventing solid-liquid separation in stability over time, further removing tooth plaque, preventing bad breath and tooth-coloring It relates to an oral composition which exhibits an excellent effect on the removal of substances.

Plaques adsorbed on teeth have been pointed out as an important factor causing gingivitis. In order to remove plaque of teeth, the oral cavity is physically washed with a brush or the like. However, cleaning the mouth with a brush takes a long time, and the removal effect of the tooth plaque thus achieved is still insufficient.

Under these circumstances, research has been undertaken to develop oral compositions such as toothpastes containing fungicides to achieve the additional effect of removing plaque on teeth. In particular, cationic fungicides are known to be effective in preventing the formation of tooth plaques. However, cationic fungicides are difficult to process into formulations due to poor compatibility with other components in the composition. To overcome this problem, it has recently been proposed to add water-insoluble noncationic fungicides (such as triclosan) which are highly compatible with other ingredients in the composition to the oral composition.

However, when a composition containing such a water-insoluble non-cationic bactericidal agent is filled into a container made of synthetic resin, the stability of these bactericides decreases with time, and the bactericidal effect is lowered because the bactericide is adsorbed on the inner wall of the container. do.

In order to solve this problem, JP-A 20288820, JP-A 6-92830, and JP-A 6-279248 disclose, for example, by improving the container using a specific polymer as the innermost layer of the container. It has been proposed to prevent the adsorption of nonionic bactericides to (the JP-A used here means published Japanese patent applications of unexamined).

On the other hand, JP-A No. 8-198623 discloses that porous calcium carbonate having excellent oil and water absorption properties has been developed and useful as a food additive. However, the use of such porous calcium carbonate in oral compositions for stabilizing fungicides, removing tooth plaques, preventing bad breath and the like has not been proposed until now.

An object of the present invention is sodium carboxymethyl cellulose having an average degree of etherification of 0.5 to 1.8 without deterioration in stability and the bactericidal activity of a water-insoluble noncationic fungicide over time even when using a conventionally used synthetic resin material such as polyethylene. It is further intended to provide an oral composition in which viscosity change and thixotropy properties at high temperatures are suppressed and solid-liquid separation and rough skin are prevented in stability over time.

Another object of the present invention is to provide an oral composition for the removal of tooth plaque, prevention of bad breath and removal of tooth-colored substances.

In order to achieve the above-mentioned object, the present inventors have intensively studied, the oral composition containing the porous calcium carbonate and water-insoluble non-cationic fungicides, the time of the water-insoluble non-cationic fungicide due to the effect of the porous calcium carbonate By increasing the stability according to the formulation of sodium carboxymethyl cellulose having an average degree of etherification of 0.5 to 1.8, it shows an improved effect of rheological properties as a formulation and stability over time, elimination of tooth plaque, prevention of bad breath and teeth It has been found that this represents an improved effect of the removal of pigmented material. The present invention has been completed based on this finding.

In the present invention, the improvement of rheological properties and stability over time as a formulation means that the viscosity change and thixotropy properties at high temperatures are suppressed and solid-liquid separation and rough skin are prevented in stability over time.

Porous calcium carbonate used in the present invention is usually used to form secondary particles by heavy calcium carbonate that does not form secondary particles, ultra fine precipitated calcium carbonate particles (e.g., primary particle size of 0.02 to 0.08 mu m) or natural aggregation. It is a porous precipitated calcium carbonate having high purity and high porosity in which secondary particles are formed by multistage carboxylation of chain fine particles and the like, different from precipitated calcium carbonate. This is available, for example, as PORECAL-N (manufactured by Shiraishi Calcium K.K.).

Porous calcium carbonate used in the present invention is not limited thereto, but the primary particle diameter of 0.05 to 0.5 μm, more preferably 0.1 to 0.5 μm, bulk density of 0.05 to 0.8 g / ml and BET of 15 to 100 m 2 / g Have a specific surface area. The porous calcium carbonate used in the present invention preferably has a secondary particle diameter of 1 to 5 mu m.

Porous calcium carbonate used in the present invention can be prepared by multistep carboxylation of chain fine particles, for example as disclosed in JP-A No. 8-198623.

The content of porous calcium carbonate in the oral composition of the present invention may range from 0.1 to 40% by weight, preferably from 0.5 to 10% by weight. If the content of the porous calcium carbonate is less than 1% by weight, the stability of the water-insoluble noncationic fungicide tends not to be sufficiently increased. On the other hand, when the content of porous calcium carbonate exceeds 40% by weight, the effect tends not to be improved any more.

The water insoluble noncationic bactericide used in the present invention is at least one compound selected from halogenated diphenyl ethers, salicylic halides, halogenated carboanilides, p-hydroxybenzoic acid esters and phenolic compounds.

Examples of halogenated diphenyl ethers include 2 ', 4,4'-trichloro-2-hydroxy-diphenyl ether (triclosan) and 2,2'-dihydroxy-5,5'-dibromo-diphenyl Ethers are included. Examples of halogenated salicylicanilides include 4 ', 5-dibromosalicylicanilide, 3,4', 5-trichlorosalicylicanilide, 2,3,3 ', 5-tetrachlorosalicylate, and 3,5- Dibromo-3'-trifluoromethylsalicyline anlide. Examples of halogenated carboanilides include 3,4,4'-trichlorocarboanilide and 3-trifluoromethyl-4,4'-dichlorocarboanilide. Examples of p-hydroxybenzoic acid esters include methyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, propyl p-hydroxybenzoate and butyl p-hydroxybenzoate. Examples of phenolic compounds include isopropylmethyl phenol.

Of the water-insoluble noncationic fungicides, halogenated diphenyl ethers are preferred, and trichloroic acid (2 ', 4,4'-trichloro-2-hydroxy-diphenyl ether) is particularly preferred. In the present invention, the content of the water-insoluble non-cationic fungicide may be in the range of 0.001 to 3% by weight, preferably 0.01 to 1% by weight based on the total composition. If the content of the water-insoluble noncationic bactericide is less than 0.001% by weight, a sufficient bactericidal effect tends not to be achieved. On the other hand, if the content exceeds 3% by weight, the resulting composition tends to irritate the oral mucosa, which is a problem in practical use.

In the oral composition used in the present invention, at least one sodium carboxymethyl cellulose having an average degree of etherification of 0.5 to 1.8 is blended. The lower limit of the average etherification degree of sodium carboxymethyl cellulose is preferably 0.6, more preferably 0.8. The upper limit of the average etherification degree of sodium carboxymethyl cellulose is preferably 1.5. In particular, it is preferred to combine sodium carboxymethyl cellulose with different average etherification degrees of 0.8 to 1.1 and 1.2 to 1.5 in the oral composition of the present invention.

If the degree of etherification is less than 0.5, the rheological properties and stability over time tend not to be sufficiently improved. If the degree of etherification exceeds 1.8, the tendency is not maintained.

The sodium carboxymethyl cellulose used in the present invention may be formulated in an amount of 0.1 to 5.0% by weight, preferably 0.5 to 3.0% by weight, based on the total amount of the oral composition. If the content of sodium carboxymethyl cellulose is less than 0.1% by weight, it tends to be difficult to suppress solid-liquid separation. If the content of sodium carboxymethyl cellulose is greater than 5% by weight, the oral composition tends to solidify.

The oral composition of the present invention can be processed into toothpaste, powder toothpaste, liquid toothpaste, ointment, skin paste, chewing gum and the like. Among these, toothpaste is preferable from a practical point of view. These compositions are, for example, in the form of monolayer tubes, laminated tubes, bottles, jars, etc., made of polyolefin resins (polyethylene, polypropylene, etc.) and polyesters, polyethylene terephthalates, polycarbonates, polystyrenes, polyamides and polyvinyl chloride resins. It can be filled in any commonly used resin container having a.

In addition to the essential (and additional) components as described above, the oral composition of the present invention may further contain suitable ingredients conventionally used in the art so long as the effects of the present invention are not impaired.

In the case of toothpaste, for example, calcium carbonate, calcium phosphate, dibasic calcium phosphate, calcium pyrophosphate, insoluble sodium metaphosphate, titanium dioxide, amorphous silica, crystalline silica, aluminosilicate, aluminum oxide, aluminum hydroxide, resins, hydroxides Abrasives such as apatite can be used alone or as a mixture of two or more. The content of these components is generally in the range of 10 to 60% by weight, based on the total composition.

Examples of anionic surfactants useful as blowing agents or detergents include sodium alkylsulfate (sodium laurylsulfate, sodium myristyl sulfate, etc.), sodium N-acylsarcosinate (sodium N-lauroyl sarcosinate, sodium N-myri). Stole sarcosinate, etc.), N-acylglutamate (sodium N-palmitoylglutamate, etc.), and sulfosuccinic acid surfactants (polyoxyethylene alkyl disodium sulfosuccinate, dialkyl sodium sulfosuccinate, etc.) Included.

Examples of nonionic surfactants useful herein include sugar fatty acid esters (sucrose fatty acid esters, maltose fatty acid esters, lactose fatty acid esters, etc.), polyoxyethylene alkyl ethers, fatty acid alkanolamides, polyoxyethylene sorbitan fatty acid esters (polyoxy Ethylene sorbitan monolaurate, polyoxyethylene sorbitan monostearate, etc.), polyoxyethylene fatty acid esters (such as polyoxyethylene hardened castor oil), sorbitan fatty acid esters, fatty acid monoglycerides, and polyoxyethylene / polyoxypropylene blocks Copolymers are included.

Examples of amphoteric surfactants useful herein include N-alkyldiaminoethylglycine (N-lauryldiaminoethylglycine, N-myristyldiethylglycine, etc.), N-alkyl-N-carboxymethylammonium betaine, 2 -Alkyl-1-hydroxyethylimidazoline betaine sodium and lauryldimethylaminoacetic acid betaine. One or a mixture of two or more of these surfactants may be used. Its content is preferably 0.1 to 10% by weight based on the total composition.

As a thickener in addition to sodium carboxymethyl cellulose, cellulose derivatives (hydroxyethyl cellulose, etc.), alkali metal alginates (sodium alginate, etc.), gums (carrageenan, xanthan gum, tragacanth gum, acacia, etc.), synthetic thickeners ( Polyvinyl alcohol, sodium polyacrylate, and the like), inorganic thickeners (silica gel, aluminum silica gel, rubber wood, etc.) and the like. One or a mixture of two or more of these thickeners may be used. Its content is generally in the range of 0.1 to 10% by weight, based on the total composition.

As the humectant, sorbitol, glycerin, ethylene glycol, propylene glycol, 1,3-butylene glycol, polyethylene glycol, polypropylene glycol, xylitol, maltitol, lactitol and the like can be used. One or a mixture of two or more of these wetting agents can be used. Its content is generally in the range of 5 to 70% by weight, based on the total composition.

As pH-adjusting agents, citric acid, phosphoric acid, malic acid, pyrophosphoric acid, lactic acid, tartaric acid, glycerophosphoric acid, acetic acid, nitric acid, silicic acid, chemically available salts thereof, sodium hydroxide and the like can be used. One or a mixture of two or more of these pH-adjusting agents can be used to adjust the pH value of the composition to 5-9. Its content is generally in the range of 0.01 to 2% by weight, based on the total composition.

In addition, the oral composition of the present invention is menthol, carbon, eugenol, methyl eugenol, methyl salicylate, methyl eugenol, thymol, anetol, limonene, ocymen, n-decyl alcohol, citronellol, α- Terpineol, methyl acetate, citronenyl acetate, cineol, linalol, ethylinalol, vanillin, thyme, nutmeg, spearmint oil, peppermint oil, lemon oil, orange oil, sage oil, rosemary oil, cinnamon oil, honey grass Flavoring agents such as oil, donglock oil, sperm oil, eucalyptus oil and piment oil may be contained. One or a mixture of two or more of these flavors may be used. Its content is in the range of 0.1 to 5% by weight, preferably 0.5 to 2% by weight, based on the total composition.

In addition, the oral compositions of the present invention comprise sodium saccharin, acesulfame potassium, stevioside, neohesperidyl dihydrochalcone, glycyrrhizin, peraryllatin, taumartin, aspartylphenylalanyl methyl ester and xylitol. May contain the same sweetener. The sweetener content is in the range of 0.01 to 1% by weight, preferably 0.05 to 0.5% by weight, based on the total composition.

The oral composition of the present invention may contain pharmaceutical ingredients in addition to water-insoluble non-cationic fungicides, such as vitamin E homologues (dl-α-tocopherol acetate, tocopherol succinate, tocopherol nicotinate, etc.), cationic fungicides (chlorexidine hydro) Chloride, cetylpyridinium chloride, benzetonium chloride, etc.), amphoteric fungicides (such as dodecyldiaminoethylglycine), enzymes (dextranase, amylase, protease, mutanase, lysozyme, lysine enzymes, etc.), alkali metal mono Fluorophosphates (sodium monofluorophosphate, potassium monofluorophosphate, etc.), fluorides (sodium fluoride, tin fluoride, etc.), tranexamic acid, epsilon-aminocaproic acid, aluminum chlorohydroxyalantoin, dihydrocholesterol, glycyrrhizin salt , Glycyrrhizinic acid, glycerophosphate, chlorophyll, sodium chloride, caropeptide and water soluble It may further contain an inorganic phosphoric acid compound. One or a mixture of two or more of these components may be used.

In order to further illustrate the invention in more detail, the following examples are described, though not limited thereto. In these examples, all content is in weight percent.

Example

[Test Example]

1. Evaluation of the stability of non-cationic fungicides

(1) Preparation of Sample

Toothpaste of the following composition is prepared by a conventional method, and filled into a laminated tube having polyethylene in the innermost layer. After 1 month of storage at 40 ° C, the residual rate and bactericidal effect of triclosan are evaluated by the method described below.

ingredient content(%)

Porous Calcium Carbonate Listed in Table 1

Heavy calcium carbonate as described above

Anhydrous silica 3.0

Sorbitol listed in Table 1

Sodium Carboxymethyl Cellulose Listed in Table 1

Sodium Lauryl Sulfate Listed in Table 1

Nonionic Surfactant As described above

Saccharin Sodium 0.1

Flavor 1.0

Water Insoluble Non Cationic Sterilizer 0.3

Purified water level

Total 100.0

(2) Measurement method of residual rate of water-insoluble non-cationic disinfectant

Hereinafter, the measuring method of the residual rate of a water-insoluble noncationic disinfectant is demonstrated using triclosan as an example.

(Measurement Method of Residual Rate of Triclosan)

20 ml of methanol is added to each toothpaste prepared above (2.5 g). The resulting mixture is stirred for 20 minutes to disperse the methanol completely in the toothpaste, followed by centrifugation at 17,000 rpm for 10 minutes to obtain a supernatant. The residue is treated the same twice additionally and the supernatant is combined. Methanol is then added to bring the total volume to 100 ml. Using the resulting mixture as a sample, triclosan is measured by liquid chromatography. The residual ratio of triclosan is measured according to the following equation and evaluated based on the criteria given below.

Residual rate (%) = (Triclosan content after 1 month / Triclosan content at manufacture) x100

standard :

(Circle): Triclosan residual ratio≥90%.

X: Triclosan residual rate 90%.

(Sterilization activity test)

5 ml of a 4-fold slurry of toothpaste is added to 0.1 ml of a suspension of Streptococcus mutaus (10 ⁸ to 10 ⁹ CFU / ml). After incubation at 37 ° C. for 3 minutes, the sample solution is inoculated on trypticase / soybean / agar (TSA) plates and subjected to anaerobic conditions (N ₂ / H ₂ / CO ₂ = 85/10/5) for 2 days. After incubation at 37 ° C., the minimum fungicide concentration (%; hereafter simply referred to as MBC) is measured. As a standard, 0.05% aqueous triclosan solution (dissolved in a small amount of SLS) is used. Evaluation is based on the following criteria.

standard :

○: The MBC of the sample is comparable to or lower than that of the standard MBC.

X: MBC of a sample is higher than MBC of a standard.

Table 1 summarizes the data of triclosan residual and the results of the bactericidal activity test.

As clearly shown in Table 1, the products of the present invention containing porous calcium carbonate have improved stability over time and continued bactericidal activity compared to the comparative products.

ingredient Example (%) Comparative Example (%) One 2 3 4 5 6 7 One 2 3 Porous calcium carbonate ¹⁾ 0.1 40.0 10.0 2.0 7.0 5.0 5.0 - - - Heavy calcium carbonate 35.0 - 20.0 25.0 20.0 35.0 35.0 30.0 - - Calcium phosphate - - - - - - - 10.0 40.0 - Anhydrous silica 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 8.0 Triclosan 0.001 3.0 1.0 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Sorbitol 35.0 35.0 35.0 35.0 35.0 35.0 10.0 35.0 35.0 35.0 Sodium carboxymethylcellulose ²⁾ 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Sodium lauryl sulfate 2.0 0.2 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Saccharin Sodium 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Flavor 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 Purified water Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount total 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 evaluation Residues Of Nonionic Sterilizers ○ ○ ○ ○ ○ ○ ○ × × × Bactericidal activity ○ ○ ○ ○ ○ ○ ○ × × ×

Porous calcium carbonate ¹⁾ : average primary particle diameter of 0.2 µm, bulk density 0.5 g / ml, and BET specific surface area of 23 m ²

Sodium carboxymethyl cellulose ²⁾ : etherification degree 1.2

2. Tooth plaque-removal model examination

(1) Preparation of Sample

Toothpastes having the following compositions are prepared in a conventional manner and used for evaluation.

ingredient content(%)

Powder Ingredients Listed in Table 2

Sorbitol 40.0

Sodium Carboxymethyl Cellulose 2.0

(Etherification degree 1.2)

Sodium Lauryl Sulfate 1.5

Pluronic-type surfactant 5.0

(POE200 POP40)

Saccharin Sodium 1.0

Flavor 1.0

Purified water level

Total 100.0

(2) evaluation

As a model of tooth plaque, S. Mutans uses 1㎎ / ㎖ solution (pH7, Vero day buffer solution) of a water insoluble glucan produced from ATCC25175 strain. 0.5 g aliquots of toothpaste (product of the invention and comparative product) described in Table 2 are mixed with 3 ml of the insoluble glucan solution mentioned above, respectively. After shaking for 30 minutes, the mixture is centrifuged and the supernatant is removed. The residue was subjected to color development of the reducing sugar by the phenol-sulfuric acid method and the absorbance was measured at 490 nm. A calibration curve is prepared by the phenol-sulfuric acid method in the same manner using the water-insoluble glucan solution described above, from which the amount of glucan adsorbed by the powder is measured. Then, the adsorption rate is computed by making the initial amount of the added glucan 100.

As shown in Table 2, the oral composition containing the porous calcium carbonate of Example 3 was applied to the product containing the conventional precipitated calcium carbonate of Comparative Example 4 or the product containing the conventional heavy calcium carbonate of Comparative Example 5. The adsorption capacity of glucan is superior. That is, the oral composition of the present invention is suitable for removing plaque of teeth.

3. Bad breath prevention model test

4 g aliquots of the quadruple slurry of Example 8 and Comparative Example 4 toothpaste as described in Table 2 are sampled and sealed in glass vials. 0.5 ml of a 2 μg / ml methylmercaptan solution in ethanol is injected into each vial and shaken gently at 37 ° C. for 10 minutes. Then, 5 ml of head space gas is taken, and the methylmercaptan contained therein is measured by gas chromatography. The concentration is measured using the calibration curve of methylmercaptan, and the deodorization rate (%) is calculated by making the initial amount of the added methylmercaptan 100.

As shown in Table 2, the product of the present invention has a better deodorizing effect than the comparative product. As such, because the porous calcium carbonate adsorbs and removes (deodorizes) the bad breath component, it is recognized that the oral composition is useful for preventing bad breath.

4. Tooth-colored substance removal model examination

As a model of the tooth-colored material, a purple solution containing 0.5% tea polyphenol and 0.5% iron (III) citrate ammonium is used. 0.5 g aliquots of the toothpaste (product of the invention and comparative product) described in Table 2 are mixed with 5 ml of the tooth-colored substance model as described above, respectively. After shaking for 30 minutes, the mixture is centrifuged and the absorbance of the supernatant is measured at 300 nm. The adsorption rate is calculated according to Equation 2 below.

Adsorption rate (%) = (A- [absorbance of the supernatant liquid after sample treatment]) / Ax100

A: absorbance of tooth-colored substance model solution

As shown in Table 2, the product of the present invention has a superior removal effect of the tooth-colored substance compared to the comparative product. Thus, oral compositions containing porous calcium carbonate are recognized to be useful for removing tooth-colored materials.

Powder ingredient content (%) Example 8 Comparative Example 4 Comparative Example 5 Porous calcium carbonate ²⁾ (average secondary particle size: 3.5㎛) 5 - - Precipitated calcium carbonate ³⁾ (secondary particles: not formed) - 35 - Heavy calcium carbonate ⁴⁾ (secondary particles: not formed) 30 - 35 evaluation Tooth plaque-removal (adsorption rate of insoluble glucan:%) 28 16 11 Bad breath prevention (methylmercaptan deodorization rate:%) 42 - 30 Tooth-colored substance removal (polyphenol + iron adsorption rate:%) 41 20 -

Porous Calcium Carbonate ²⁾ :

Average primary particle size 0.3 mu m, bulk density 0.4 g / ml, and BET specific surface area 23 m 2

Precipitated calcium carbonate ³⁾ :

Average primary particle size 1 mu m, bulk density 0.4 g / ml, and BET specific surface area 5 m 2

Heavy calcium carbonate ⁴⁾ :

An average primary particle diameter of 5 mu m, a bulk density of 1.0 g / ml, and a BET specific surface area of 1 m 2

5. Evaluation of Stability and Rheological Properties over Time of Formulations

Toothpaste described in Table 3 below was prepared according to a conventional method, and filled in a laminated tube. The obtained sample was stored at 40 ° C. for one month, and then stability over time was evaluated according to the following criteria.

(Evaluation standard of stability over time)

A: No change.

B: Slight phase separation.

C: Difficulty in phase separation and practical use.

D: Rough skin and solidification.

(Evaluation Criteria for Rheological Properties)

A: No change.

B: Slightly high thixotropy.

C: High thixotropy.

D: A viscosity falls remarkably above 40 degreeC.

ingredient Example (% by weight) Comparative Example (% by weight) 9 10 11 12 13 14 15 One 2 3 4 5 Porous calcium carbonate ¹⁾ 0.5 40.0 10.0 2.0 7.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Heavy calcium carbonate 35.0 - 20.0 25.0 20.0 35.0 35.0 30.0 20.0 20.0 20.0 20.0 Sorbitol 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 Sodium Carboxymethyl Cellulose (etherification) 0.20.40.81.21.5 --0.5-- --- 0.5- ---- 0.5 -0.30.5-- --0.2-0.5 --0.30.30.3 --- 0.5- -0.5 --- 0.5 ---- -0.5 --- 0.5 ---- ----- Xanthan gum - - - - - - - - - 1.0 - - Carrageenan - - - - - 1.0 - - - - 1.0 3.0 Sodium lauryl sulfate 2.0 2.0 1.5 1.5 1.0 1.0 0.5 - 1.0 1.5 1.5 1.5 Saccharin Sodium 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 POE (200), POP (40) block copolymer - - - - 0.5 0.5 1.0 2.0 0.5 - - - Flavor 0.5 0.1 0.2 1.0 0.1 0.5 0.5 0.5 0.2 0.8 1.8 2.8 Purified water Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount total 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 evaluation Stability over time B A A A A A A D D C D D Rheological properties A B B A A A B B B B A A Overall rating ○ ○ ○ ○ ◎ ◎ ○ × × × × ×

Porous calcium carbonate ¹⁾ : average primary particle diameter of 0.2 µm, bulk density 0.5 g / ml, and BET specific surface area of 23 m ²

As is evident from the results in Table 3, the examples incorporating porous calcium carbonate and sodium carboxymethyl cellulose having an etherification degree of 0.5 to 1.8 show a marked improvement in stability and rheological properties over time compared to the comparative examples.

Example 16

The toothpaste of the following composition is manufactured by a conventional method, and filled in the same laminated tube as mentioned above.

ingredient content(%)

Porous Calcium Carbonate 30.0

(Average primary particle size: 0.2 mu m, bulk density: 0.5 g / ml,

BET specific surface area: 23㎠)

Aluminum Hydroxide 5.0

Sorbitol 20.0

Xylitol 5.0

Sodium Carboxymethyl Cellulose 1.5

(Etherification degree: 1.3)

Sodium Lauryl Sulfate 1.5

Saccharin Sodium 0.1

Flavor 0.9

Triclosan 0.1

Purified water level

Total 100.0

Example 17

The toothpaste of the following composition is manufactured by a conventional method, and filled in the same laminated tube as mentioned above.

ingredient content(%)

Porous Calcium Carbonate 6.0

(Average primary particle size: 0.08 mu m, bulk density: 0.4 g / ml,

BET specific surface area: 35㎠)

Calcium Phosphate 25.0

Sorbitol 30.0

Propylene Glycol 5.0

Sodium Carboxymethyl Cellulose 1.2

(Etherification degree: 1.0)

Sodium N-lauryl Sarcosinate 1.5

Sodium Monofluorophosphate 0.5

Stevioside 0.1

Flavor 0.9

Isopropylmethyl phenol 0.5

Polyoxyethylene (200) / polyoxypropylene (70) 1.0

Block copolymer

Purified water level

Total 100.0

Example 18

The toothpaste of the following composition is manufactured by a conventional method, and filled in the same laminated tube as mentioned above.

ingredient content(%)

Porous Calcium Carbonate 20.0

(Average primary particle size: 0.1 mu m, bulk density: 0.2 g / ml,

BET specific surface area: 60㎠)

Sorbitol 25.0

Sodium Carboxymethyl Cellulose 1.5

(Etherification degree: 0.8)

Sodium Lauryl Sulfate 1.5

Saccharin Sodium 0.1

Flavor 0.9

Ethyl p-hydroxybenzoate 0.1

Triclosan 0.2

Sodium Fluoride 0.2

Polyoxyethylene (200) / polyoxypropylene (70) 2.0

Block copolymer

Purified water level

Total 100.0

Example 19

Liquid toothpaste of the following composition is prepared by a conventional method, and filled in a PET resin container.

ingredient content(%)

Silica Anhydrous 20.0

Porous Calcium Carbonate 0.5

(Average primary particle size: 0.05 mu m, bulk density: 0.1 g / ml,

BET specific surface area: 90㎠)

Sorbitol 25.0

Glycerin 12.0

Carrageenan 1.0

Sodium Lauryl Sulfate 1.5

Sodium benzoate 0.2

Saccharin Sodium 0.1

Flavor 0.5

Triclosan 0.3

dl-α-tocopherol acetate 0.5

Polyoxyethylene (150) / polyoxypropylene (35) 1.5

Block copolymer

Sodium Silicate 0.5

Purified water level

Total 100.0

Example 20

The toothpaste of the following composition is manufactured by a conventional method, and filled in the same laminated tube as mentioned above.

ingredient content(%)

Porous Calcium Carbonate 6.0

(Average primary particle size: 0.3 µm, bulk density: 0.4 g / ml,

BET specific surface area: 25㎠)

Calcium Phosphate 25.0

Sorbitol 30.0

Propylene Glycol 5.0

Sodium Carboxymethyl Cellulose 1.2

(Etherification degree: 1.2)

Sodium N-Lauroyl Sarcosinate 1.5

Sodium Monofluorophosphate 0.5

Stevioside 0.1

Flavor 0.9

Polyoxyethylene (200) / polyoxypropylene (70) 1.0

Block copolymer

Purified water level

Total 100.0

Example 21

The gum gum of the following composition is manufactured by a conventional method.

ingredient content(%)

Sword Base 28.0

Porous Calcium Carbonate 0.5

(Average primary particle size: 0.3 µm, bulk density: 0.4 g / ml,

BET specific surface area: 25㎠)

Xylitol 40.0

Reduced Maltose Syrup 26.5

Flavor 5.0

Total 100.0

Example 22

Liquid toothpaste of the following composition is prepared by a conventional method, and filled in a PET resin container.

ingredient content(%)

Porous Calcium Carbonate 0.5

(Average primary particle size: 0.2 mu m, bulk density: 0.5 g / ml,

BET specific surface area: 23㎠)

Precipitated Sodium Carbonate 30.0

Sorbitol 35.0

Sodium Carboxymethyl Cellulose 0.5

(Etherification degree: 1.8)

Sodium Lauryl Sulfate 1.5

Saccharin Sodium 0.1

POE (200) / POP (40) Block Copolymer 1.0

Flavor 0.9

Triclosan 0.1

Purified water level

Total 100.0

Example 23

Toothpaste of the following composition is prepared by a conventional method and filled in a laminated tube as described above.

ingredient content(%)

Porous Calcium Carbonate 5.0

(Average primary particle size: 0.2 mu m, bulk density: 0.5 g / ml,

BET specific surface area: 23㎠)

Heavy Sodium Carbonate 30.0

Sorbitol 35.0

Sodium Carboxymethyl Cellulose 0.5

(Etherification degree: 1.8)

Sodium Carboxymethyl Cellulose 0.3

(Etherification degree: 0.6)

Sodium Lauryl Sulfate 1.5

Saccharin Sodium 0.1

POE (200) / POP (40) Block Copolymer 1.0

Flavor 0.9

Triclosan 0.1

Purified water level

Total 100.0

The oral compositions prepared in Examples 16-19 exhibit high stability over time and very stable bactericidal activity of water insoluble noncationic fungicides such as triclosan. The oral compositions of Examples 16-23 are effective at removing tooth plaques, preventing bad breath and removing tooth-colored substances.

The present invention has improved stability over time of a water-insoluble noncationic bactericide in a container having an innermost layer made of synthetic resin, exhibits stabilized bactericidal activity, inhibits viscosity change and thixopropy properties at high temperatures, and It provides an oral composition which prevents solid-liquid separation in the stability according to, and is effective in removing tooth plaque, preventing bad breath and removing tooth-colored substance.

Claims (12)

An oral composition comprising porous calcium carbonate. An oral composition comprising a porous calcium carbonate and a water insoluble noncationic fungicide. The oral composition of claim 2, wherein the water-insoluble noncationic fungicide is at least one compound selected from the group consisting of halogenated diphenyl ethers, salicylic halides, halogenated carboanilides, p-hydroxybenzoic acid esters, and phenolic compounds. The oral composition according to claim 2, wherein the water-insoluble noncationic fungicide is 2 ', 4,4'-trichloro-2-hydroxy-diphenyl ether (triclosan). The oral composition of claim 1, wherein the porous calcium carbonate has an average primary particle diameter of 0.05 to 0.5 μm, a bulk density of 0.05 to 0.8 g / ml, and a BET specific surface area of 15 to 100 m 2 / g. The oral composition of claim 1, further comprising one or more sodium carboxymethyl celluloses having an average degree of etherification of 0.5 to 1.8. The oral composition of claim 2, further comprising at least one sodium carboxymethyl cellulose having an average degree of etherification of 0.5 to 1.8. 7. The oral composition according to claim 6, wherein the amount of at least one sodium carboxymethyl cellulose is 0.1 to 5% by weight based on the oral composition. 8. The oral composition of claim 7, wherein the amount of at least one sodium carboxymethyl cellulose is 0.1 to 5% by weight based on the oral composition. The oral composition of claim 1, wherein the oral composition is for removing plaque of the tooth. The oral composition according to claim 1, for preventing bad breath. The oral composition of claim 1, for removing tooth-colored material.