JPS6234007B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a stable oral composition containing extracts of plants of the Lamiaceae family, such as sage and rosemary. Extracts of plants of the Lamiaceae family, such as sage and rosemary, are blended into oral compositions such as toothpaste to provide effects such as suppressing bad breath, and especially when used in combination with sodium alkyl sulfate and monoglyceride laurate, When used synergistically, they exhibit excellent antibacterial activity specifically against Fusobacterium nucleatum (Japanese Patent Application Nos. 139075 and 139076). However, when an extract of a Lamiaceae plant is blended into an oral composition, there is a problem with its storage stability, and its effects may not be fully exhibited if stored for a long period of time. The present inventors conducted various studies to solve the above problems, and found that by adjusting the pH of the oral composition to an acidic range, more preferably 6.6 or less,
The inventors have discovered that the deactivation of extracts of plants of the Lamiaceae family, such as sage and rosemary, is suppressed and that the storage stability of oral compositions containing this extract as an active ingredient is improved, leading to the present invention. It is something. The present invention will be explained in more detail below. The present invention is a composition in which an extract of a plant of the Lamiaceae family is blended into an oral composition such as a toothpaste, a liquid toothpaste, a mouthwash, etc., and the pH of the oral composition is adjusted to an acidic range. This increases the stability of extracts from plants belonging to the Lamiaceae family. In this case, the raw materials used to obtain extracts of plants of the Labiata family, such as sage and rosemary, include powders of plants of the Labiata family, such as sage and rosemary; residues and other essential oils obtained by extracting oil from these plants by steam distillation; Collection residue; or by extracting Lamiaceae plants such as sage and rosemary with a polar solvent such as ethyl ether, ethylene chloride, dioxane, acetone, lower alcohol such as ethanol or methanol, ethyl acetate, propylene glycol, glycerin, or water. Obtained oleoresin and its extraction residue; Lamiaceae plants such as sage and rosemary are mixed with n-hexane, petroleum ether,
An oleoresin obtained by extraction with a nonpolar solvent such as ligroin, cyclohexane, carbon tetrachloride, chloroform, dichloromethane, 1,2-dichloroethane, toluene, benzene, etc., and an extraction residue thereof are used. . When obtaining extracts of Lamiaceae plants from these raw materials, one or more of these raw materials are mixed with a polar solvent and/or
Alternatively, extraction is performed with a non-polar solvent (the solvents listed above may be used), and the extract (extract liquid or a product from which the solvent has been distilled off) is collected. In the present invention, this extract can be used as it is, but it is also possible to use a steam distillation residue obtained by subjecting this extract to a steam distillation treatment, or a steam distillation residue obtained by subjecting this extract or the steam distillation residue to activated carbon, diatomaceous earth, or acid clay. It is also possible to suitably use extracts of plants of the Lamiaceae family, such as extracts treated with adsorbents such as L. Note that a known method can be used as the extraction method, for example, a method such as digesting a dried powder of a Lamiaceae plant in a solvent can be used. In this case, the solvent is preferably an organic solvent, and an organic solvent extract obtained by extracting the raw material with an organic solvent is more effective. In the present invention, as the extract of the Lamiaceae plant, one type obtained by the above-mentioned method may be used, or two or more types may be used in combination. In addition, the amount of extracts of Lamiaceae plants such as sage and rosemary added to the oral composition is
0.0005% (weight%, same below) to 5%, especially
It is preferably 0.005 to 2%. As other components of the present invention, appropriate components are used depending on the type of oral composition. For example, in the case of toothpaste, dibasic calcium phosphate dihydrate and anhydrous salt, calcium carbonate, calcium pyrophosphate, calcium sulfate, insoluble sodium metaphosphate, amorphous silica, crystalline silica, aluminosilicate, aluminum hydroxide, Abrasives such as aluminum oxide and resin (compounding amount usually 20-60
%), carboxymethyl cellulose, hydroxyethyl cellulose, alginate, carrageenan,
Contains binders such as gum arabic and polyvinyl alcohol (0.3 to 5%), thickeners such as polyethylene glycol, sorbitol, glycerin, and propylene glycol (10 to 70%), and, if necessary, sodium alkyl sulfate and dodecyl. Foaming agents such as sodium bebezenesulfonate, sodium hydrogenated coconut fatty acid monoglyceride monosulfate, sodium lauryl sulfoacetate, sodium N-lauroylsarcosinate, N-acylglutamate, lauryl diethanolamide, sucrose fatty acid ester (0.5%) is blended. Furthermore, essential oils such as peppermint and spearmint, fragrance materials such as l-menthol, carvone, eugenol, and anethole, saccharin sodium, stevioside, neohesperidyl dihydrochalcone, glycyrrhizin, perillartin, p-methoxycinnamic aldehyde, and thaumatin. Components such as sweeteners and preservatives may also be included. In addition, in the present invention, in addition to extracts of plants of the Lamiaceae family, such as sage and rosemary, lysozyme chloride, dextranase, lytic enzyme, mutanase,
Chlorhexidine or its salts, sorbic acid, alexidine, hinokitiol, cetylpyridinium chloride, alkylglycine, alkyldiaminoethylglycine salt, allantoin, ε-aminocaproic acid, tranexamic acid, azulene, vitamin E, sodium monofluorophosphate, sodium fluoride, Active ingredients such as stannous fluoride, water-soluble primary or secondary phosphates, quaternary ammonium compounds, and sodium chloride may also be incorporated. Of the above ingredients, when sodium alkyl sulfate or monoglyceride lauric acid is used in combination with extracts of plants of the Lamiaceae family, such as sage and rosemary, these act synergistically against Fusobacterium sculatum and exhibit a high antibacterial effect. Therefore, sodium caprylic sulfate, sodium lauryl sulfate, sodium myristyl sulfate, sodium palimithylsulfate, etc. have an alkyl group with a carbon number of 8 to 18.
0.1-5% of the total sodium alkyl sulfate,
In particular, 0.5 to 3%, or lauric acid monoglyceride 0.001 to 10%, especially 0.01 to 3%.
It is preferable to mix them. The oral composition of the present invention is prepared by blending appropriate ingredients depending on the type of composition in addition to the extract of the Lamiaceae plant. It is preferably prepared to have a pH of 6.6 or less, thereby suppressing the deactivation of the extract of the Lamiaceae plant and increasing the storage stability of the composition. On the other hand, if the pH of the oral composition is 7 or higher, the extract of the Lamiaceae plant will be severely deactivated, making it impossible to achieve the object of the present invention. The method for adjusting the pH of the oral composition to an acidic range is not particularly limited. When insoluble sodium metaphosphate, calcium pyrophosphate, or silica is used alone as an abrasive, the composition can be made acidic as it is. Also, citric acid, tartaric acid,
By blending acidic substances such as malic acid, malonic acid, maleic acid, succinic acid, acetic acid, organic acids and their salts such as phosphonic acid, phosphoric acid and its salts, sulfuric acid, hydrochloric acid, and stannous fluoride, acidic It can also be prepared in the area. Thus, oral compositions in the acidic range,
The extract of the Lamiaceae plant is stably retained for a long period of time and effectively exhibits its effects over a long period of time. Next, a production example of the Lamiaceae plant used in the present invention will be shown. Production Example 300 ml of methanol was added to 100.0 g of dry sage powder, and the mixture was refluxed for 1 hour on a water bath at 70 to 80°C with a cooling tube attached. Next, the methanol fraction was separated, fresh methanol was added to the residue, and the same reflux was repeated twice, for a total of three extraction operations. The methanol extracts were collectively concentrated under reduced pressure to obtain 27.4 g of a dark green paste. Further, 150 ml of methanol was added to 30 g of dried rosemary powder, and the mixture was refluxed for 1 hour on a water bath at 70 to 80° C. with a cooling tube attached. The following procedure was carried out in the same manner as in the case of sage to obtain 7.3 g of a dark greenish brown solid. Other solvents were operated in the same manner as above to obtain various extracts of sage and rosemary. Table 1 shows the extraction results.

[Table] Hereinafter, the present invention will be specifically explained with reference to Examples and Comparative Examples. Examples 1 to 3, Comparative Examples 1 to 3 Toothpastes having the following formulations with various pH values were prepared by adjusting the pH values as shown in Table 2. Prescription abrasive (silica) 40.0g Propylene glycol 2.0 Glycerin 25.0 Carboxymethyl cellulose 1.0 Fragrance 1.0 Rosemary extract No. 6 0.05 Satucalin 0.1 Sodium lauryl sulfate 1.5 Water Remaining 100.0% Next, immediately after preparing the above toothpaste and at 50℃, 1 The effectiveness (stability) of the rosemary extract after storage for 2 months and at 50°C for 2 months was evaluated by the following method for measuring deodorization rate. The results are shown in Table 2. How to measure deodorization rate: Put 1.5 ml of Tris/hydrochloric acid buffer and 1 g of sample (toothpaste) into a test tube with a capacity of approximately 23 ml. Add 0.5 ml of 1 ppm methyl mercaptan CH ₃ SH solution to this, cover with a rubber stopper, and stir for 1 minute. Next, the test tube is incubated at 37°C for 6 minutes. Inject 5 ml of air into the test tube and stir for 30 seconds. Collect 5 ml of headspace gas in a test tube. This is injected into a gas chromatograph and the integral counts of the methyl mercaptan peak are shown. The deodorization rate is obtained by the following formula. Deodorization rate = C-S/C x 100% C: CH ₃ SH integral count of toothpaste immediately after preparation S: CH ₃ SH integral count of sample toothpaste

[Table] From the results in Table 2, it is found that toothpaste with a pH in the acidic range stably retains rosemary extract. Example 4 Toothpaste Propylene Glycol 2.0% Sorbit (60% liquid) 30.0 Carboxymethyl cellulose 1.0 Calcium phosphate dihydrate 45.0 Sodium phosphate 0.5 Flavor 1.0 Rosemary extract No. 6 0.15 Satucalin 0.1 Sodium lauryl sulfate 1.5 Water Residual 100.0% PH after 3 months storage at 40℃ 6.74 〃 Deodorization rate 65% Example 5 Toothpaste propylene glycol 2.5% Glycerin 26.0 Carrageenan 1.0 Dibasic calcium phosphate 40.0 Tartaric acid 0.1 Titanium oxide 5.0 Flavoring 1.0 Rosemary extract No. 9 0.25 Satucalin 0.1 Lauryl diethanolamide 1.2 Water Remaining 100.0% PH after 3 months storage at 40℃ 〃 Deodorization rate 70% Example 6 Toothpaste propylene glycol 2.0% Sorbit (60% liquid) 15.0 Glycerin 10.0 Carboxymethyl cellulose 0.9 Dibasic calcium phosphate・Dihydrate 42.0 Citric acid 0.1 Fragrance 1.0 Rosemary extract No.10 0.05 Saccharin 0.1 Sodium lauryl sulfate 1.5 Water Remaining 100.0% PH after 3 months storage at 40℃ 6.50 Deodorization rate 52% Example 7 Propylene toothpaste Glycol 2.5% Sorbit (60% liquid) 30.0 Carboxymethyl cellulose 1.0 Calcium phosphate dihydrate 20.0 Silica 10.0 Titanium oxide 5.0 Flavor 1.0 Rosemary extract No. 7 0.25 Satucharin 0.1 Sodium lauryl sulfate 1.5 Water Balance 100.0% 40℃, 3 PH after storage for months 6.71 〃 Deodorization rate 74% Example 8 Toothpaste propylene glycol 2.0% Sorbiturate solution (60%) 32.0 Carboxymethylcellulose 1.2 Dibasic calcium phosphate dihydrate 30.0 Insoluble sodium metaphosphate 10.0 Flavor 1.0 Rosemary extract No.6 0.15 Satucalin 0.1 Sodium lauryl sulfate 1.0 Water Remaining 100.0% PH after 3 months storage at 40℃ 6.40 〃 Deodorization rate 61% Example 9 Toothpaste propylene glycol 2.0% Glycerin 25.0 Carboxymethyl cellulose 1.0 Insoluble sodium metaphosphate 45.0 Hydrochloric acid Chlorhexidine 0.001 Fragrance 1.0 Rosemary extract No.5 0.15 Satucharin 0.1 Sodium lauryl sulfate 1.5 Water Remaining 100.0% PH after 3 months storage at 40℃ 4.91 〃 Deodorization rate 64% Example 10 Toothpaste propylene glycol 2.0% Sorbit (60 % liquid) 28.0 Carboxymethyl cellulose 1.1 Calcium pyrophosphate 45.0 Flavor 1.0 Sage extract No. 1 0.1 Saccharin 0.1 Sodium lauryl sulfate 1.5 Water Remaining 100.0% PH after 3 months storage at 40℃ 5.81 〃 Deodorization rate 63% Example 11 Toothpaste Propylene glycol 2.5% Glycerin 25.0 Carboxymethyl cellulose 1.0 Silica 25.0 Fragrance 1.0 Sage extract No. 4 0.15 Saccharin 0.11 Sodium lauryl sulfate 1.0 Water Remaining 100.0% PH after 3 months storage at 40℃ 6.64 〃 Deodorization rate 62% Example 12 Washing Mouthwatering ethanol 1.0% Glycerin 1.0 Polyoxyethylene hydrogenated castor oil derivative 0.6 Rosemary extract No. 6 0.15 Satucharin 0.05 Fragrance 0.2 NaH ₂ PO ₄ 0.5 Water Remaining 100.0% PH after 3 months storage at 40℃ 5.0 〃 Deodorization rate 72%

Claims (1)

[Scope of Claims] 1. An oral composition containing an extract of a plant belonging to the Lamiaceae family and having a pH in the acidic range. 2. The oral composition according to claim 1, which has a pH of 6.6 or less. 3. The oral composition according to claim 1, wherein the Lamiaceae plant is sage or rosemary.