JPS632923B2 - - Google Patents

Description

[Detailed description of the invention]

FIELD OF THE INVENTION The present invention relates to a surfactant-free dentifrice composition containing hydroxyethyl cellulose. Conventional technology Generally, toothpaste contains abrasives, wetting agents, binders, sweeteners, flavorings, and surfactants to solubilize them, but in recent years, consumers have become more natural-oriented or safety-oriented. With the improvement of toothpaste, the demand for surfactant-free toothpaste has increased, and its market share is increasing. However, when using a toothpaste that does not contain such a surfactant, compared to a normal toothpaste that contains about 1.4% sodium lauryl sulfate as a surfactant, fragrance irritation to the oral mucosa during brushing is stronger and the usability is inferior. There is a problem. Summary of the Invention The present inventors have conducted intensive studies to obtain a surfactant-free toothpaste that does not cause fragrance irritation to the oral mucosa, and have found that hydroxyl The inventors discovered that adding ethylcellulose significantly reduces the irritation of fragrances, leading to the completion of the present invention. That is, the present invention provides a surfactant-free dentifrice composition containing hydroxyethyl cellulose. In the present invention, fragrance irritation when using the dentifrice composition has been significantly reduced because, in conventional toothpastes without surfactants, emulsification is insufficient and the fragrance is dispersed, which directly irritates the oral mucosa during brushing. This is presumed to be due to improved performance. Therefore, according to the dentifrice composition of the present invention, although it does not contain a surfactant, there is little fragrance irritation during brushing, and it has an excellent feeling of use. Detailed Description of the Invention Next, Table 1 shows the results of testing the fragrance irritation suppressing effects of various additives including hydroxyethyl cellulose. The test method is as follows. (1) Test toothpaste composition A (combined with binder) Ingredients Amount (% by weight) Calcium carbonate 40.00 Carboxyl methyl cellulose 1.00 Sodium carrageenan 0.20 Glycerin 10.00 Sorbitol 35.00 Additives Fragrances listed in Table 1 (l-menthol in the fragrance 50% by weight) 1.00 Water Balance Total 100.00 Various additives were evaluated using a toothpaste manufactured according to a conventional method with the above composition. In addition, the 2% viscosity (hereinafter abbreviated as viscosity), average degree of substitution (hereinafter abbreviated as DS), and average number of moles of ethylene oxide substitution (hereinafter abbreviated as MS) of the hydroxyethyl cellulose used were measured using a B-type viscometer.
are 500cps, 1.3 and 2.5 respectively. (2) Evaluation method Evaluation of each additive was based on the following headspace gas chromatography method and panel evaluation method. (a) Headspace gas chromatography sample preparation: 2.0 g of test dentifrice was placed in a vial (capacity: 9
ml), add 1.0 ml of ion-exchanged water, and stir quickly to make a uniform slurry. After sealing the vial, leave it at 40°C for 4 hours to equilibrate. Measurement procedure: After allowing the vial to stand, collect the headspace gas in the vial and quantitatively analyze it using a headspace gas chromatograph. L-menthol, which is the main component in fragrances, was used as an indicator substance, and the difference in the amount of l-menthol volatilized from each dentifrice due to differences in dentifrice formulation was evaluated as a peak area ratio using the following formula. Peak area ratio = Peak area (additive formulation)/Peak area (additive-free formulation) x 100 The evaluation criteria are as follows. 〇...48 or more and less than 70 △...70 or more and less than 90 ×...90 or more The results are shown in Table 1. Note that the measurement conditions of the gas chromatograph are as follows. Equipment: PerkinElmer Sigma 3B Headspace Sampler HS6 Detector: Flame Ionization Detector (FID) Column: Fused Slilica Capillary Column
OV-101 0.23mmφ×50m Column temperature: 250℃ Detector temperature: 250℃ Carrier gas: N ₂ 10ml/min Air 50ml/min H ₂ 20ml/min (b) Panel evaluation method The test toothpaste was evaluated by a panel of five experts. Fragrance irritation during use is evaluated by brushing. Table 1 shows the results of evaluating fragrance stimulation during brushing in comparison with a regular toothpaste (containing 1.4% sodium lauryl sulfate). The evaluation criteria are as follows. 0: Same as regular toothpaste 1: Almost same as regular toothpaste 2: Slightly stronger than regular toothpaste 3: Stronger than regular toothpaste 4: Very stronger compared to regular toothpaste

【table】

[Table] Next, using the same method as above, the various polysaccharide mucilage substances mentioned above, including hydroxyethyl cellulose, were tested based on the following formulation composition (each binder alone), and the results are shown below. It is shown in Table 2. Note that the hydroxyethyl cellulose used was the same as described above. Test toothpaste composition B (binder-only system) Component Amount (% by weight) Calcium carbonate 40.00 Glycerin 10.00 Sorbitol 35.00 Additive (polysaccharide mucilage) Flavoring listed in Table 2 (l-menthol in the flavoring is 50% by weight) )
2.00 water Remainder total 100.00

[Table] As is clear from Tables 1 and 2,
Among various additives other than surfactants, only hydroxyethyl cellulose among polysaccharide mucilages has an excellent effect on alleviating fragrance irritation, and even when used in combination with other binders,
May be used alone. Therefore, hydroxyethylcellulose is used as an additive (binder) in the dentifrice composition of the present invention. Furthermore, we tested and evaluated the amount of hydroxyethylcellulose used in the present invention when it was used alone and when it was used in combination with other binders using the same method as above. Third
Shown in the table. The composition of the test toothpaste is as follows. Test toothpaste composition ingredients Amount (% by weight) Calcium carbonate 40.00 Glycerin 10.00 Sorbitol 35.00 Additives (binder) Flavorings listed in Table 3 (l-menthol in the fragrance is 50% by weight)
1.00 water Remainder Total 100.00 Results were shown according to the evaluation criteria below. Physical properties (viscosity: B type viscometer, 30℃): 〇...500cps or more and 100cps or less △...less than 500cps 400cps or more, or 1000cps
More than 1,500 cps ×...Less than 400 cps or more than 1,500 cps The overall evaluation was based on the following criteria.

【table】

[Table] As is clear from Table 3, the amount of hydroxyethylcellulose in the present invention is:
The amount is preferably 0.2 to 2.0% by weight based on the total amount of the composition. If the blending amount is less than 0.2% by weight, the fragrance will be more irritating during use, while if it exceeds 2.0% by weight, an appropriate viscosity cannot be obtained. However, in a low viscosity range (0.2 to 0.7% by weight), hydroxyethyl cellulose alone cannot maintain the viscosity and shape retention properties of toothpaste, and it is preferable to use other binders together. In this case, any other binder that is commonly used in dentifrice compositions can be used. Furthermore, there are no particular limitations on the degree of polymerization, average degree of substitution (DS), average number of moles of ethylene oxide substitution (MS), etc. of hydroxyethylcellulose, and any commercially available hydroxymethylcellulose can be used. In addition to the above fragrance and hydroxyethylcellulose, the toothpaste composition of the present invention may contain any of the abrasives, wetting agents, binders, sweeteners, etc. used in ordinary toothpastes in addition to surfactants. , these are processed according to conventional methods to obtain a dentifrice composition. Examples Next, the present invention will be explained in more detail with reference to examples. In addition, all % means weight %, and viscosity means 2% viscosity at 20° C. measured with a B-type viscometer. Example 1 A toothpaste composition was manufactured according to a conventional method using the following component composition. Ingredients Amount (%) Calcium carbonate 40.00 Carboxymethylcellulose 0.90 Sodium carrageenan 0.20 Glycerin 10.00 Sorbitol 35.00 Water 12.60 Fragrance 1.00 Hydroxyethylcellulose 0.30 (Viscosity: 10000cps, DS: 1.0, MS: 1.8) Fragrance when using the obtained toothpaste The irritation was comparable to that of products containing ordinary surfactants, the viscosity was appropriate, and the stability over time was also good. Example 2 Component Amount (%) Calcium hydrogen phosphate 45.00 Glycerin 8.00 Sorbitol 12.00 Water 32.55 Satucalin sodium 0.20 Bactericide and preservative 0.10 Flavor 1.00 Allantoin chlorohydroxy 0.05 Aluminum hydroxyethyl cellulose 1.20 (Viscosity: 500 cps, DS: 1.3, MS: 2.5) A toothpaste composition was obtained in the same manner as in Example 1 using the above blending amount. The fragrance irritation during use of the resulting toothpaste was comparable to that of a toothpaste containing a normal surfactant, as in Example 1, the viscosity was appropriate, and the stability over time was also good. Example 3 Ingredients Amount (%) Aluminum hydroxide 45.00 Carboxymethyl cellulose 0.50 Sodium carrageenan 0.50 Glycerin 10.00 Sorbitol 10.00 Water 32.00 Satucalin sodium 0.20 Bactericides and preservatives 0.10 Fragrance 1.00 Lysozyme chloride 0.50 Hydroxyethyl cellulose 0.20 Degree: 100000cps, DS : 1.2, MS: 2.5) A toothpaste composition was obtained in the same manner as in Example 1 using the above blending amounts. The fragrance irritation during use of the obtained toothpaste was comparable to that of a toothpaste containing a normal surfactant, as in Example 1, and the viscosity was appropriate and the stability over time was also good. Example 4 Silicic anhydride 15.00 Sodium polyacrylate 1.10 Glycerin 10.00 Sorbitol 60.00 Water 11.34 Satucalin sodium 0.20 Bactericides and preservatives 0.10 Fragrance 1.00 Sodium monofluorophosphate 0.76 Hydroxyethyl cellulose 0.50 (Viscosity: 20 cps, DS: 1.3, MS: 2.5) A toothpaste composition was obtained in the same manner as in Example 1 using the above blending amount. The fragrance irritation during use of the obtained toothpaste was comparable to that of a toothpaste containing a normal surfactant, as in Example 1, and the viscosity was appropriate and the stability over time was also good.

Claims (1)

[Scope of Claims] 1. A surfactant-free toothpaste composition characterized by containing hydroxyethyl cellulose. 2. The composition according to item 1 above, which contains 0.2 to 2.0% by weight of hydroxyethylcellulose based on the total amount of the composition.