JP5440150B2 - Oral composition - Google Patents

Description

  The present invention relates to an oral composition containing sodium fluoride and aluminum lactate, and the composition has a neutral pH range. More specifically, the present invention promotes high fluoride deposition on the tooth in the neutral pH range. The present invention relates to a composition for oral cavity that is effective and has excellent storage stability, and as a result, can be expected to have a high caries-preventing effect and is excellent in use feeling.

  It is widely known that caries can be prevented by using various fluoride-containing preparations such as dentifrices, mouthwashes, coating agents, and tablets. Among them, the most widely used at present are dentifrices and mouthwashes, including those in other countries. However, the caries preventive effect in these preparations is not always sufficient, and generally the caries inhibition rate is about 20 to 40% (especially about 20 to 30% for dentifrices). As one of the factors that do not necessarily have a sufficiently high caries prevention effect, fluoride is washed away from the oral cavity (tooth surface, plaque, mucous membrane, etc.) by brushing the mouth after using a dentifrice. It is considered that it is difficult to remain in the oral cavity. In addition, it is considered that after use of the mouthwash, the fluoride is washed away over time by saliva.

Therefore, in order to further improve the caries prevention effect when using oral compositions such as dentifrices and mouthwashes, the retention of fluoride in the oral cavity and the surface of the tooth surface after use can be improved. It is considered that improving the depositability of chemical compounds is an important issue. For that purpose, increasing the compounding concentration of fluoride in the preparation is one of the selection means. In fact, in Europe and the United States, the fluoride ion concentration (F ⁻ ) is 5,000 ppm (1.105 mass% with respect to the whole preparation). Dentifrice containing sodium fluoride is commercially available. However, increasing the concentration of fluoride in the formulation raises concerns about human safety (harmful effects due to overdose due to mottled teeth, etc.), and its application is significantly limited (for example, children) Can't be used or needs a prescription to get). Therefore, a technique for improving the effect derived from fluoride without increasing the fluoride concentration is desired.

  As an alternative to high-concentration fluoride, normal fluoride concentration (in Japan, dentifrice is about 500-1,000 ppm as fluoride ion concentration, mouthwash is 200-500 ppm) Within the range, there has been proposed a method for improving the effect derived from fluoride by using in combination with other components (pharmacologically acceptable and highly safe components).

  For example, using fluoride and water-soluble aluminum in combination, the technology to improve the effect of fluoride (improvement of dentin hypersensitivity, promotion of remineralization of demineralized tooth, etc.), and these components were blended as optional components Techniques have been proposed (Patent Documents 1 to 10).

  Patent Document 1 (Japanese Patent Laid-Open No. 5-155745) contains a water-soluble aluminum compound (aluminum salt of carboxylic acid such as aluminum lactate, aluminum chloride) and fluoride (sodium monofluorophosphate, sodium fluoride, etc.). The fluoride (F ion) concentration is 100 to 2,000 ppm, and the molar ratio of fluorine (F) and aluminum (Al) is 0.3 to 3 (0.046 to 9.28% by mass as aluminum lactate). Therefore, the composition ratio of sodium fluoride and aluminum lactate is equivalent to 1.779 to 17.79 in terms of mass%.), And the oral composition having a pH of 5 to 10 is effective in alleviating dentin hypersensitivity. It has the effect of promoting remineralization of dentin (preventive effect of root caries), and the astringent feeling of aluminum compound at this compounding molar ratio. Shokumi is suppressed (improved feeling) it is disclosed. In this Patent Document 1, the effect of suppressing the fluid permeability of the dentinal tubule (the narrowing of the entrance of the dentinal tubule) is exerted under the above-mentioned conditions, and the sensitivity of the dentinal sensation is alleviated, and recalcification on the dentin root surface It is said that it has the effect of preventing root caries by promoting oxidization.

  However, when the present inventors actually produced an oral composition using sodium fluoride, which is one of water-soluble fluorides, and aluminum lactate, which is one of water-soluble aluminum carboxylic acid salts, it is difficult to obtain a fluoric acid. Compared with sodium chloride alone, the use of aluminum lactate together increased the effect of promoting the deposition of fluoride on hydroxyapatite, but it was found that the preparation had a strong acidity and a need to improve the feeling of use. Therefore, the inventors further set the pH of the mixed solution of sodium fluoride and aluminum lactate (pH 3.8 to 5.6) to a neutral region (pH 6.0) using an alkaline substance (for example, sodium hydroxide). ~ 8.0), and when it was tried to improve the feeling of use, remarkable precipitation was observed after storage for several days at room temperature, and the concentration of dissolved aluminum and fluoride ions was decreased. A decrease in the effect of promoting fluoride deposition was also clearly observed. The same was observed for tin fluoride, sodium silicon fluoride, and ammonium fluoride. In addition, in the case of sodium monofluorophosphate, precipitation that adversely affects the effect was not observed, but even when used in combination with aluminum lactate, the improvement in the effect derived from fluoride was not as remarkable as sodium fluoride. .

JP-A-5-155745 JP-A-5-155746 JP-A-7-291844 JP 2000-178150 A JP 2002-302429 A JP 2003-73246 A Japanese Patent Laid-Open No. 2004-026816 JP 2007-84471 A JP-A-6-298632 JP-A-61-36212 Japanese Patent Laid-Open No. 10-17446 JP 2005-179230 A JP 2001-163743 A JP 2006-182658 A JP 2007-91712 A

  Therefore, when sodium fluoride and aluminum lactate are used in combination, and the pH is in the neutral range (pH 6.0 to 8.0), the above problems such as a decrease in the effect of promoting the deposition of fluoride on the tooth surface and precipitation over time In addition, even when sodium fluoride and aluminum lactate are used in combination and the pH is neutral (pH 6.0 to 8.0), the storage stability is high (precipitation is not observed over time), and It is an object of the present invention to develop an oral composition that effectively exhibits a high fluoride deposition promoting effect on the tooth surface and has an excellent usability.

  The present invention has been made in view of the above circumstances, and in an oral composition containing sodium fluoride and aluminum lactate and adjusting the pH of the composition to a neutral region (pH 6.0 to 8.0), High fluoride deposition promoting effect on quality, no precipitation even at neutral pH range, high storage stability over time, excellent use feeling, resulting in high caries prevention or suppression effect An object of the present invention is to provide an oral composition that can be expected.

  As a result of intensive studies to solve the above problems, the present inventors have found that when cationized cellulose is blended in a solution in which sodium fluoride and aluminum lactate are mixed in a specific blending amount and blending ratio, a pH neutral region (pH 6). 0.0 to 8.0), precipitation formation is remarkably suppressed, and no significant decrease in the effect of promoting fluoride deposition on the tooth surface is observed. Sodium fluoride and aluminum lactate are used in combination to adjust the pH to a neutral range ( It has been found that problems such as a decrease in the effect of promoting the deposition of fluoride on the tooth surface and precipitation over time in the oral composition adjusted to pH 6.0 to 8.0) can be solved, and the object of the present invention can be achieved. According to the present invention, sodium fluoride, aluminum lactate and cationized cellulose are appropriately used in combination in an oral composition containing sodium fluoride and aluminum lactate and having a pH of 6.0 to 8.0. As a result, a high fluoride deposition promoting effect on the tooth surface can be obtained, and an oral composition having excellent storage stability with time and excellent usability can be obtained.

  In addition, as a prior art which used fluoride and cationized cellulose together, the technique (patent document 11) which employ | adopted the cationized cellulose in order to improve the retention property of the bactericide in an oral cavity, and cationized cellulose as an arbitrary component are included. Although those described (Patent Documents 12 to 15) have been proposed, none of these techniques is a technique for improving the retention of fluoride, but sodium fluoride and aluminum lactate are blended to adjust the pH of the preparation. There are no problems such as the effect of promoting fluoride deposition and the decrease in storage stability when 6.0 to 8.0. From the description of these patent documents, the effect of promoting fluoride deposition and the improvement of storage stability and usability when sodium fluoride and aluminum lactate are included and the pH is adjusted to 6.0 to 8.0 cannot be predicted.

Accordingly, the present invention provides the following oral composition.
Claim 1:
(A) It is a composition for oral cavity containing sodium fluoride and (B) aluminum lactate, and pH of the composition is 6.0-8.0, and (A) sodium fluoride is 0.02- 0.5% by mass, (B) 0.05 to 1.0% by mass of aluminum lactate, and (C) 0.008 to 0.5% by mass of cationized cellulose, and (B) component / (A ) Component mass ratio is 0.3 to 10, and (C) component / [(A) component + (B) component] mass ratio is 0.08 to 0.8. .
Claim 2:
(C) The cationized cellulose is at least one cation-modified hydroxyethyl cellulose selected from O- [2-hydroxy-3- (trimethylammonio) propyl] hydroxyethylcellulose and hydroxyethylcellulose dimethyldiallylammonium chloride. The composition for oral cavity of description.
Claim 3:
The composition for oral cavity of Claim 1 or 2 prepared as a mouthwash.
Claim 4:
The composition for oral cavity of Claim 1 or 2 prepared as a dentifrice.

  According to the present invention, in an oral composition in which sodium fluoride and aluminum lactate are used in combination, and the pH of the composition is adjusted to a neutral region (pH 6.0 to 8.0), high fluoride for tooth A composition for oral cavity that exhibits an effect of promoting deposition, does not generate precipitation even in a neutral pH range, has high storage stability over time, and has an excellent feeling of use, and is therefore effective in preventing or suppressing caries. Can provide things.

  Hereinafter, the present invention will be described in more detail. The composition for oral cavity of the present invention uses (A) sodium fluoride, (B) aluminum lactate, and (C) cationized cellulose in a specific amount and a mixing ratio. And pH is a neutral area | region, It is characterized by the above-mentioned.

(A) As sodium fluoride, what is necessary is just used for the composition for oral cavity normally, For example, commercially available things, such as a reagent special grade by Wako Pure Chemical Industries, Ltd., can be used.
The blending amount of (A) sodium fluoride is 0.02 to 0.5% by mass, preferably 0.05 to 0.3% by mass, based on the fluoride deposition promoting effect. . When the blending amount of sodium fluoride is less than 0.02% by mass, a sufficient fluoride deposition promoting effect cannot be obtained, and when it exceeds 0.5% by mass, the fluoride deposition promoting effect cannot be obtained.

(B) Aluminum lactate can use what is normally used for a composition for oral cavity, for example, aluminum lactate (product number: 018-13275) by Wako Pure Chemical Industries, Ltd., industry by Showa Kako Co., Ltd. Commercially available products can be used.
The blending amount of (B) aluminum lactate is 0.05 to 1.0% by mass, preferably 0.1 to 0.5% by mass, based on the fluoride deposition promoting effect and storage stability. %. If the blending amount is less than 0.05% by mass, a sufficient fluoride deposition promoting effect cannot be obtained, and if it exceeds 1.0% by mass, precipitation occurs and the storage stability is poor.

  (A) The blending ratio [(B) / (A)] of (B) aluminum lactate to sodium fluoride is within the range of 0.3 to 10 in terms of mass ratio in terms of the effect of promoting the deposition amount of fluoride. , Preferably 1-5. If the blending ratio is less than 0.3 or exceeds 10, the effect of promoting fluoride deposition is not satisfactorily exhibited.

  (C) As the cationized cellulose, cation-modified hydroxyethylcellulose such as O- [2-hydroxy-3- (trimethylammonio) propyl] hydroxyethylcellulose, hydroxyethylcellulose dimethyldiallylammonium chloride is suitably used. A cationized cellulose can be mix | blended individually by 1 type chosen from these or in combination of 2 or more types.

  Specifically, as the cationized cellulose of component (C), commercially available Cellcoat H-100 which is hydroxyethyl cellulose dimethyl diallylammonium chloride (nitrogen content: 1.0 mass%, 2 mass% aqueous solution viscosity: 500-2,750 mPa S (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), Cellcoat L-200 (nitrogen content: 2.0 mass%, 2 mass% aqueous solution viscosity: 35- 350 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), which can be obtained as a product of NSC Japan (the difference in grade is the molecular weight of cellulose, Ethylene oxide (EO) average added mole number, degree of cationization, etc.).

  Further, Leogard G (nitrogen content: 1.8% by mass, 2% by mass aqueous solution viscosity: 100 to 600 mPa · s (BH type), which is O- [2-hydroxy-3- (trimethylammonio) propyl] hydroxyethylcellulose chloride Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)) Leoguard GP (nitrogen content: 1.8 mass%, 2 mass% aqueous solution viscosity: 100 to 600 mPa · s (BH type Brookfield) Viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), Leoguard MGP (nitrogen content: 1.8% by mass, 1% by mass aqueous solution viscosity: 500 to 1,200 mPa · s (BH type Brook) Field viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), Leoguard MLP (nitrogen content: 0.6 mass%, 1 mass% water) Liquid viscosity: 1,000-2,600 mPa · s (BH Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), Leoguard LP (nitrogen content 1.0% by mass, 2 Mass% aqueous solution viscosity: 300 to 800 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), Leoguard KGP (nitrogen content 1.8% by mass, 2% by mass) Aqueous solution viscosity: 5 to 50 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)), etc. The difference depends on the molecular weight of cellulose, the average added mole number of EO and the degree of cationization).

  (C) The amount of the cationized cellulose is 0.008 to 0.5% by mass, preferably 0.03 to 0.2% by mass, based on the whole composition, in terms of storage stability and usability. . When the blending amount is less than 0.008% by mass, precipitation occurs during storage and the storage stability is inferior. When it exceeds 0.5% by mass, it is stable immediately afterwards, but there is a problem in temporal stability, and the oral mucosa Feels uncomfortable (feeling irritated, feeling numb, etc.) and inferior to the feeling of use.

  In the present invention, the blending ratio of (C) cationized cellulose to (A) sodium fluoride and (B) aluminum lactate, that is, the mass ratio of (C) / [(A) + (B)] is storage stability. Or 0.08 to 0.8, preferably 0.10 to 0.50 in terms of the effect of promoting the deposition of fluoride. If the blending ratio is less than 0.08, precipitation occurs over time and the storage stability is poor, and if it exceeds 0.8, the effect of promoting the deposition of fluoride is not sufficiently improved. Although the details are not clear, the relative ratio of cationized cellulose to the concentration of colloid composed of aluminum ions and fluoride ions is related to the inference of the effect and stability mechanism described later. This is considered to be due to the fact that it is too high, strongly stabilized, and the colloidal deposition on the apatite surface is inhibited.

  The composition of the present invention has a pH at 25 ° C. of 6.0 to 8.0, preferably 6.0 to 7.0, in terms of usability and storage stability. If the pH is less than 6.0, sourness is generated and the feeling of use is inferior. If the pH exceeds 8.0, the formation of precipitates becomes remarkable even when sodium fluoride and aluminum lactate are used in combination with cationized cellulose. Inferior.

The pH can be adjusted with sodium hydroxide or potassium hydroxide.
The pH was measured by using a pH electrode (manufactured by Toa DKK, HM-30R type) and three standard solutions (pH 4.01 phthalate buffer, pH 6.86: phosphate buffer, 9.18: borate buffer). , Both were calibrated with Wako Pure Chemical Industries, Ltd. standard solution), then the electrode was brought into contact with the sample (solution or dentifrice), and the displayed value after 3 minutes was read (room temperature (15-30 ° C.)) Measured in).

  The mechanism for improving the effect of promoting fluoride deposition according to the present invention is not clear at present, but is presumed as follows. That is, the effect of promoting the fluoride deposition is improved because some electrostatic interaction occurs between aluminum lactate and sodium fluoride, which is a water-soluble fluoride, to form a colloidal complex. This is presumably because it became easy to deposit on the tooth surface via van der Fahls force. Further, the size of the colloid is closely related to the blending concentration of both components and the molar ratio thereof. If the colloid is too small, the effect of promoting the deposition of fluoride is low. It is presumed that the colloidal particles are easily detached by the shearing force at the time, and the effect of promoting the deposition of fluoride is not improved.

  Furthermore, in the present invention, the action mechanism of cationized cellulose is not clear but is estimated as follows. In other words, the positively charged site in the cationized cellulose molecule interacts electrostatically with the negatively charged site in the colloid described above, acting so that the colloidal particles do not become too large. It is presumed that This is consistent with the fact that sodium carboxymethyl cellulose and nonionic hydroxyethyl cellulose, which are anionic polymers, did not have a stabilizing effect.

The composition for oral cavity of the present invention is prepared in various dosage forms such as toothpaste, toothpaste such as toothpaste and liquid toothpaste, mouthwash, gel and the like, and may be in the form of liquid, liquid, paste, gel, etc. However, it is particularly suitable as a dentifrice or mouthwash, and a liquid preparation is more preferred. Here, when preparing into various dosage forms, for example, in addition to the above components (A) to (C), other known components, and further water, depending on the dosage form and the like, a range that does not impair the effects of the present invention. And can be prepared by a usual method. For example, in the case of a dentifrice such as toothpaste, abrasives, thickeners, binders, surfactants, sweeteners, fragrances, coloring agents, preservatives, active ingredients and medicinal ingredients can be blended. In the case of a mouthwash, for example, wetting agents, surfactants, alcohols, solvents, organic acids, preservatives, bactericides, fragrances, sweeteners, colorants, active ingredients and medicinal ingredients can be blended. Furthermore, you may mix | blend an abrasive | polishing agent and a binder with liquid formulations, such as a mouthwash, as needed.
The following are mentioned as an arbitrary component, 1 type can be used individually or in combination of 2 or more types as appropriate.

Examples of the abrasive include silica-based abrasives such as silicic anhydride, precipitated silica, silica gel, aluminosilicate, zirconosilicate, dicalcium phosphate dihydrate and anhydrous, calcium pyrophosphate, calcium carbonate, aluminum hydroxide. Alumina, magnesium carbonate, tribasic magnesium phosphate, zeolite, zirconium silicate, synthetic resin-based abrasive and the like are preferably used. In addition, since this invention composition contains a fluoride, especially a silica type abrasive | polishing agent is preferable as an abrasive | polishing agent.
In the case of dentifrice, the compounding amount of these abrasives is preferably 2 to 50% by mass, particularly 10 to 30% by mass, based on the whole composition. When mix | blending with a liquid formulation, 0-5 mass% is good.

  Examples of the surfactant include water-soluble salts of higher alkyl sulfates having 8 to 18 carbon atoms in the alkyl group such as sodium lauryl sulfate and sodium myristyl sulfate, fatty acid groups such as sodium lauryl monoglyceride sulfonate and sodium coconut monoglyceride sulfonate. A fatty acid group such as a water-soluble salt of higher fatty acid monoglyceride sulfonic acid having 10 to 18 carbon atoms, olefin sulfonic acid, paraffin sulfonic acid and other anionic surfactants, stearyl monoglyceride, sucrose mono and dilaurate. -18 sucrose fatty acid ester, lactose fatty acid ester, lactitol fatty acid ester, maltitol fatty acid ester, stearic acid monoglyceride, polyoxyethylene sorbitan monolaurate Nonionic surfactants such as polyoxyethylene hydrogenated castor oil, sorbitan monostearate condensate added with about 60 mol of ethylene glycol, polymers of ethylene oxide and propylene oxide, derivatives such as polyoxyethylene polyoxypropylene monolauryl ester, Examples of the surfactant include amphoteric surfactants such as betaine type and amino acid type (blending amount: usually 0.5 to 5% by mass with respect to the whole composition).

  As binder, cellulose derivatives other than component (C) such as carrageenan, sodium carboxymethyl cellulose, methyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, sodium carboxymethyl hydroxyethyl cellulose, alkali metal alginates such as sodium alginate, propylene glycol alginate, xanthan gum , Gums such as gum tragacanth, karaya gum, gum arabic, and the like, and synthetic binders such as polyvinyl alcohol, sodium polyacrylate, carboxyvinyl polymer, polyvinylpyrrolidone, etc. (blending amount; 1-5 mass%).

  Examples of the wetting agent (thickening agent) include sugar alcohols such as glycerin, sorbitol, xylitol, maltitol, erythritol, lactitol, trehalose, mannitol, isomalt and the like. In particular, sorbitol, glycerin, xylitol, and erythritol are more preferable from the viewpoint of stable supply as a raw material. In addition, polyhydric alcohols such as ethylene glycol, propylene glycol, 1,3-butylene glycol, polyethylene glycol, and polypropylene glycol can be used as raw materials that help the swelling of the binder.

Examples of the sweetening agent include saccharin sodium, stepioside, neohesperidyl dihydrochalcone, glycyrrhizin, perilartin, thaumatin, aspartylphenylalanine methyl ester, p-methoxycinnamic aldehyde, sodium cyclamate and the like. Examples of preservatives include p-hydroxymethyl benzoic acid, p-hydroxyethyl benzoic acid, p-hydroxypropyl benzoic acid, p-hydroxybutyl benzoic acid, and the like, and benzoic acid such as sodium benzoate. Examples include salts and lower fatty acid monoglycerides. As a fragrance | flavor, winter green oil, spearmint oil, peppermint oil, sassafras oil, clove oil, eucalyptus oil, etc. may be mix | blended. Moreover, you may mix | blend a whitening agent, silicone, a pigment | dye, and other components.
As the colorant, Blue No. 1, Yellow No. 4, titanium dioxide and the like can be blended in usual amounts.

  Moreover, you may mix | blend an active ingredient or medicinal ingredient other than (A) sodium fluoride and (B) aluminum lactate, and it can also contain a various active ingredient as needed. For example, anti-inflammatory agents such as epsilon aminocaproic acid, tranexamic acid, glycyrrhetinic acid, enzymes such as dextranase, protease, mutanase, lysozyme, lytic enzyme, antibacterials such as chlorhexidine salts, cetylpyridinium chloride, isopropylmethylphenol, triclosan, etc. One or two or more active ingredients such as an agent, vitamins such as vitamin C and E, and a hypersensitive hyposensitivity agent such as potassium nitrate may be blended. In addition, the compounding quantity of an active ingredient or a medicinal ingredient can be made into an effective quantity in the range which does not inhibit the effect of this invention.

  EXAMPLES Hereinafter, although an Example, a comparative example, and a formulation example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples, “%” means “% by mass” unless otherwise specified.

[Examples and Comparative Examples]
Mouthwashes having the compositions shown in Tables 1 and 2 were prepared according to the treatment liquid preparation methods shown below and evaluated as follows. The results are shown in Tables 1 and 2.
<Preparation method of treatment liquid (mouth rinse liquid of Examples and Comparative Examples)>
First, an appropriate amount of aluminum lactate was dissolved in distilled water, and then sodium fluoride was added and stirred well until it became transparent. Further, a cationized cellulose aqueous solution diluted to 1 or 3% (Cell Coat L200: manufactured by Nippon SC Co., Ltd. (nitrogen content: 2.0%, 2% aqueous solution viscosity: 159 mPa · s (BH Brookfield viscometer, rotor No. 2 and 20 rotations, 21 ° C., measurement time 1 minute), and the mixture was stirred well, and then the pH was adjusted to a predetermined value with dilute sodium hydroxide aqueous solution. Adjusted to 0%.

<Effectiveness evaluation test (evaluation of fluoride deposition promoting effect on hydroxyapatite powder)>
As a substitute for tooth surface, hydroxyapatite powder with similar chemical properties (hydroxyapatite filler NR001C, average particle size: 80 to 150 μm, specific surface area: 500 cm ² / g, PENTAX Corporation, Tokyo) (hereinafter referred to as apatite) The experiment was conducted using abbreviated). The apatite (50 mg) was weighed into a 10 mL test tube, and the treatment liquid (Example) or the comparative treatment liquid (Comparative Example) (2 mL) was added to the test tube, followed by treatment for 10 minutes (at room temperature Lightly shake). Next, the treatment solution or the comparison treatment solution was discarded, and distilled water (5 mL) was added to the test tube to wash the apatite. This washing operation was repeated twice to remove the fluoride not deposited on the apatite with water. Thereafter, 1N hydrochloric acid (1 mL) is added to dissolve the apatite, then 1 mL of a buffer (TISAB (Total Ionic Strength Buffer), Thermo) is added, and distilled water is further added to make a total volume of 5 mL. The amount of fluoride deposited on the apatite was measured with an ion electrode (Thermo).

Judgment Criteria of Effects Regarding the caries prevention effect of fluorine, since the effect of using a mouthwash containing fluorinated sodium fluoride (226 ppm as F) is clinically recognized, Concentration is considered the lowest effective concentration. Therefore, the determination of the effect is that the fluoride deposition amount on the apatite is equal to or larger than the deposition amount (2.8 ng / 50 mg HA) obtained at this concentration (0.05% sodium fluoride), and the treatment solution or comparative treatment solution When the amount of deposition was 1.5 times or more higher than the amount of fluoride deposition measured in the same manner as described above in the composition of each example with sodium fluoride alone (no water-soluble aluminum compound and cellulose derivative) Judgment was made based on the following evaluation criteria.

Evaluation criteria for the effect of promoting fluoride deposition Comparison with sodium fluoride alone composition Evaluation 1.0 times or more and less than 1.5 times ×
1.5 times or more and less than 2.0 times ○
2.0 times or more ◎

<Evaluation of storage stability>
The mouthwash of each example prepared by the above preparation method was put in a transparent 100 mL plastic container, and the solution was sealed with a lid. The solution was observed on that day, and the presence or degree of precipitation or turbidity of the product immediately after preparation was observed and evaluated according to the following criteria. Subsequently, this was stored at room temperature for 4 weeks, and similarly, the presence or degree of precipitation or turbidity was observed and evaluated according to the following criteria.

Evaluation criteria for storage stability
Evaluation Transparent with no orientation or precipitation ◎
There is almost no sediment and no sediment, and very small suspended matter when shaken ○
Although it is recognized, it is a problem-free level and is transparent.
A lot of orientation and turbidity is recognized ×

<Evaluation of lack of mucosal discomfort (feeling irritated or numb) or acidity>
A panel of 5 people contained the mouthwash (5 mL) of each example prepared in the above preparation method in the mouth, washed in the usual manner for 30 seconds, and then felt on the oral mucosa such as lips, cheeks, and tongue. The discomfort and sourness were evaluated according to the following criteria.
3 points that do not feel uncomfortable or sour at all 2 points that feel somewhat uncomfortable or sour 2 points that feel uncomfortable or sour 1

Regarding the feeling of use, the total score of the evaluation of the sense of incongruity and acidity of the panel of five people was obtained, and judged according to the following criteria.
Usability criteria Criterion criteria Evaluation 12 points or more ◎
9 points or more and less than 12 points ○
5 points or more and less than 9 points ×

Details of the components used are as follows.
・ Sodium fluoride: Special grade reagent manufactured by Wako Pure Chemical Industries, Ltd. ・ Aluminum lactate: Special grade reagent made by Wako Pure Chemical Industries, Ltd. ・ Cationized cellulose (Cellcoat L200): Made by NSC Japan (nitrogen content: 2.0) %, 2% aqueous solution viscosity: 159 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute))
Aluminum tartrate: manufactured by Mitsuwa Chemicals Co., Ltd. (same molar concentration as aluminum lactate in Example 18)
Aluminum chloride hexahydrate: Reagent special grade manufactured by Wako Pure Chemical Industries, Ltd. (same molar concentration as aluminum lactate in Example 18)
・ Hydroxyethylcellulose (hydroxyethylcellulose): Wako Pure Chemical Industries, Ltd. Wako first grade ・ Carboxymethylcellulose sodium: Wako Pure Chemical Industries, Ltd.

<About the results of Tables 1 and 2>
In the present invention, by blending sodium fluoride, aluminum lactate and cationized cellulose in appropriate amounts and proportions, a high fluoride deposition promoting effect on the tooth surface can be obtained, and the storage stability and usability are also excellent. Was confirmed. On the other hand, when an aluminum compound other than aluminum lactate (aluminum tartrate as the carboxylate and aluminum chloride hexahydrate as the inorganic salt) was used, a high effect was not obtained. In the case of aluminum chloride, a large amount of precipitation was seen when the pH was adjusted to neutral (about 7.0). From this, it is surmised that the concentration of aluminum ions dissolved in water was considerably reduced. In the case of aluminum tartrate, it is presumed that the aluminum ion was chelated strongly and the effect was not expressed. In addition, when carboxymethylcellulose sodium salt or nonionic hydroxyethylcellulose which is the anionic polymer having the same cellulose skeleton of cationized cellulose is used, a stabilizing effect like cationized cellulose cannot be obtained and is high. The effect was not obtained.

The dentifrices and mouth washes of the following formulation examples 1 to 8 were prepared by conventional methods and evaluated in the same manner. All of these preparations were excellent in the effect of promoting fluoride deposition, stability, and feeling of use, and were excellent in these effects even after being stored at room temperature for 1 month. The details of the components used were as follows, and the other components were the same as described above.
(C) Cationized cellulose Leogard G: Nitrogen content: 1.8%, 2% aqueous solution viscosity: 330 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)
Leogard MGP: Nitrogen content: 1.8%, 1% aqueous solution viscosity: 782 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)
Cell coat H100: Nitrogen content: 1.0%, 2% aqueous solution viscosity: 1515 mPa · s (BH type Brookfield viscometer, rotor No. 2, 20 revolutions, 21 ° C., measurement time 1 minute)

[Prescription Example 1] Toothpaste (pH 6.0)
(A) Sodium fluoride 0.1%
(B) Aluminum lactate 0.15
(C) Leo Guard G 0.2
70% sorbite solution 30
Propylene glycol 1.0
Silicic anhydride 20
Saccharin sodium 0.02
Sodium lauryl sulfate 1.0
Sodium benzoate 0.1
Methylparaben 0.05
Sodium carboxymethylcellulose 1.2
Potassium nitrate 5.0
Triclosan 0.3
1N aqueous sodium hydroxide solution 0.01
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 1.5 (C) / ((A) + (B)) = 0.800)

[Prescription Example 2] Toothpaste (pH 8.0)
(A) Sodium fluoride 0.1%
(B) Aluminum lactate 0.2
(C) Leoguard MGP 0.1
(C) Cell coat L200 0.1
70% sorbite solution 30
85% glycerin solution 5
Xylitol 10
Propylene glycol 1.0
Silicic anhydride 20
Saccharin sodium 0.02
Sodium lauryl sulfate 1.0
Sodium benzoate 0.1
Methylparaben 0.05
Sodium carboxymethylcellulose 1.2
Potassium nitrate 5.0
Triclosan 0.3
1N aqueous sodium hydroxide solution 0.1
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 2.0 (C) / ((A) + (B)) = 0.667)

[Prescription Example 3] Toothpaste (pH 7.5)
(A) Sodium fluoride 0.1%
(B) Aluminum lactate 0.3
(C) Cell coat L200 0.05
(C) Cell coat H100 0.05
70% sorbite solution 30
85% glycerin solution 5
Propylene glycol 1.0
Silicic anhydride 20
Saccharin sodium 0.02
Sodium lauryl sulfate 1.0
Sodium benzoate 0.1
Methylparaben 0.05
Sodium carboxymethylcellulose 1.2
Potassium nitrate 2.0
Triclosan 0.3
1N aqueous sodium hydroxide solution 0.08
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 3.0 (C) / ((A) + (B)) = 0.25)

[Prescription Example 4] Toothpaste (pH 7.0)
(A) Sodium fluoride 0.2%
(B) Aluminum lactate 0.1
(C) Cell coat H100 0.1
70% sorbit solution 25
85% glycerin solution 5
Xylitol 5
Propylene glycol 1.0
Saccharin sodium 0.02
Sodium lauryl sulfate 1.0
Sodium benzoate 0.1
Methylparaben 0.05
Carrageenan 1.2
Potassium nitrate 5.0
Triclosan 0.3
1N aqueous sodium hydroxide solution 0.05
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 0. 5 (C) / ((A) + (B)) = 0.333)

[Prescription Example 5] Toothpaste (pH 7.0)
(A) Sodium fluoride 0.2%
(B) Aluminum lactate 0.3
(C) Leo Guard G 0.05
(C) Cell coat H100 0.1
70% sorbit solution 45
Propylene glycol 2.0
Saccharin sodium 0.02
Sodium lauryl sulfate 1.0
Sodium benzoate 0.1
Methylparaben 0.05
Sodium carboxymethylcellulose 0.8
Carrageenan 0.8
Potassium nitrate 5.0
Triclosan 0.3
1N aqueous sodium hydroxide solution 0.05
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 1.5 (C) / ((A) + (B)) = 0.3)

[Prescription Example 6] Toothpaste (pH 6.8)
(A) Sodium fluoride 0.2%
(B) Aluminum lactate 0.2
(C) Cell coat L200 0.2
70% sorbite solution 20
85% glycerin solution 10
Propylene glycol 1.0
Saccharin sodium 0.02
Sodium lauryl sulfate 1.0
Sodium benzoate 0.1
Methylparaben 0.05
Sodium carboxymethylcellulose 0.6
Carrageenan 1.2
1N aqueous sodium hydroxide solution 0.03
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 1.0 (C) / ((A) + (B)) = 0.5)

[Prescription Example 7] Mouthwash (pH 7.0)
(A) Sodium fluoride 0.02%
(B) Aluminum lactate 0.1
(C) Cell coat L200 0.01
70% sorbite solution 2.0
Xylitol 0.5
Saccharin sodium 0.02
Sodium lauryl sulfate 0.1
Sodium benzoate 0.1
Ethanol 1.0
Triclosan 0.1
1N aqueous sodium hydroxide solution 0.05
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 5.0 (C) / ((A) + (B)) = 0.083)

[Prescription Example 8] Mouthwash (pH 6.0)
(A) Sodium fluoride 0.1%
(B) Aluminum lactate 0.2
(C) Cell coat H100 0.1
70% sorbite solution 1.0
Xylitol 5.0
Saccharin sodium 0.02
Sodium lauryl sulfate 0.1
Sodium benzoate 0.1
Ethanol 2.0
Triclosan 0.1
Potassium nitrate 3.0
1N aqueous sodium hydroxide solution 0.01
Fragrance 0.1
Purified water balance <100.0% total
((B) / (A) = 2.0 (C) / ((A) + (B)) = 0.333)

Claims (4)

  (A) It is a composition for oral cavity containing sodium fluoride and (B) aluminum lactate, and pH of the composition is 6.0-8.0, and (A) sodium fluoride is 0.02- 0.5% by mass, (B) 0.05 to 1.0% by mass of aluminum lactate, and (C) 0.008 to 0.5% by mass of cationized cellulose, and (B) component / (A ) Component mass ratio is 0.3 to 10, and (C) component / [(A) component + (B) component] mass ratio is 0.08 to 0.8. .   (C) The cationized cellulose is at least one cation-modified hydroxyethyl cellulose selected from O- [2-hydroxy-3- (trimethylammonio) propyl] hydroxyethylcellulose and hydroxyethylcellulose dimethyldiallylammonium chloride. The composition for oral cavity of description.   The composition for oral cavity of Claim 1 or 2 prepared as a mouthwash.   The composition for oral cavity of Claim 1 or 2 prepared as a dentifrice.