JPS60130511A - Production of toothpaste - Google Patents

Abstract

PURPOSE:To prevent aggregation and precipitation of a water-soluble salt of chlorhexidine in a production process of dentifrice and incorporate stably and uniformly the water-soluble salt in a toothpaste, by incorporating an aqueous solution of the water-soluble salt of the chlorhexidine in a kneading water containing a binder and a thickener as a base. CONSTITUTION:A water-soluble salt of chlorhexidine, e.g. chlorhexidine gluconate, as an active constituent for preventing dental caries is incorporated in toothpaste. In the process, an aqueous solution containing <=10wt%, preferably 0.1-5wt% above-mentioned active constituent is incorporated in a kneading water containing a binder and thickener to react the above-mentioned active constituent with other components in the production process of the dentifrice, etc. Thus, the aggregation and precipitation of the active constituent is prevented, and the above-mentioned active constituent is incorporated stably and uniformly in the toothpaste to exhibit fully the effect thereof.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing dentition containing a water-soluble salt of chlorhexidine, and in particular, the water-soluble salt of chlorhexidine is stably and uniformly blended by preventing aggregation and precipitation during the toothpaste production process. The present invention relates to a method for manufacturing toothpaste that can be used in various ways.

Traditionally, chlorhexidines have been added to oral compositions such as toothpastes as active ingredients for caries prevention, etc., but chlorhexidines, especially chlorhexidine water-soluble salts, are mixed with other ingredients during the manufacturing process. Aggregation and precipitation are likely to occur due to reactions.

Chlorhexidine exerts its action when it comes into contact with bacteria, so if chlorhexidine does not become solubilized and aggregates or precipitates, it may come into sufficient contact with bacteria. A problem arises in that the effects of chlorhexidine against bacteria are not sufficiently exerted.

In view of this, it is desired to stably incorporate a water-soluble salt of chlorhexidine into tooth brushing.

Conventionally, as a method for stably incorporating a water-soluble salt of chlorhexidine into a toothpaste, a method has been proposed in which sodium carboxymethylcellulose is swollen and dissolved in a thickening agent in a non-aqueous system, and then a water-soluble chlorhexinone salt or its aqueous solution is added. However, the stabilizing effect of the water-soluble salt of chlorhexidine is not necessarily sufficient.

Conventionally, when manufacturing toothpaste, a binder is dispersed and swollen in a thickening agent, and an aqueous Sankarin solution is added to prepare a clarified water.
A method of kneading fragrances, active ingredients, etc. is widely adopted, and as described above, a two-step process of preparing a water concentrate and a kneading process is used in general toothpaste production. In this case, the active ingredients in each other.

When producing multiple types of toothpaste with different flavorings and other mixing ingredients, since the mixing water is common to each other, the desired active ingredients and mixing ingredients such as fragrances are added to the mixing water. It is possible to produce a plurality of types of toothpaste having different compositions, and since there is no need to prepare different hydrophobicity for each toothpaste, the process for preparing the water paste is simplified.

However, the method disclosed in Japanese Patent Publication No. 58-17166 mentioned above involves adding a water-soluble salt of chlorhexidine to a binder and a thickening agent to make it hydrophobic, so other toothpastes that do not contain a water-soluble salt of chlorhexidine cannot be When manufacturing, it is necessary to prepare water for mixing separately.
When the method of Publication No. 6 is adopted, toothpaste containing chlorhexidine water-soluble salt must be manufactured on a line separate from the general toothpaste manufacturing process.

The present inventors have conducted extensive research into a method for producing wire toothpaste containing lorhexidine water-soluble groups, which can stably incorporate water-soluble salts of chlorhexinone and can be incorporated into the normal toothpaste manufacturing process.
After adding water to a mixture of a binder and a thickener such as IJum, if water-soluble salt of chlorhexidine is mixed, flocculation and precipitation will occur. It has been found that when a chlorhexidine salt aqueous solution having a concentration of 10% by weight or less (weight %, the same applies hereinafter) or less is mixed with a hydrophobic substance, the chlorhexidine water-soluble salt is stably and uniformly blended, and the present invention This is what we have come to do.

According to the present invention, while all conventionally known methods for stabilizing water-soluble salts of chlorhexidine involve mixing a water-soluble salt of chlorhexidine in a mixture with a caking agent and a thickening agent, the present invention By mixing an aqueous chlorhexicine salt solution with a concentration of 10% or less of chlorhexidine water-soluble salt in water prepared with a paste and a thickening agent, the chlorhexidine water-soluble salt can be prevented from coagulating and precipitating during the toothpaste manufacturing process. Since the water-soluble salt of chlorhexidine is added to the water in this way, when producing other toothpastes that do not contain the water-soluble salt of chlorhexidine, the hydrophobic composition of are common, therefore, multiple types of toothpaste can be manufactured using the same refining water, and the method of the present invention can be easily incorporated into the general toothpaste manufacturing process.

The present invention will be explained in more detail below.

The method for producing a toothpaste containing a chlorhexidine water-soluble salt according to the present invention includes mixing a chlorhexidine salt aqueous solution containing a chlorhexidine water-soluble salt at a concentration of 10% or less into a paste containing a binder and a thickening agent. This is a characteristic feature.

In the method of the present invention, as described above, a paste is first prepared using a binder and a thickening agent. Cellulose derivatives such as ethylcellulose, sodium calgoxymethylhydroxyethylcellulose, alkali metal alginates such as sodium alginate, zolobylene glycol alginate, xanthan gum.

Gums such as gum tragacanth, gum karaya, and gum arabic, synthetic binders such as I-rivinyl alcohol, sodium polyacrylate, cal-xyvinyl pol-I-J mer, and yje-livinyl pyrrolidone, gluformable silica, and dullable aluminum silica. , Begum.

One or more inorganic binders such as laponite are usually used in an amount of 0.5 to 10% of the total toothpaste.

In addition, sorbitol and glycerin are used as thickeners.

Ethylene glycol, propylene glycol, 1゜3-
One or more of butylene glycol, polyethylene glycol, polypropylene glycol, xylit, maltit, lactit, etc. usually accounts for 10 to 70% of the total toothpaste.
is used.

In the present invention, when preparing water, the binding agent is added to the thickening agent, the binding agent is dispersed and swollen in the thickening agent, and water is added to this, or the binding agent is gradually added to the water. In addition to this, a method of dispersing and swelling a binder in water and adding a thickening agent thereto is preferably adopted. The water used here is pre-added with saccharin sodium.

Stevioside, neohesberidyl dihydrochalcone,
One or more sweeteners such as glycyrrhizin, perillartin, thaumatin, asparatylphenylalanine methyl ester, p-methoxycinnamic aldehyde, sucrose, lactose, fructose, and saccharin sodium are usually added in an amount of 0.01 to 0.5 of the total amount. However, when saccharin sodium is used as a sweetener, direct mixing of saccharin sodium and chlorhexidine water-soluble salt will form an insoluble salt, so saccharin sodium should be dissolved in advance in the water used for hydrophobic adjustment. It is preferable to use this saccharin sodium aqueous solution, and when the saccharin sodium is previously included in the refining water, no precipitation occurs even if the chlorhexinone aqueous solution is subsequently added thereto. Furthermore, sodium monofluorophosphate is used for water preparation.

Other water-soluble active ingredients can also be dissolved. Here, the amount of water used for hydrophobic preparation is preferably such that the binder is contained in the mixing water in an amount of 5 to 20, particularly 1 to 5.

In the present invention, a water-soluble salt of chlorhexidine is added to the above-mentioned mixing water at a concentration of 10% or less, preferably 0.1 to 5%, thereby stabilizing the water-soluble salt of dichlorhexidine. Moreover, the toothpaste is uniformly dispersed and blended, and a toothpaste with a good toothpaste texture and an excellent appearance can be obtained. On the other hand, if the concentration of the chlorhexidine salt aqueous solution is more than 10 or more, the water-soluble salt of chlorhexinone will coagulate and precipitate during the manufacture of the toothpaste, and the texture of the toothpaste will deteriorate, making it impossible to achieve the object of the present invention.

Here, as the water-soluble salt of chlorhexidine, chlorhexidine gluconate or the like is used. The amount of chlorhexidine water-soluble salt in the total toothpaste is 0.0005 to 1.
H, more preferably 0.001 to 0.1%.

In the present invention, commonly used components such as abrasives, surfactants, fragrances, etc. are added to the water for mixing. In this case, these components may be added at the same time as the aqueous chlorhexidine salt solution, but it is preferable to add them before or after adding the aqueous chlorhexidine salt solution.

Here, the abrasives include dibasic calcium phosphate dihydrate and anhydride, dibasic calcium phosphate, dicalcium phosphate, calcium carbonate, calcium birophosphate, titanium oxide, alumina, water-containing alumina, precipitated silica, and other silica. system abrasive.

Aluminum silicate, insoluble sodium metaphosphate,
Insoluble potassium metaphosphate, tertiary magnesium phosphate,
Magnesium carbonate, calcium sulfate.

One or more of methyl methacrylate, bentonite, zirconium silicate, synthetic resin, etc. may be blended (
The blending amount is usually 5% to 75% of the total amount).

In addition, as surfactants, sodium lauryl sulfate,
The number of carbon atoms in the alkyl group, such as sodium myristyl sulfate, is 8.
Water-soluble salts of higher alkyl sulfates of ~18, water-soluble higher fatty acid monoglyceride monosulfates such as hydrogenated coconut oil fatty acid monoglyceride sodium monosulfate, alkylaryl sulfonates such as sodium dodecylbenzenesulfonate, higher alkyl sulfones. acid salt, 1.2-
Substances of lower aliphatic aminocarboxylic acid compounds such as higher fatty acid esters of dihydroxyzolo/f sulfonates, sodium, potassium or ethanolamine salts of N-ra r)loyl, N-myristoyl or N-noglumitoyl sarcosine anionic surfactants such as saturated higher aliphatic acylamides, sucrose fatty acid esters in which the fatty acid group has 12 to 18 carbon atoms such as sucrose mono- and dilaurate, lactose fatty acid esters, lactitol fatty acid esters, maltitol fatty acid esters, Stearic acid monoglyceride, preoxyethylene sorbitan monolaurate, polyoxyethylene rubitan monostearate,
Polyoxyethylene (10,20.

40.60.80,100 mol) Hydrogenated castor oil, polymers of ethylene oxide and propylene oxide, and condensation of polyethylene oxide such as polyoxyethylene polyoxypropylene monolauryl ester with fatty acids, fatty alcohols, polyhydric alcohols, and polyethylene oxide. Two or more kinds of nonionic surfactants such as nonionic surfactants, amphoteric surfactants such as betaine type, amino acid type, etc. (compounding amount usually θ to 7%, preferably 0.5 to 5%) may be blended.

In addition, fragrances include wintergreen oil, spearmint oil, varmint oil, satsafras oil, clove oil,
Eucalyptus oil or the like may be added.

In the present invention, if necessary, p-hydroxymethylpenzoic acid, p-hydroxybutylbenzoic acid, p-hydroxy 7'' lobil benzoic acid, p-hydroxybutylbenzoic acid,
Preservatives such as thorium benzoate and lower fatty acid monoglycerides, gelatin, ibutone, arginine hydrochloride, albumin, casein, brighteners, silicones, pigments, and other ingredients may be blended.

Furthermore, active ingredients other than chlorhexidine water-soluble salt,
For example, enzymes such as allantoin, epsilon aminocaproic acid, tranexamic acid, dextranase, amylase, protease, mutanase, lysozyme, lytic enzyme, Lytec enzyme, alkali metal monofluorocarbons such as sodium monofluorophosphate, potassium monofluorophosphate, etc. phosphate, sodium fluoride, ammonium fluoride, fluorides such as stannous fluoride, dihydrocholesterol, glycyrrhetinic salts, clycyrrhetinic acid,
Glycerophosphate, chlorophyll, caloisitide, water-soluble inorganic phosphoric acid compound, vitamins, anti-tartar agent,
One or more active ingredients such as antibacterial agents and plaque inhibitors may be combined.

In this case, these components may be mixed in advance in the training water, or may be added at the same time or before or after adding the above components, and furthermore, water-soluble salts that do not react with the water-soluble salt of chlorhexidine may be added. If it is chlorhexidine, it can be dissolved in a water-soluble salt of chlorhexidine in advance and added to the kneading water.

By mixing an aqueous chlorhexidine salt solution containing the concentration below, the water-soluble salt of chlorhexinone does not aggregate or precipitate during the manufacturing process, and is stably and uniformly dispersed in the toothpaste. It is also in good condition and has an excellent appearance. Further, according to the present invention, since the composition of the water refining is common to that used in manufacturing other toothpastes, the method of the present invention can be incorporated into the general toothpaste manufacturing process. Figure 1 shows this, with propylene glycol and carboxymethyl cellulose (IJ'7)
When preparing A toothpaste containing chlorhexidine gluconate by mixing a mixture of sorbitol, sorbitol, and saccharin with gluconizable silica and water to prepare a hydrophobic powder, use the hydrophobic solution containing chlorhexidine gluconate. Add
Furthermore, dibasic calcium phosphate dihydrate, fragrance, and surfactant are added and kneaded.In addition, when manufacturing B toothpaste, an aqueous solution of sodium monofluorophosphate is added to the same hydrophobic solution, and then aluminum hydroxide is added. , fragrance, and surfactant are added and kneaded, and when manufacturing C toothpaste, calcium carbonate, fragrance, and surfactant are added and kneaded to the same water. Therefore, according to the present invention, when producing a plurality of types of toothpaste, including a toothpaste containing a chlorhexidine water-soluble salt, only one water refining process is required, and the toothpaste manufacturing equipment can be simplified.

Next, the present invention will be explained in more detail by showing Examples and Comparative Examples.

[Example 1, Comparative Example] The following formulation Propylene glycol 2 Sodium thicarboxymethylcellulose 160% sorbitol solution 30 Sodium saccharin 0.1 Glycatable silica 2 Calcium phosphate dihydrate 45 Sodium lauryl sulfate 1.8 Flavor A toothpaste composition containing 0.8% chlorhexidine gluconate and 0.5% was prepared by the following method.

First, sodium carboxymethylcellulose is added to propylene glycol and dispersed, then a 60% sorbitol solution is added, and then a solution of sodium saccharin in a predetermined amount of water and silica are added and dispersed. To this, chlorhexinone gluconate aqueous solutions of various concentrations shown in Table 1 prepared by dissolving chlorhexinone gluconate in the remaining water were added, and further dibasic calcium phosphate dihydrate and lauryl sulfate were added. Sodium and fragrance were added to obtain a dentifrice composition. This dentifrice composition was filled into an ordinary aluminum cube, and the skin condition was sensory evaluated based on the following evaluation criteria. The results are also shown in Table 1.

Evaluation criteria ×: Appears to have a rough appearance.

△: -It has a slightly rough appearance, but there is no problem as a product.

○: Good.

Table 1 As is clear from the results in Table 1, by employing the method of the present invention, chlorhexyl gluconate does not precipitate during the manufacturing process, and toothpaste with a good appearance can be obtained. Admitted.

[Example 2] Using an aqueous solution of chlorhexidine gluconate having a concentration of 7, a toothpaste with the same formulation was produced in the same manner as in Example 1,
Adjust the content of chlorhexidine gluconate in toothpaste cheap.

In this case, the content of chlorhexidine gluco/acid is determined by the amount of toothpaste present in the root part a, the middle part, and the local part cX of the toothpaste tube 1 shown in Figure 2 (2 in the figure is the gap). The amount of chlorhexidine gluconate was determined for these samples. The results are shown in the table below. The results are expressed as the chlorhexidine gluconate content (ie, effective amount) relative to the chlorhexidine gluconate content (0.5% of the total toothpaste).

From the above results, the effective amount of chlorhexidine gluconate/acid is very high. Therefore, there is no aggregation or precipitation of chlorhexidine gluconate in one shuttle, and chlorhexidine gluconate/acid is present in the entire toothpaste. It is found that it is evenly mixed and contained.

[Brief explanation of the drawing]

Figure 1 is a diagram of the toothpaste manufacturing process. FIG. 2 is a plan view showing an example of a toothpaste cheese. Applicant: Lion Corporation Agent: Patent Attorney Takashi Kojima Figure 1

Claims (1)

[Claims] 1. Manufacture of a toothpaste characterized by mixing an aqueous solution of chlorhexidine salt containing a water-soluble salt of chlorhexidine at a concentration of 10% by weight or less with water paste containing a binder and a thickening agent. Method. 2. The manufacturing method according to claim 1, wherein the chlorhexinone salt is chlorhexidine gluconate.