JPS60146814A - Tooth paste composition - Google Patents

Abstract

PURPOSE:A tooth paste composition that contains sodium chloride and/or potassium chloride to stabilize p-hydroxybenzoic alkyl ester as an antiseptic, thus containing alkaline abrasive of increased preservability. CONSTITUTION:The objective tooth paste is prepared by adding methyl or ethyl p-hydroxybenzoate as an antiseptic (preferably 0.01-0.5wt%) and sodium chloride and/or potassium chloride as a stabilizer to a tooth paste compositioncontaining an abrasive whose 10wt% aqueous suspension shows a pH of 8-11 such as calcium carbonate, calcium tertiary phosphate, aluminum hydroxide, magnesium carbonate or magnesium tertiary phosphate in an amount 1-30wt% based on the total amount. EFFECT:The paste can keep its antispetic power for a long period of time.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides methyl guraoxybenzoate and/or
The present invention also relates to an alkaline abrasive-containing dentifrice composition that stably contains ethyl laoxybenzoate and therefore has a high shelf life.

It is known that 9-hydroxybenzoic acid alkyl esters are used as preservatives in conventional polishing compositions.

In this case, the oxybenzoic acid alkyl esters are stably blended into the dentifrice composition, and even when the dentifrice composition is stored for a long period of time, it maintains its initial preservative effect and maintains its preservative effect. It is desirable to be able to avoid secondary contamination caused by low carbon dioxide emissions.

However, although a surfactant is usually blended into the 1m polishing composition, butyl ester among the Noyaraoki 7-benzoic acid alkyl esters is affected by the surfactant's 11P and its preservative effect is almost completely lost. Not done. On the other hand, methyl halaoxybenzoate and ethyl paraoxybenzoate are less affected by the effects of surfactants and exhibit high antiseptic effects.

In particular, methyl guraoxybenzoate exhibits an excellent antiseptic effect. Therefore, it is necessary to incorporate para-oxybenzoic acid alkyl esters as a preservative into a dentifrice composition, but in this case, the preservative is not affected by the interfacial T6 agent contained in the dentifrice composition. It is desirable to use iJl methyl paraoxybenzoate and ethyl paraoxybenzoate, which are effective.

However, according to the studies of the present inventors, among the various abrasives that are the main components of toothpaste compositions, those containing alkaline abrasives whose - of the 10-ridge water suspension is in the range of 8 to 11. The stability of the oil in the tooth a composition decreases, especially) 4
It was found that the stability of methyl hydroxybenzoyl is extremely poor.

For this reason, the present inventors have conducted extensive research on methods for making methyl oxybenzoate and ethyl p-oxybenzoate safe when these substances are added to toothpaste compositions containing alkaline abrasives as abrasives. As a result, by adding sodium J1 and/or potassium chloride, it was possible to stabilize 9-methyl oxybenzoate and 12-ethyl oxybenzoate even in systems containing alkaline abrasives. It has been found that even when stored for a long period of time, a decrease in stability is prevented as much as possible and its preservative effect is effectively exhibited, so that it is possible to obtain a dentifrice composition that maintains its preservative power over a long period of time. , which led to the present invention.

Hereinafter, the single output tllIt will be explained in more detail.

The dentifrice composition of the present invention contains an alkaline abrasive as an abrasive, and has methyl oxybenzoate and/or ethyl oxybenzoate as a preservative, and sodium chloride and/or chloride. It contains potassium and exhibits excellent preservative power over a long period of time.

In this case, the alkaline polishing agent is 10j! : 1% aqueous suspension with - in the range of 8 to 11, such as calcium carbonate, tertiary calcium phosphate, aluminum hydroxide, magnesium carbonate, tertiary magnesium phosphate, etc. One or more of these can be used.

The amount of these alkaline abrasives used in the toothpaste composition is generally 1 to 95 times a day, but especially in the case of calcium carbonate, tribasic calcium phosphate, and aluminum hydroxide, the amount is 1 to 95 times a day.
In the case of 95% by weight, preferably 5 to 60% by weight, and in the case of magnesium carbonate or tertiary magnesium phosphate, it is preferably 1 to 20% by weight, preferably 1 to 10% by weight.

In addition, the amount of methyl haloxybenzoate and/or ethyl oxybenzoate distributed is 0.01 to 0.0 based on the entire composition.
．． It is preferable to use 5-layer weight, especially 0.01 to 0.3 weight. If the blending amount is less than 0.01 J
If the dentifrice composition exceeds 100%, the feeling of use of the toothpaste composition may not be satisfactory.

According to the present invention, the preservative power is the same as that of the above when using methyl oxybenzoate or ethyl oxybenzoate in combination with sodium chloride or potassium chloride. It is possible to reduce the amount of methyl benzoate used (0.3 mm or less), and even when used in a small amount, it has good preservative power and provides a good feeling when used.

The present invention provides the above-mentioned alkaline polishing agent and... Laoki 7
This is a toothpaste composition containing methyl benzoate and/or ethyl benzoate, which contains methyl benzoate and/or potassium chloride. The stability in an alkaline abrasive group has been completely increased, and its preservative power can be exhibited for a long period of time.

In this case, the amount of sodium chloride and/or potassium chloride is 1 to 30 AJtt%, especially 5 to 3% of the total composition.
The content is preferably 0% by weight. If the blending amount is less than 1% by weight, the stabilizing power of methyl nocraoxybenzoate and ethyl /4'laoxybenzoate may not be sufficiently achieved, and if the amount is more than 1% by weight, the feeling of use Unfavorable situations may arise from this point of view.

The dentifrice composition of the present invention may further contain appropriate ingredients depending on its type and purpose of use.

For example, in addition to the alkaline abrasives mentioned above, other abrasives such as dibasic calcium phosphate dihydrate and anhydride, dibasic calcium phosphate, calcium pyrophosphate, alumina, hydrated alumina.

One or two of the following: precipitated 7-liquid, other silica-based abrasives, aluminum silicate, insoluble sodium metaphosphate, insoluble potassium metaphosphate, calcium sulfate, polymethyl methacrylate, bentonite, zolconium silicate, synthetic) H fat, etc. More than one species can be blended.

In addition, in the case of toothpaste, caradanan, sodium calgeximethylcellulose, methylcellulose, and hydroxyethylcellulose are used as binders.

Cellulose derivatives such as sodium carboxymethyl hydroxyethyl sululose, alkali metal alginates such as sodium alginate, propylene glycol alginate, gums such as xanthan gum, tragacanth gum, karaya gum, gum arabic, polyvinyl alcohol, polyacrylic acid Sodium, Cal? Synthetic binders such as xyvinyl polymer and polyvinylpyrrolidone, 5r silica, aluminum silica,
1 or 2 of inorganic binders such as begum and laponite
More than one species can be blended (the blending amount is usually 0.5 to 5%).

In addition, sorbitol, glycerin, ethylene glycol, and clopylene glycol are used as thickening agents.

1. One or more of 3-butylene glycol, polyethylene glycol, polypropylene glycol, xylit, malnut, lactit, etc. may be blended (the blending amount is usually 10 to 70%).

In addition, water-soluble salts of higher alkyl sulfates whose alkyl groups have carbon atoms of 8 to 18, such as sodium lauryl sulfate and sodium myristyl sulfate, and water-soluble higher fatty acid monoglyceride monoglycerides such as hydrogenated 7-oil fatty acid monoglyceride monosulfate, etc. sulfates, alkylaryl sulfo/acids such as sodium dodecylbenzenesulfonate, higher alkyl sulfonates, higher fatty acid esters of 1,2-dihydroxynolopanesulfonate, N-lafuroyl,
anionic activators such as substantially saturated higher aliphatic acylamides of lower aliphatic aminocarbonic acid compounds, such as the sodium, potassium or ethanolamine salts of N-myristoyl or N-norumitoyldercosine; Sugar fatty acid esters in which the fatty acid group has 12 to 18 carbon atoms such as sucrose mono- and dilaurate;
Lactose fatty acid ester, lactitol fatty acid ester, maltitol fatty acid ester, stearic acid monoglyceride, sorbitan fatty acid ester, I-lyoxyethylene sorbitan monolaurate, holoxyethylene sorbitan monostear V-), polyoxyethylene (1
0,20,40,60゜80.100 mol) Hydrogenated castor oil, polymers of ethylene oxide and clopylene oxide, and polyethylene oxide and fatty acids such as polyoxyethylene polyoxyzolopyrene monolauryl ester.

One or more types of surfactants such as nonionic surfactants such as fatty alcohols, polyhydric alcohols, and condensation products with polypropylene oxide, and amphoteric surfactants such as betaine type and amino acid type (compounding amount is usually 0 to 7 surfactants). , preferably 0.5 to 5 inches).

The present invention further includes sweeteners such as saccharin sodium, stevioside, neohess (lysyl dihydrochalcone, glycyrrhizin, perillartin, thaumatin, Asuno's tylphenylalanine methyl ester, p-methoxycunnamic aldehyde, sucrose, lactose, fructose, and saccharin sodium). o-iLs, good t L, < ha 0.0
1-0.5%), wintergreen oil, spearmint oil, K.9-mint oil, satsafras oil, clove oil,
Flavoring agents such as eucalyptus oil, gelatin, -2 noton, arginine hydrochloride, albumin, whitening f11J such as lactosein, titanium dioxide, silicone, pigments, and ingredients of the song can be blended, for example, in the case of kneaded mm. It can be produced by mixing the above-mentioned desired ingredients with an appropriate amount of water.

Furthermore, in the present invention, allantoins, isosilone aminoproic acid, tranexamic acid, dextranase,
amylase, grotease, mutanaze, lysozyme,
Enzymes such as bacteriolytic enzymes and Lytec Endeim, alkali metal monofluorophosphates such as sodium monofluorophosphate and potassium monofluorophosphate, fluorides such as sodium fluoride, ammonium fluoride, and stannous fluoride, chlorhexinone salts, Dihydrocholesterol.

GuIJ 5-luretin salts, glycyrrhetinic acid, glycerophosphate, chlorophyll, calopegtide, water-soluble inorganic sulfur compounds, vitamins, anti-tartar agents, antibacterial +
Contains one or more active ingredients such as IJ and plaque inhibitors.
It is possible.

In addition, the dentifrice composition of the present invention includes:
In addition to methyl and ethyl paraoxybenzoate, there is no harm in using other preservatives such as Ikeno, paraoxybenzoic acid alkyl esters, and sodium benzoate.

As explained above, the toothpaste composition according to the present invention 1) 27
It has an alkaline abrasive as an abrasive and methyl/4'-oxybenzoate and/or ethyl oxybenzoate as a preservative, to which sodium chloride and/or potassium chloride are added. Particularly, the stability of the above-mentioned paraoxy-7benzoic acid alkyl esters is high, and the preservative power is effectively exhibited over a long period of time.

Hereinafter, the effects of the present invention will be specifically explained with reference to experimental examples.

[Experimental Example 1] σ retention stability of paraoxybenzoic acid alkyl ester 1st
A toothpaste with the following formulation containing 4'-benzoic acid alkyl ester as shown in the table was prepared by the method, filled into a tube and stored for 11 months. The amount of esters was measured and the residual rate compared to the initial value before storage was determined. The results are shown in Table 1.

In addition, the measurement of mother oxybenzene and alkyl ester was carried out using a high performance liquid chromatograph.

j Tei Shunkal 7 A 45% 45% 45% (10 Tislary-ptig, 6) Gellable Silica 2 1.5 1 Force g Ki7 Methyl Cell 1.2 t, ii,.

Loose sodium sorbitol 16 16 16 Pribilene glycol 2 2 2 Sodium lauryl sulfide 2 2 2 Saccharin sodium 0.05 0.05 Of) 5
Tanishina 1 1 1 Norioki 7 Azikoic acid 0.1 01 0,1 alkyl ester sodium chloride 0 3 10 Total 100.0 Tei 10011chi 100Ωchi 1st
Table O: Residual rate 90% or more Δ: 〃 70-90%
Toothpastes No. 4 to A6 were prepared, and the residual rate of methyl paraoxybenzoate was determined in the same manner as in Experimental Example 1. The results are shown in Table 2.

A4A3'A6 (10 TiS slurry - 15H9Ω) Gellable silica 2 1.5 1 Power dexymethyl cell 0.8 0.7 0.60 Sodium spring ginan 0.3 0.3 0.3 Sorbit 1
0 10 10 Glycerin 8 8 8 Sodium lauryl sulfate 1' 1.5 1.5 1.5
Satucharin sodium 0.1 0.1 0.1 Flavoring
1 1 1 Mother Oxybenzoic Acid 0.2 0.2 0.2 Methyl Sodium Chloride 0 3 10 4 ## Water Remaining Remaining Total i o o, ochi 100.0% 100.0% Table 2 The criteria for determining the survival rate are the same as in Experimental Example 1.

According to Experimental Example 1, in the toothpaste composition to which sodium chloride is not added, the storage stability of methyl paraoxybenzoate is good, and the storage rate after storage at 50° C. for one month is 90 qb. However, the stability of methyl paraoxybenzoate and methyl paraoxybenzoate is poor, with a residual rate of less than 90% after storage at 50°C for one month.In particular, methyl paraoxybenzoate is extremely stable at less than 70%. Bad sex. In contrast, in dentifrice compositions containing sodium chloride, the A4r ratios of methyl paraoxybenzoate and ethyl paraoxybenzoate were both 90% or higher; It was found that the compound stabilized methyl oxbenzoate and ethyl oxybenzoate.

In addition, as can be seen from the results of Experimental Example 2, when using aluminum hydroxide with a slurry PII of 9.0 as an abrasive, when all sodium chloride was mixed, 9.
The residual rate of methyl hydroxybenzoate was 90% or more, and it was confirmed that it was stabilized by the addition of sodium chloride, as in Experimental Example 1 in which calcium carbonate was used as the polishing agent.

In addition, magnesium carbonate (10
Heavy stitch slurry is 9.7), tertiary calcium phosphate,
Tertiary Magnesium Phosphate (10 times slurry, l(
Even in the toothpaste composition containing 10.0)'i, the stabilizing effect of methyl p-oxybenzoate and ethyl p-hydroxybenzoate was observed by adding sodium chloride.

Furthermore, results showing similar effects were obtained when potassium chloride was used in place of sodium chloride.Examples will be shown below.

[Example 1] Calcium carbonate 40.0% Gellable silica 2.0 Glopyrene glycol 2.0 Solpi, ) 16.0 Cal? Sodium chrysanthemum methylcellulose 1.2 Sodium lauryl sulfate 2.0 Polyoxyethylene hydrogenated castor oil 0.5 (addition of E060 mole) Sodium saccharin 0.05 Chlorhexinone hydrochloride 0.01 Tocopherol acetate 0.2 Methyl 9-hydroxybenzoate 0.15 Paraoxy Butyl benzoate 0.01 Sodium chloride 10.0, fragrance 1.0 Purified water balance ioo, ochi [Example 2] Aluminum hydroxide 30.0 chi! Calcium diphosphate 5.0 Globylene glycol 3.0 Sodium carboxymethyl cellulose 0.6 Carrageenan 0.5 Sodium lauryl sulfate 2.3 Sodium satucharin 0.1 Tranexamic acid 0.1 Potassium glycyrrhizinate 0.1 Methyl 79-laoxybenzoate 0 .05 Ethyl paraoxybenzoate 0.05 Sodium chloride 20.0 Aroma 1.5 Total 100.0% [Example 3] Aluminum hydroxide 45. o Tidalizable silica 2.0 Glopylene glycol 2.0 Sorbi,) 20.0 Carrageenan 0.5 Sodium alginate 0.5 Sodium lauryl sulfate, e Lauryl a jetanolamide 1.5 Sodium saccharin 0.2 Mono Sodium fluorophosphate 0.76 Dextranase 3000 u/g /9 Ethyl hydroxybenzoate 0.2 Sodium chloride 5.0 Flavor 1.0 Ice making Remaining total 100.01 [Example 4] Calcium carbonate 35.0 Magnesium carbonate 5.0 Glycerin 5.0 Sorbi, To 10.0 Cal? Sodium oxymethylcellulose 10 Sucrose fatty acid ester 2.0 Lauroyl dercosinate 0.5 Sodium satucalin o, i e-amitsukagulonic acid 0.05 Ara/toin chlorohydroxyaluminum O91no! Radoxybenzoyl methyl 0.1 Potassium chloride 15.0 Aromaceae 1.0 Total ioo, os [Example 5] Aluminum hydroxide 35.0 Magnesium triphosphate S, O chlorinating silica 3.0 Propylene Glycol 2.0 Glycerin 15.0 Polyethylene glycol φ400 1.0 Calgexymethyl cellulose sodium 0.7 Carrageenan 0.
3 Sodium lauryl sulfate 2.0 Polyoxyethylene hydrogenated castor oil 1.0 (EO20-
(1-l addition) Sodium quince 0.1 Chlorhexinone gluconate o, oi/4' methyl benzoyl 0.1 Sodium chloride 8.0 Flavor 1.0 Tank water Remaining total 100.0 [Example 6] Calcium carbonate 38. Otigelling Silica 2.0 Propylene Glycol 2.0 Sorbit 16.0 Sodium Carboxymethyl Cellulose 1.0 Sodium Alginate 0.2 Sodium Lauryl Sulfate 2.0 Polyoxyethylene Sorbitan Monostearate 0.
5 (IM) 40 moles added) Sodium saccharin 0.05 Sodium benzoate 0.2 Tranexam 11 0.05 Vitamin E nicotine ester 0.3 Methyl paraoxybenzoate 0.05 Ethyl paraoxybenzoate 0.03 Sodium chloride 1O10 δ Material 1.0 η 100.0% [Example 7] Calcium carbonate 75. O tiglycerin 5.0 Polyethylene glycol $400 5.0 Sodium lauryl sulfate 1.2 Sodium saccharin 0.1 79 Methyl laoxybenzoate 0.05 Sodium chloride 5.0 Flavoring 1.0 Total 100.0 Chi [Implemented] Example 8] Calcium carbonate 25.0 Aluminum hydroxide 20.0 Nrubitsu 15.0 Propylene glycol 2.0 Cal? Sodium oxymethylcellulose 1.2 Sodium myristyl sulfate 2.0 Sodium saccharin 0.15 Methyl paraoxybenzoate 0.1 Sodium chloride 5.0 Potassium chloride 5.0 Flavor 1.0 Applicant Takashi Kojima, Agent at Lion Corporation Shite continuation? i13 tl3 γ1) (voluntary) 1982
June 22, 2015 Kazuo Wakasugi, Commissioner of the Japan Patent Office 1, Indication of the case, Patent Application No. 248145 of 1982, 2, Name of the invention fIi polishing composition 3, Person making the amendment Relationship with the case Holder 1 Applicant Address 1-3-7 Honjo, Sumida-ku, Tokyo Name (6
76) Line A Line Co., Ltd. Representative Noriyoshi Kobayashi 4, Agent 〒104 6, Contents of amendment (1) Line 10 of the 16th line of the specification: ``Preservation rate,'' 1 is replaced with ``survival rate.'' I am corrected.

(2) Page 16, line 11 [90%J]
0% or more is corrected as J.

Below

Claims (1)

[Claims] 1. In a toothpaste composition containing an abrasive in which the abrasive's 10-fold Nk and the - of the aqueous suspension are in the range of 8 to 11, 5! Methyl laoxybenzoate and/or no! A dentifrice composition comprising ethyl hydroxybenzoate and sodium chloride and/or potassium chloride. 2. The dentifrice composition according to claim 1, wherein the abrasive is calcium carbonate, tertiary calcium phosphate, aluminum hydroxide, magnesium carbonate, or tertiary magnesium phosphate. 3. The amount of methyl p-oxybenzoate and/or ethyl p-oxybenzoate is 0.01 to 0.5 [
3. The dentifrice composition according to claim 1 or 2, which is .rl. 4. The dentifrice composition according to any one of claims 1 to 3, wherein the amount of sodium chloride and/or potassium chloride is 1 to 30% by weight of the total composition.