KR102345066B1 - Liquid composition for oral use and method for improving resilience to freezing thereof - Google Patents

Abstract

It contains an emulsion (A) consisting of oil and fat that has an oily component that is liquid at 25°C and N-acyltaurine salt (B), which is excellent in appearance stability (freeze recovery) during freeze-thawing and can give a good feeling of use. And, the content of the N-acyl taurine salt (B) is 0.2 to 0.8 mass %, a liquid oral composition characterized in that, and an oily component is a liquid oral cavity containing an emulsion (A) consisting of a liquid oil at 25 ° C. Provided is a method for improving freeze recovery properties of the liquid oral cavity composition, in which 0.2 to 0.8% by mass of N-acyltaurine salt (B) is blended with the composition for use.

Description

Liquid oral composition and method for improving freeze resilience thereof TECHNICAL FIELD

The present invention provides an emulsion formulation containing a liquid composition for oral use that is excellent in appearance stability (freeze recovery property) at the time of freezing and thawing, and can give a good feeling of use, and The present invention relates to a method for improving freeze stability.

Conventionally, as a technique for blending an emulsion with a liquid oral composition, a technique for blending a specific emulsion in order to suppress the ethanol stimulation of an ethanol formulation formulation (Patent Document 1; Japanese Patent Laid-Open No. 2005-179231), the retention of medicinal ingredients Techniques to improve functionality and improve functionality (Patent Document 2: Japanese Patent Application Laid-Open No. 2005-179231, Patent Document 3: Japanese Patent Application Laid-Open No. 11-335253, Patent Document 4: Japanese Patent No. 5043588, Patent Document 5: Japanese Patent Application Laid-Open No. 2011-168506, Patent Document 6: Japanese Patent Application Laid-Open No. 2012-12394, Patent Document 7: International Publication No. 2011/115034, Patent Document 8: International Publication No. 2011/077847) etc. are proposed have.

However, in the emulsion composition, the aqueous phase and the oil phase are mixed through the emulsifier, and aggregation or coalescence of the emulsion occurs due to long-term storage, mechanical vibration, rapid temperature change, etc. In liquid formulations, the appearance changes due to emulsification destruction, which causes problems in quality, and the above-mentioned patent literature also proposes improvement of storage stability. There is still room for improvement regarding the restoration of the city's exterior.

In addition, the said patent document does not mention about the recovery|restorability at the time of freezing in low-temperature severe condition storage.

Japanese Patent Laid-Open No. 2005-179231 Japanese Patent Laid-Open No. 2005-179231 Japanese Patent Laid-Open No. 11-335253 Japanese Patent Publication No. 5043588 Japanese Patent Laid-Open No. 2011-168506 Japanese Patent Laid-Open No. 2012-12394 International Publication No. 2011/115034 International Publication No. 2011/077847

Therefore, the liquid composition for oral cavity which mix|blended the emulsion WHEREIN: The improvement of the external appearance stability (freeze restoration property) at the time of freezing and thawing was a technical subject.

The present invention has been made in view of the above circumstances, and provides an emulsion-blended composition for liquid oral use that is excellent in appearance stability (freeze recovery property) at the time of freezing and thawing (freeze recovery property) and can give a good feeling of use, and a method for improving freeze recovery property thereof aim to do

As a result of the present inventors earnestly examining in order to achieve the said objective, an N-acyl taurine salt (B) to the liquid composition for oral cavity which mix|blended the emulsion (A) which oil-based component consists of a liquid fat and oil at 25 degreeC. ), the appearance stability (freeze recovery property) at the time of freezing and thawing is improved, and it has been found that it can give a stable appearance of the formulation, and can also give a good feeling of use, leading to the achievement of the present invention.

That is, in the present invention, when the emulsion (A) and the N-acyl taurine salt (B) are combined, the stability of the emulsion-blended liquid formulation upon freezing and thawing, specifically, the stability of the appearance after freezing at a low temperature of -20°C This remarkably improved, and as shown in the examples to be described later, the change in the turbidity of the liquid even after freezing at -20°C for 24 hours and then leaving it at 25°C for 24 hours to thaw, even after repeating the freeze-thaw operation 5 times. It gives freeze stability that can suppress In this case, by the combination of components (A) and (B), aggregation and coalescence of the emulsion due to rapid temperature change (increasing the emulsion particle size) is specifically suppressed, and the stability of the emulsion is improved, It gives the said effect, and the irritation|stimulation feeling derived from (B) component is reduced, and not only the irritation|stimulation feeling at the time of using in an oral cavity is suppressed, but also gives a feeling of cleanliness effectively in an oral cavity, and gives a good feeling of use.

In the present invention, in particular, the content of the oily component contained in the emulsion particles of the emulsion (A) is within a specific range with respect to the entire composition, and (content of the oily component contained in the emulsion particles of the emulsion (A))/( When the content of the N-acyl taurine salt (B)) is within a specific ratio range, the appearance stability (freeze recovery property) at the time of freezing and thawing and the feeling of use are further improved. Therefore, it is preferable to mix|blend (A) and (B) component within the said range.

Moreover, when isopropylmethylphenol (C) is mix|blended, while being excellent in the said effect, the oral biofilm sterilization power of isopropylmethylphenol is fully expressed, and it can give a high periodontal pathogenic biofilm sterilization effect.

In addition, when the fragrance (D) containing clove oil and/or thyme oil is blended, the spiciness derived from the N-acyl taurine salt (B) is suppressed, the irritation caused by the pungency is suppressed, and a better feeling of use can be given

Accordingly, the present invention provides the following liquid oral composition and a method for improving freeze restoration properties thereof.

[One]
The oily component contains an emulsion (A) consisting of a liquid fat and oil at 25°C, and an N-acyl taurine salt (B), and the content of the N- acyl taurine salt (B) is 0.2 to 0.8 mass %, (emulsion ( Content of the oil-based component contained in the emulsion particle of A)/(content of N-acyl taurine salt (B)) is 0.15-3 in mass ratio, The liquid composition for oral cavity characterized by the above-mentioned.

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[2]

The liquid composition for oral cavity as described in [1] whose oily component is 1 type, or 2 or more types of fats and oils selected from olive oil, camellia oil, castor oil, and C6-C12 tri-fatty acid glyceryl of a fatty acid.

[3]

The liquid composition for oral cavity as described in [1] or [2] whose content of the oil-based component contained in the emulsion particle of an emulsion (A) is 0.02-1.0 mass % of the whole composition.

[4]
[1], [2] or [3], wherein the N-acyl taurine salt (B) is a lauroyl methyl taurine salt.
[5]
The liquid oral composition according to any one of [1] to [4], wherein the emulsion (A) is an O/W emulsion in which a polyhydric alcohol and water are used as a dispersion medium and an oily component is emulsified with a nonionic surfactant. .
[6]
In addition to the nonionic surfactant used as the emulsifier of the emulsion (A), the liquid composition for oral use as described in [5] which further contains a nonionic surfactant other than that.
[7]
The liquid composition for oral cavity according to [6], wherein the nonionic surfactant further contained is polyoxyethylene hydrogenated castor oil.
[8]
Furthermore, the composition for liquid oral cavity in any one of [1]-[7] containing 0.01-0.2 mass % of isopropylmethylphenol (C).
[9]
Further, it contains a fragrance (D) containing clove oil and/or thyme oil, wherein the content of the clove oil and/or thyme oil is 0.00001 to 0.01 mass% of the total composition in any one of [1] to [8]. A liquid oral composition as described.
[10]
The liquid composition for oral cavity in any one of [1]-[9] whose content of ethanol in a composition is 100 ppm or less.
[11]
0.2-0.8 mass % of N-acyl taurine salt (B) is mix|blended with the liquid composition for oral cavity which oil-based component mix|blended the emulsion (A) which consists of liquid fats and oils at 25 degreeC, (in the emulsion particle of emulsion (A)) The method for improving the freeze recovery properties of the composition for liquid oral cavity, wherein the content of the contained oily component)/(the content of the N-acyl taurine salt (B)) is 0.15 to 3 as a mass ratio.
[12]
[11] The method for improving freeze recovery properties of the liquid oral composition according to [11], wherein the content of the oily component contained in the emulsion particles of the emulsion (A) is 0.02 to 1.0 mass% of the total composition.
[13]
The method for improving freeze recovery properties of the liquid oral composition according to [11] or [12], wherein the N-acyl taurine salt (B) is a lauroyl methyl taurine salt.
[14]
[11], [12] or [13], wherein the emulsion (A) is an O/W emulsion in which a polyhydric alcohol and water are used as a dispersion medium and an oily component is emulsified with a nonionic surfactant. A method for improving the freeze recovery properties of a composition.
[15]
In addition to the nonionic surfactant used as the emulsifier of the emulsion (A), the method for improving freeze recovery properties of the liquid oral composition according to [14], which further contains a nonionic surfactant.
[16]
The method for improving freeze recovery properties of the liquid oral composition according to any one of [11] to [15], wherein the content of ethanol in the composition is 100 ppm or less.
[17]
Further, the method for improving freeze recovery properties of the liquid oral composition according to any one of [11] to [16], wherein 0.01 to 0.2 mass% of isopropylmethylphenol (C) is blended.
[18]

Any of [11] to [17], wherein the fragrance (D) containing clove oil and/or thyme oil is blended so that the content of the clove oil and/or thyme oil is 0.00001 to 0.01 mass % of the total composition The method of improving the freeze recovery property of the liquid oral composition as described in one.

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ADVANTAGE OF THE INVENTION According to this invention, it is excellent in external stability (freeze recovery property) at the time of freezing and thawing, and also can provide the liquid oral composition containing an emulsion which can give a good feeling of use, and the method of improving its freeze recovery property can be provided. Moreover, in this invention, isopropyl methyl phenol can also be mix|blended and high oral biofilm sterilization power can also be provided.

Hereinafter, the present invention will be described in more detail. The liquid composition for oral cavity of this invention contains the emulsion (A) which consists of oils and fats which an oily component is liquid at 25 degreeC, and N-acyl taurine salt (B).

The emulsion (A) consists of oils and fats in which the oily component contained in the emulsion particles is liquid at 25°C. As this emulsion (A), polyhydric alcohol, water, etc. are used as a dispersion medium, and an O/W type (oil-in-water type) emulsion obtained by emulsifying the said oil and fat with an emulsifier can be used, It is preferable to add and mix|blend such an O/W type emulsion. In this case, the oil drop particle of an O/W type emulsion is disperse|distributed in the composition for liquid oral cavity, the said dispersion medium mixes with the aqueous phase of the liquid oral cavity composition, and exists as an O/W type emulsion.

Examples of oils and fats that are liquid at 25° C., which are oily components, include liquid oils such as olive oil, camellia oil, and castor oil, and glyceryl tri-fatty acid having a carbon chain length of 6 to 12. It can be used individually or in combination of 2 or more types. As tri-fatty acid glyceryl, tricaprylic acid glyceryl, tricapric acid glyceryl, tri(capuryl capric acid) glyceryl, etc. are mentioned. Among them, trifatty acid glyceryl, particularly tri(capuryl capric acid) glyceryl, is preferable because it is difficult to cause discoloration due to oxidation and is also stable.

The amount of oily components in the emulsion is preferably 10 to 60% (mass %, the same hereinafter) of the entire emulsion including the dispersion medium, and particularly preferably 20 to 50%. The amount of oil component is adjusted according to the average particle diameter of the emulsion particles, and the stability of the emulsion is improved by decreasing the amount of the oil component as the average particle diameter becomes smaller. If it is 10 % or more, emulsion formation can fully be carried out. If it is 60% or less, oily components do not separate, and it is suitable for preventing appearance stability from being impaired.

As an emulsifier, 1 type(s) or 2 or more types of nonionic surfactants, such as glycerol fatty acid ester, polyoxyethylene hydrogenated castor oil, and polyoxyethylene alkyl ether, can be used, The thing of HLB value 10-16 is preferable. Examples of the glycerin fatty acid ester include decaglycerin monofatty acid esters having 12 to 16 fatty acid carbon atoms, such as decaglyceryl monomyristate and decaglyceryl monolaurate. The average added mole number of ethylene oxide in polyoxyethylene hydrogenated castor oil is preferably 10 to 100 moles, particularly preferably 20 to 60 moles. As for the average added mole number of ethylene oxide of polyoxyethylene alkyl ether, 4-20 moles, 6-15 moles are especially preferable.

Among these, decaglycerin monofatty acid ester and polyoxyethylene hydrogenated castor oil are preferable, and in particular, from the viewpoint of external stability (freeze recovery property) in freeze recovery, decaglyceryl monomyristate and polyoxyethylene hydrogenated castor oil are preferable.

The amount of the emulsifier to be added is usually preferably 5 to 30% of the total emulsion including the dispersion medium, and more preferably 5 to 20%. The amount of the emulsifier added is adjusted according to the average particle diameter of the emulsion particles to be formed, and the stability of the emulsion is improved by increasing the content of the emulsifier as the average particle diameter decreases. If it is 5% or more, the oily component will not separate, and if it is 30% or less, it is suitable for gelation suppression.

As a dispersion medium, in addition to water, 1 type, or 2 or more types, such as polyhydric alcohol, such as glycerol, propylene glycol, 1, 3- butylene glycol, dipropylene glycol, and polyethyleneglycol with an average molecular weight of 190-630, can be used.

The emulsion preferably has an average particle diameter of the emulsion particles of 30 to 300 nm, particularly 40 to 250 nm. If the average particle diameter is within the above range, it is more suitable for suppressing irritation in the oral cavity and providing a feeling of cleanliness, while improving external stability (freeze recovery property). When the average particle diameter is too small, the irritation at the time of use may become strong, and if it is too large, the feeling of cleanliness after use may not be obtained.

In addition, the measuring method of the average particle diameter of an emulsion particle is as showing below.

Using a dynamic light scattering photometer DLS-8000 manufactured by Otsuka Electronics Co., Ltd., the emulsion was diluted 1000 times with purified water, put into a cell, and the average particle diameter at 25°C was measured.

As the emulsion (A), in particular, using glycerin or dipropylene glycol and water as a dispersion medium, trifatty acid glyceryl as an oily component, decaglycerin monofatty acid ester having 12 to 16 fatty acid carbon atoms or ethylene oxide has an average added mole number of 20 An O/W type emulsion emulsified with ~60 moles of polyoxyethylene hydrogenated castor oil and having an average particle diameter of 30 to 250 nm of emulsion particles may be suitably added and blended.

A well-known method can be employ|adopted for the preparation method of an emulsion.

For example, after stirring a predetermined amount of a nonionic surfactant, a polyhydric alcohol as a dispersion medium, and a half amount of water with a homomixer, an oily component is added to form an emulsion, and finally, the remaining water is added /W type emulsion can be prepared. Thereafter, the prepared emulsion can have an average particle size adjusted by using a high-pressure homogenizer.

In emulsification using a high-pressure homogenizer, the average particle size is adjusted by the difference in shear force. When the emulsified particles are atomized, the stability over time is further improved. As the high-pressure homogenizer, a microfluidizer (manufactured by Microfluidex International CO., , any model may be sufficient as long as it is the same mechanism. The pressure at the time of emulsification (high pressure emulsification) is 30 Mpa or more normally, and 30-100 Mpa is preferable. It is preferable to perform injection|throwing-in to the water phase of an oily phase, and emulsification operation under the temperature condition of about 25-50 degreeC.

In this invention, although the emulsion prepared by the said method can be added and mix|blended as an emulsion (A), a commercial item can also be used. For example, NET-TE-50 manufactured by Nikko Chemicals Co., Ltd. or the like can be used.

In the present invention, the content of the oily component contained in the emulsion particles of the emulsion (A) is preferably 0.02 to 1.0% of the total composition, more preferably 0.05 to 0.5%. It is preferable to add and mix|blend the emulsion (A) so that content of the oily component in a composition may become in the said range. When the content of the oil-based component contained in the emulsion particles is 0.02% or more, it is possible to prevent the feeling of irritation during use from becoming strong. When it is 1.0 % or less, the external appearance stability (freeze recovery property) at the time of freezing and thawing improves, and also it can prevent that the feeling of cleanliness after use is insufficient.

Moreover, as for the addition amount of emulsion (A) (addition amount of emulsion containing a dispersion medium), 0.1 to 4% of the whole composition is preferable, More preferably, it is 0.2 to 1.0%.

(B) As N-acyl taurine salt which is a component, a cocoyl methyl taurine salt, a lauroyl methyl taurine salt, myristyl methyl taurine salt, etc. are mentioned, These sodium salt is used suitably. Among them, lauroyl methyl taurine salt is preferable from the viewpoint of freeze recovery properties.

Specific examples of the N-acyl taurine salt include commercially available products such as NIKKOL CMT-30, NIKKOL CMT-30T, NIKKOL LMT, NIKKOL LMT-30, NIKKOL LMT-P, and NIKKOL MMT manufactured by Nikko Chemicals.

Content of N-acyl taurine salt (B) is 0.2 to 0.8 % of the whole composition, Preferably it is 0.3 to 0.5 %. The effect of this invention can be provided as content is in the said range. When it is less than 0.2%, the cloudiness of the composition changes after freeze recovery, and the appearance stability (freeze recovery property) is impaired. In addition, a feeling of cleanliness cannot be imparted to the oral cavity. When it exceeds 0.8%, the stability of the emulsion is lowered after freeze recovery, the color tone of the composition fades (transparency), and the appearance stability (freeze recovery property) is impaired. In addition, it gives a feeling of irritation in the oral cavity, and the feeling of use is impaired.

In addition, the content of component (B) is preferably adjusted according to the amount of oily component contained in the emulsion particles of the emulsion (A) within the above range, and it is more preferable to adjust it to an optimum range according to the average particle diameter of the emulsion particles. do.

In the composition of the present invention, the content of the oily component contained in the emulsion particles of the emulsion (A) with respect to the entire composition (hereinafter, it is abbreviated as the amount of the oily component in the emulsion (A)), and the composition of the N-acyltaurine salt (B) As for the ratio with respect to content with respect to the whole, ie, (oil-based component amount in emulsion (A))/(B) component amount, as mass ratio, 0.15-3 are preferable, More preferably, 0.2-2.5, More preferably, 0.3-0.9 to be. If it is within this range, the external appearance stability (freeze recovery property) especially at the time of freezing and thawing improves more, and the effect of this invention is more excellent. If the ratio is too small, sufficient freeze-resistance cannot be obtained and satisfactory appearance stability cannot be provided in some cases. Moreover, when it is too large, a feeling of stimulation may express strongly and the usability|use_condition may fall.

Moreover, in this invention, the ratio of the average particle diameter of the particle|grains of emulsion (A), content of N-acyl taurine salt of (B) component, (amount of oily component in emulsion (A))/(B) component amount is any one of the following limits If it is a combination of, the effect of the present invention is more excellent.

(i)

average particle diameter of the particles of the emulsion (A); 30~250nm

Content of N-acyl taurine salt (B); 0.2~0.8%

(Amount of oily component in emulsion (A))/(B) Amount of component; 0.20 to 1.0 by mass ratio

(ii)

average particle diameter of the particles of the emulsion (A); 40~200nm

Content of N-acyl taurine salt (B); 0.2~0.6%

(Amount of oily component in emulsion (A))/(B) Amount of component; 0.25 to 0.8 by mass ratio

(iii)

average particle diameter of the particles of the emulsion (A); 40-100nm

Content of N-acyl taurine salt (B); 0.2~0.4%

(Amount of oily component in emulsion (A))/(B) Amount of component; 0.3 to 0.7 by mass ratio

In the above (i) to (iii), if the average particle diameter of the particles of the emulsion (A) is within the above range and the content of the N-acyl taurine salt (B) is too small, the appearance stability at the time of freezing and thawing (freeze stability) This may not fully improve, and when there is too much, the irritation|stimulation feeling at the time of use may become strong. Moreover, when the ratio of (amount of oily component in emulsion (A))/(B) component amount is too small, the irritation|stimulation feeling at the time of use may become strong, and when too large, freeze recovery property may not fully improve.

In this invention, it is preferable to further add isopropyl methyl phenol (C), and when isopropyl methyl phenol is added and mix|blended, high biofilm sterilization power can be provided with the outstanding external stability (freeze recovery property).

Isopropylmethylphenol is a sterilization component which can be mix|blended with an oral product, it is mix|blended with liquid formulations, such as a commercially available mouthwash, and it is known that it has the sterilization power to a biofilm. However, since isopropylmethylphenol is poorly water-soluble, it is necessary to solubilize with a surfactant in order to mix|blend it stably with aqueous solution, and it is known that the level of bactericidal power changes with the solubilization state. When isopropylmethylphenol (C) was added to the structure of this invention, it turned out that the biofilm sterilization effect excellent unexpectedly was acquired. When adding isopropylmethylphenol to the composition of the present invention, 0.01 to 0.2% of the total composition, particularly preferably 0.02 to 0.1%.

The liquid composition for oral cavity of the present invention is prepared as a mouthwash, a liquid skirt, etc., in addition to the above-mentioned ingredients, a known component according to the dosage form in a range that does not interfere with the effect of the present invention can be combined. For example, it can contain a wetting agent, a thickener, surfactant, a solvent, and also a pH adjuster, a sweetener, a coloring agent, a fragrance|flavor, an active ingredient, etc. as needed.

Examples of the wetting agent include sugar alcohols such as sorbitol, xylite, maltite, and lactite, and polyhydric alcohols such as glycerin and propylene glycol. The blending amount of these wetting agents is usually 5 to 15%, and the total amount including the dispersion medium of the emulsion (A) is preferably within the above range.

As a thickener, xanthan gum, sodium alginate, polyvinyl alcohol, hydroxyethyl cellulose, etc. are mentioned (combination amount is 0-1% normally, especially 0-0.5%).

As surfactant, in addition to the nonionic surfactant used as an emulsifier of an emulsion (A), surfactant other than N-acyltaurine salt normally used for liquid oral composition can be added and mix|blended. Specifically, as a nonionic surfactant, polyethylene glycol fatty acid ester, sucrose fatty acid ester, as an amphoteric surfactant, betaine acetate type amphoteric surfactants such as alkyldimethylaminoacetic acid betaine and fatty acid amide propyldimethylaminoacetic acid betaine, N -amino acid type surfactants, such as imidazoline type amphoteric surfactants, such as fatty-acid acyl-N-carboxymethyl-N-hydroxyethyl ethylenediamine salt, and N-fatty acid acyl-L- alginate salt, etc. are mentioned. The amount of these surfactants added is preferably 0.1 to 2%, particularly preferably 0.1 to 1.0%.

In the present invention, the total content of the surfactant including the emulsifier of the emulsion (A) is preferably within the above range, particularly from the viewpoint of stability of the emulsion. When there is too little addition amount of surfactant, freeze recovery property may worsen, and when too much, the emulsion may melt|dissolve.

In addition, anionic surfactants other than N-acyl taurine salts, especially alkyl sulfates such as sodium lauryl sulfate, and acyl sarcosine salts such as sodium lauroyl sarcosine do not need to be blended, but in the present invention It is good to add it in a range that does not interfere with the effect of In the case of addition, the amount added is preferably 0.2% or less of the total composition, particularly preferably 0.1% or less.

As a solvent, purified water is generally used and a compounding quantity is 60 % or more normally.

Examples of the pH adjuster include phthalic acid, phosphoric acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid, carbonic acid, potassium salts, sodium salts, ammonium salts, ribonucleic acid or salts thereof, sodium hydroxide and the like. In addition, the composition of the present invention preferably has a pH of 5.5 to 8.5 at 25°C, and a combination of citric acid and sodium citrate as a pH adjuster in the vicinity thereof, phosphoric acid and its sodium salt (especially sodium dihydrogen phosphate and sodium monohydrogen phosphate) A combination with

Examples of the sweetener include sodium saccharin, stevioside, sucralose, reduced palatinose, and erythritol.

As a colorant, water-soluble pigments with high safety such as Blue No. 1, Green No. 3, Yellow No. 4, and Red No. 105 can be added.

As fragrances, peppermint oil, spearmint oil, anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime oil, Lavender oil, rosemary oil, laurel, chamomile oil, caraway oil, marjoram oil, bay oil, lemongrass oil, oliganum oil, pine needle oil, neroli oil, rose oil, jasmine oil, grapefruit oil, sweet milk, milk Natural fragrances such as lees, iris concrete, absolute peppermint, absortrose, and orange flower, and processing treatment of these natural fragrances (current part cut, downstream part cut, Fragrances obtained by fractionation, liquid extraction, essence, powder flavoring, etc.) and menthol, carbon, anetol, cineol, methyl salicylate, cinnamic aldehyde, eugenol 3-l -Mentoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone, methyl acetate, N-substituted-paramentane-3-carboxamide, pinene, octylaldehyde, citral, Pulegon, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, hexanal, butanol, isoamyl alcohol, Individual fragrances such as hexanol, dimethyl sulfide, cyclotene, furfural, trimethylpyrazine, ethyl lactate and ethyl thioacetate, strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, It can be used combining well-known fragrance materials used for oral composition, such as a combination fragrance|flavor, such as a mango flavor, a butter flavor, a milk flavor, a fruit mix flavor, and a tropical fruit flavor. As for content of these fragrance|flavors, 0.00001 to 3% of a composition is preferable in the range which does not impair the effect of this invention.

Further, in the present invention, when, in particular, clove oil and/or thyme oil as a fragrance is contained in an amount of preferably 0.00001 to 0.01%, more preferably 0.0001 to 0.003% of the total composition, irritation at the time of use is further suppressed, and the formulation the feeling of use is further improved.

In this case, it is preferable to mix|blend the fragrance|flavor (D) containing clove oil and/or thyme oil so that content of clove oil and/or thyme oil in a composition may become the said range. When content of clove oil and/or thyme oil is in the said range, the pungent taste derived from N-acyl taurine salt (B) is suppressed, the irritation|stimulation by pungency is suppressed, and usability improves more.

As an active ingredient, in addition to isopropylmethylphenol, for example, fungicides such as triclosan, cetylpyridinium chloride, benzethonium chloride, anti-inflammatory agents such as tranexamic acid and epsilon-aminocaproic acid, dextranase, amylase, protease, no Enzymes such as Thanase, Lysozyme, Lysozyme, Litecenzyme, Sodium fluoride, Sodium monofluorophosphate, Fluoride such as stannous fluoride, Aluminum Chlorhydroxyalantoin, Allantoin, Azulene, Lysozyme Chloride, Ascor Vitamin C such as vinic acid, tocopherol acid ester, dihydrocholesterol, glycyrrhetin salt, glycyrrhetic acid, hydrocholesterol, chlorophyll, sodium copper chlorophyllin, thyme, gold, sperm, plant extract such as hamamelis, glue Copper conate, caropeptide, sodium polyphosphate, water-soluble inorganic phosphate compound, polyvinylpyrrolidone, sodium lauroyl sarcosine, tartar inhibitor, anti-plaque agent, potassium nitrate, aluminum lactate, etc. can be added. In addition, these active ingredients can be mix|blended in an effective amount in the range which does not interfere with the effect of this invention.

The composition for liquid oral cavity of this invention is more preferable from the point of stabilization of an emulsion that ethanol is not included substantially. Here, "substantially free of ethanol" means that the amount of ethanol in the composition is preferably 100 ppm or less, more preferably 50 ppm or less, and particularly preferably 10 ppm or less with respect to the entire composition. In addition, in the liquid oral composition, even if ethanol is unblended, there are cases where a trace amount of ethanol derived from the raw material is contained in the fragrance compounded in the composition. It is preferred not to contain ethanol.

Example

Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not limited to the following Example. In addition, in the following examples, all % denotes mass % unless otherwise specified.

[Examples 1 to 16, Comparative Examples 1 to 10]

The liquid oral compositions (cleansing agents) shown in Tables 1 to 4 were prepared by the usual method, and the appearance stability at the time of freezing and thawing (freeze recovery property), the feeling of cleanliness after use in the oral cavity, and the absence of irritation at the time of use by the following method evaluated. In addition, about the composition for liquid oral cavity which mix|blended the isopropyl methylphenol shown in Tables 3 and 4, the following method further evaluated the biofilm sterilization power. The results were put together in Tables 1-4.

In addition, the preparation method and composition of the used emulsion are as follows. The prepared emulsions A1 to A5 were blended in the amounts indicated in the table.

<Method of preparing emulsion>

An O/W type emulsion having the following composition was prepared by the following method. In addition, stirring by a homomixer was performed at 25-50 degreeC in the well-known high-pressure homogenizer (pressure condition of 30-100 MPa), input into the oil phase, and emulsification operation.

In addition, the average particle diameter of the emulsion particles, using a dynamic light scattering photometer DLS-8000 manufactured by Otsuka Electronics Co., Ltd., diluted 1000 times with purified water, put into a cell, and measured the average particle diameter at 25 ° C.

<Composition of emulsion>

[Emulsion A1 (average particle size 50 nm)]

Decaglyceryl monolaurate 20%

Tri (capuryl capric acid) glyceryl 20

glycerin 15

water 45

Total 100%

After preliminary stirring of glycerin, a half amount of water and decaglyceryl monolaurate, tri(capuryl capric acid) glyceryl was added, followed by stirring with a homomixer, and finally the remaining water was added to prepare.

[Emulsion A2 (average particle size 200 nm)]

Decaglyceryl Monomyristate 10%

Tri(capuryl capric acid) glyceryl 50

glycerin 15

water 25

Total 100%

After preliminary stirring of glycerin, a half amount of water, and decaglyceryl monomyristate, tri (capuryl capric acid) glyceryl was added, followed by stirring with a homomixer, and finally the remaining water was added to prepare.

[Emulsion A3 (average particle size 100 nm)]

Decaglyceryl monolaurate 10%

Tri (capuryl capric acid) glyceryl 30

glycerin 15

water 45

Total 100%

After preliminary stirring of glycerin, a half amount of water and decaglyceryl monolaurate, tri(capuryl capric acid) glyceryl was added, followed by stirring with a homomixer, and finally the remaining water was added to prepare.

[Emulsion A4 (average particle size 100 nm)]

Polyoxyethylene (60) hydrogenated castor oil 20%

Tri (capuryl capric acid) glyceryl 30

Propylene glycol 10

water 40

Total 100%

Propylene glycol, a half amount of water, and polyoxyethylene (60) hydrogenated castor oil were pre-stirred, tri(capuryl capric acid) glyceryl was added, stirred with a homomixer, and finally the remaining water was added to prepare.

[Emulsion A5 (average particle diameter 50 nm)]

Polyoxyethylene (20) hydrogenated castor oil 20%

Tri (capuryl capric acid) glyceryl 20

Dipropylene glycol 10

water 50

Total 100%

After preliminary stirring with dipropylene glycol, a half amount of water, and polyoxyethylene (20) hydrogenated castor oil, tri (capuryl capric acid) glyceryl was added, followed by stirring with a homomixer, and finally the remaining water was added to prepare.

In addition, the detail of the raw material used is shown.

sodium lauroylmethyltaurine; Nikko Chemicals Co., Ltd.

isopropylmethylphenol; Osaka Chemical Co., Ltd. product

Polyoxyethylene (60) hydrogenated castor oil;

Average added mole number of ethylene oxide 60, Nikko Chemicals Co., Ltd.

In addition, the fragrance|flavor used contains clove oil and thyme oil, and the Example and comparative example shown in Tables 1-4 contain 0.00001% of clove oil and 0.00001% of thyme oil in a composition, respectively.

(1) Evaluation method of appearance stability (freeze stability) at the time of freezing and thawing

As for the external appearance of the composition for liquid oral cavity of emulsion compounding, the liquid is cloudy by the scattering phenomenon of an emulsion. If the stability of the emulsion is poor, agglomeration, coalescence or solubilization occurs, and the turbidity increases as the particle size increases due to aggregation or coalescence, or conversely, when the solubilization proceeds under the influence of a surfactant, etc., the whiteness decreases. changes are observed. From this, visual observation evaluated the change of the cloudiness of the composition for liquid oral cavity for stability of an emulsion as an index|index.

Moreover, when the particle diameter of an emulsion is small, the external appearance of the composition for liquid oral cavity of this invention becomes light cloudy, and becomes cloudy as a particle size becomes large.

450 ml of a sample (liquid oral composition) is filled in a colorless and transparent PET container (manufactured by Yoshino Kogyo Co., Ltd.) with a capacity of 500 ml, frozen at -20°C, left to stand for 24 hours, and then 25 The sample was thawed by allowing it to stand for 24 hours at ℃. This operation was repeated 5 times as 1 cycle. For the obtained freeze-thaw product, the appearance stability (turbidity of the liquid by the dispersed emulsion) was compared with a control product left at -5°C for 24 hours and then at 25°C for 24 hours, and visually judged according to the following criteria. did Those of ◎ and ○ were judged to have good appearance stability (freeze recovery property).

Evaluation criteria for appearance stability (freeze stability):

◎: No change is recognized in the liquid turbidity

○: A slight change is recognized in the liquid turbidity.

△: A change is recognized in the turbidity of the liquid

x: The turbidity of the liquid is changing greatly.

(2) Evaluation method of feeling of cleanliness after use

After 10 evaluators held 10 ml of each liquid oral composition in their mouth and held it for 30 seconds, the feeling of cleanliness after washing was evaluated. It was evaluated according to the following four-step rating criteria, and it was determined according to the following evaluation criteria from the average score of 10 people.

Rating criteria:

4 points: A high sense of cleanliness was obtained

3 points|pieces: A slightly high feeling of cleanliness was obtained

2 points|pieces: A very slight feeling of cleanliness was obtained

1 point|piece: A feeling of cleanliness was hardly obtained.

Evaluation criteria for feeling of cleanliness after washing:

◎: Average score of 3.5 or more and 4.0 or less

○: Average point 3.0 or higher but less than 3.5

△: average score of 2.0 or more but less than 3.0

×: Average score less than 2.0

(3) Evaluation method of no feeling of irritation at the time of use

Ten evaluators evaluated the absence of irritation when 10 ml of each liquid oral composition was held in their mouth and rubbed for 30 seconds. The evaluation was performed according to the following four-step rating criteria, and it was determined according to the following evaluation criteria from the average score of 10 persons.

Rating criteria:

4 points: no irritation

3 points|pieces: There was little stimulation

2 points: There was slight irritation

1 point: There was quite a bit of irritation

Criteria for the evaluation of the sense of irritation at the time of passage:

◎: Average score of 3.5 or more and 4.0 or less

○: Average point 3.0 or higher but less than 3.5

△: average score of 2.0 or more but less than 3.0

×: Average score less than 2.0

(4) Evaluation method of biofilm sterilization power

A hydroxyapatite (HA) plate (manufactured by Asahi Optical Co., Ltd.) having a diameter of 7 mm and a thickness of 3.5 mm was treated with human non-stimulated saliva filtered through a 0.45 μm filter for 4 hours as a model biofilm production carrier. was used.

As a culture medium, hemin (made by Sigma) 5 mg/L and vitamin K (made by Wako Pure Chemical Industries, Ltd.) 1 mg/L were added to a solution obtained by dissolving 30 g of trypticase soy broth (manufactured by Difco) in 1 liter of purified water.

All oral bacteria used for the production of the model biofilm were purchased from the American Type Culture Collection (ATCC), and Streptococcus gordoni ATCC51656 strain and Actinomyces naesul were common oral bacteria. Lundi ATCC51655 strain, Porphyromonas gingivalis ATCC33277 strain was used as a pathogenic bacterium.

Each of these 3 strains ^{was inoculated into the above-mentioned culture solution to become 2×10 7} cfu/ml (clony forming units), and together with the HA carrier treated with saliva at 37° C. under anaerobic conditions (80 vol% nitrogen, 10 vol% carbon dioxide, 10 vol% hydrogen) for 2 weeks (the substitution rate of the culture solution was 10 vol%) was performed to form a model biofilm of a mixture of three strains on the HA surface.

The formed model biofilm was immersed in 2 ml of an evaluation agent (liquid oral composition) for 3 minutes, and washed 6 times with 1 ml of sterile physiological saline. Thereafter, the model biofilm is dispersed by ultrasonication (200 μA, 10 seconds) with 4 ml of sterile physiological saline,

Spread 50 μl on a Bacteroides agar plate (blood agar plate with kanamycin addition), and anaerobic culture (80 vol% nitrogen, 10 vol% carbon dioxide, 10 vol% hydrogen). The number of grown colonies was counted, the viable cell number (cfu) of the remaining Porphyromonas gingivalis bacteria was calculated|required, and it judged according to the following criteria. It was judged that the thing of (double-circle) and (circle) was excellent in biofilm sterilization power.

Evaluation standard :

◎: less than ^{10 6}

○ : 10 ⁶ or more and less ^{than 10 7}

△: 10 ⁷ or more and less ^{than 10 8}

×: 10 ⁸ or more

[Table 1]

[Table 2]

As shown in Table 2, Comparative Examples 1 to 3 lacking component (B) were inferior in appearance stability (freeze recovery property) even if they contained sodium lauryl sulfate and sodium lauroyl sarcosine, which are anionic surfactants. , (B) Comparative Example 4 with a small amount of component was also inferior in appearance stability (freeze recovery property). (B) In Comparative Example 5 with too many components, the color tone of the cloudy liquid faded (transparency) after freezing restoration, it was inferior to appearance stability (freeze restoration property), and the irritation|stimulation feeling derived from (B) component expressed.

[Table 3]

[Table 4]

As shown in Table 4, when isopropylmethylphenol is added, Comparative Examples 6 to 8 lacking component (B) contain sodium lauryl sulfate and sodium lauroyl sarcosine which are anionic surfactants, The biofilm sterilization power was also low along with the inferior appearance stability (freeze recovery property), and Comparative Example 9 with a small amount of (B) component also had a low biofilm sterilization power.

[Examples 17-22]

The liquid oral composition (wash mouthwash) of Examples 17 to 22 shown in Table 5 was prepared in the same manner as described above, and in the same manner as described above, the appearance stability (freeze recovery property) at the time of freezing and thawing, the feeling of cleanliness after use in the oral cavity, The absence of irritation at the time of use and the biofilm sterilization power were evaluated, and the absence of pungent taste at the time of use was evaluated by the following method. In addition, the absence of spiciness of Example 9 shown in Table 3 was evaluated similarly, and the said result was written together in Table 5 with this result.

In addition, the fragrance|flavors a-f used in Examples 17-22 all contain clove oil and thyme oil, and content of clove oil and content of thyme oil in the composition of each example are as showing in Table 5.

(5) Evaluation method of no spiciness at the time of use

Ten evaluators put 10 ml of each liquid oral composition in their mouth, and evaluated the absence of a pungent taste at the time of slurping for 30 seconds. The evaluation was performed according to the following four-step rating criteria, and it was determined according to the following evaluation criteria from the average score of 10 persons.

Rating criteria:

4 points: No spicy taste

3 points: There was hardly any spicy taste

2 points: Slightly spicy

1 point: Spicy taste was quite good

Evaluation criteria for the lack of spiciness in Segushi:

◎: Average score of 3.5 or more and 4.0 or less

○: Average point 3.0 or higher but less than 3.5

△: average score of 2.0 or more but less than 3.0

×: Average score less than 2.0

[Table 5]

As can be seen from the results in Table 5, when a fragrance (D) containing clove oil and/or thyme oil is contained, and a specific amount of clove oil and/or thyme oil is contained in the composition, the pungency is suppressed, The irritation at the time of use was more suppressed, and the feeling of use was improved.

A prescription example is shown below. In addition, the raw material used is the same as that mentioned above.

[Prescription 1] Eyewash amount

(A) Emulsion A1 (average particle size 50 nm) 0.5%

Content of oily component in emulsion (A) 0.10%

(B) Sodium lauroylmethyltaurine 0.3%

Sodium Fluoride 0.05%

Copper gluconate 0.05%

Glycerin 3%

Propylene glycol 4%

Polyoxyethylene (60) hydrogenated castor oil 0.20%

Citric acid 0.70%

Sodium Citrate 0.3%

Fragrance containing clove oil and thyme oil 0.2%

Content of clove oil in composition 0.00001%

The content of thyme oil in the composition is 0.00001%

water rest

Total 100%

[Prescription 2] Eyewash solution

(A) Emulsion A1 (average particle size 50 nm) 0.5%

Content of oily component in emulsion (A) 0.10%

(B) Sodium lauroylmethyltaurine 0.3%

(C) isopropylmethylphenol 0.05%

Allantoin 0.05%

Glycerin 3%

Propylene glycol 4%

Polyoxyethylene (60) hydrogenated castor oil 0.20%

Citric acid 0.70%

Sodium Citrate 0.3%

Fragrance containing clove oil and thyme oil 0.2%

Content of clove oil in composition 0.00001%

The content of thyme oil in the composition is 0.00001%

water rest

Total 100%

[Prescription 3] Eyewash solution

(A) Emulsion A1 (average particle size 50 nm) 0.5%

Content of oily component in emulsion (A) 0.10%

(B) Sodium lauroylmethyltaurine 0.3%

(C) isopropylmethylphenol 0.05%

Sodium Fluoride 0.02%

Glycerin 3%

Propylene glycol 4%

Polyoxyethylene (60) hydrogenated castor oil 0.20%

Citric acid 0.70%

Sodium Citrate 0.3%

Fragrance containing clove oil and thyme oil 0.2%

Content of clove oil in composition 0.00001%

The content of thyme oil in the composition is 0.00001%

water rest

Total 100%

Claims (16)

The oily component contains an emulsion (A) consisting of a liquid fat and oil at 25°C, and an N-acyl taurine salt (B), and the content of the N- acyl taurine salt (B) is 0.2 to 0.8 mass %, (emulsion ( A liquid composition for oral cavity characterized in that content of the oily component contained in the emulsion particle of A)/(content of N-acyl taurine salt (B)) is 0.15-3 as mass ratio. According to claim 1,
The oily component is one or two or more types of fats and oils selected from olive oil, camellia oil, castor oil, and glyceryl tri-fatty acid having 6 to 12 carbon atoms of fatty acids. 3. The method of claim 1 or 2,
Content of the oily component contained in the emulsion particle of an emulsion (A) is 0.02-1.0 mass % of the whole composition, The liquid composition for oral cavity characterized by the above-mentioned. 3. The method of claim 1 or 2,
N-acyl taurine salt (B) is a lauroyl methyl taurine salt, The liquid composition for oral cavity characterized by the above-mentioned. 3. The method of claim 1 or 2,
Emulsion (A) uses polyhydric alcohol and water as dispersion medium, and it is O/W type emulsion which emulsified the oily component with the nonionic surfactant, The liquid composition for oral cavity characterized by the above-mentioned. 6. The method of claim 5,
In addition to the nonionic surfactant used as an emulsifier of an emulsion (A), it further contains a nonionic surfactant in addition to that, The liquid composition for oral cavity characterized by the above-mentioned. 7. The method of claim 6,
In addition, the nonionic surfactant contained further is polyoxyethylene hydrogenated castor oil, The liquid composition for oral cavity characterized by the above-mentioned. 3. The method of claim 1 or 2,
Moreover, 0.01-0.2 mass % of isopropylmethylphenol (C) is contained, The liquid composition for oral cavity characterized by the above-mentioned. 3. The method of claim 1 or 2,
Moreover, it contains the fragrance|flavor (D) containing clove oil and/or thyme oil, Content of the said clove oil and/or thyme oil is 0.00001-0.01 mass % of the whole composition, The liquid composition for oral cavity characterized by the above-mentioned. 3. The method of claim 1 or 2,
Content of ethanol in a composition is 100 ppm or less, The composition for liquid oral cavity characterized by the above-mentioned. 0.2-0.8 mass % of N-acyl taurine salt (B) is mix|blended with the liquid composition for oral cavity which oil-based component mix|blended the emulsion (A) which consists of liquid fats and oils at 25 degreeC, (in the emulsion particle of emulsion (A)) Content of the oily component contained)/(content of N-acyl taurine salt (B)) shall be 0.15-3 as mass ratio, The cryoprecoverability improvement method of the said liquid oral cavity composition characterized by the above-mentioned. 12. The method of claim 11,
Content of the oily component contained in the emulsion particle of an emulsion (A) is 0.02-1.0 mass % of the whole composition, The cryoprecoverability improvement method of the composition for liquid oral cavity characterized by the above-mentioned. 13. The method of claim 11 or 12,
N-acyl taurine salt (B) is a lauroyl methyl taurine salt, The method for improving freeze recovery properties of a liquid oral composition, characterized in that. 13. The method of claim 11 or 12,
The emulsion (A) is an O/W type emulsion in which a polyhydric alcohol and water are used as a dispersion medium and an oily component is emulsified with a nonionic surfactant, The method for improving freeze recovery properties of a liquid oral composition. 15. The method of claim 14,
In addition to the nonionic surfactant used as an emulsifier of the emulsion (A), the method for improving freeze recovery properties of a liquid oral composition comprising further comprising a nonionic surfactant in addition to that. 13. The method of claim 11 or 12,
A method for improving freeze recovery properties of a liquid oral composition, characterized in that the content of ethanol in the composition is 100 ppm or less.