Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
  • A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/04—Dispersions; Emulsions
  • A61K8/06—Emulsions
  • A61K8/062—Oil-in-water emulsions
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/34—Alcohols
  • A61K8/345—Alcohols containing more than one hydroxy group
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/37—Esters of carboxylic acids
  • A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
  • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
  • A61K2800/21—Emulsions characterized by droplet sizes below 1 micron

Definitions

• the present invention relates to an emulsion-blended liquid oral composition and a method for improving the freeze-restorability thereof, which are excellent in appearance stability (freeze-restorability) at the time of freeze-thawing and can give a good feeling of use.
• Patent Document 1 JP-A-2005-179231
• Patent Document 2 Japanese Patent Laid-Open No. 2005-179231
• Patent Document 3 Japanese Patent Laid-Open No. 11-335253
• Patent Document 4 Japanese Patent No. 5043588,
• Patent Document 5 Special 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. 2011/0777847
• the emulsion composition is a state in which the water phase and the oil phase are mixed via an emulsifier, and the emulsion is agglomerated or coalesced due to long-term storage, mechanical vibration, rapid temperature change, etc.
• the appearance changes due to emulsion breakage, causing problems in quality, and in the above patent document, improvement of storage stability has been proposed. There was still room for improvement in the restoration of appearance.
• the said patent document does not mention the recoverability at the time of freezing by low temperature severe condition preservation
• the present invention has been made in view of the above circumstances, and is excellent in appearance stability (freezing / restoring property) at the time of freezing and thawing, and can also give a good feeling of use, and a liquid oral composition containing an emulsion and its It is an object of the present invention to provide a method for improving freezing and restoring properties.
• an N-acyl taurine salt When B) is blended, the appearance stability (freezing / restoring property) at the time of freezing and thawing is improved, a stable formulation appearance can be given, and a good feeling of use can be given, and the present invention has been made. It was.
• the appearance stability at the time of freezing and thawing of the emulsion-containing liquid preparation specifically frozen at a low temperature of ⁇ 20 ° C.
• the restorability of the appearance afterwards was remarkably improved. Even after freezing and thawing work of freezing at ⁇ 20 ° C. for 24 hours and then allowed to stand at 25 ° C. for 24 hours to thaw, the liquid could be recovered. Freezing and restoring properties that can suppress changes in white turbidity are provided.
• the combination of the components (A) and (B) specifically suppresses aggregation and coalescence of the emulsion due to a rapid temperature change (enlargement of the emulsion particle size), and improves the stability of the emulsion.
• it effectively imparts a refreshing feeling to the oral cavity and provides a good feeling of use. give.
• 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 is also contained in the emulsion particles of the emulsion (A).
• the content of the oily component / (the content of the N-acyl taurine salt (B)) is within the specific ratio range, the appearance stability (freezing / restoring property) upon freezing and thawing and the feeling of use are further improved. Therefore, it is preferable to mix
• isopropylmethylphenol (C) when isopropylmethylphenol (C) is blended, the above-described effects are excellent and the oral biofilm bactericidal power of isopropylmethylphenol is sufficiently expressed, and a high periodontal pathogenic biofilm bactericidal effect can be provided. Furthermore, when the fragrance (D) containing clove oil and / or thyme oil is blended, the pungent taste derived from the N-acyl taurine salt (B) can be suppressed, the irritation caused by the pungent taste can be suppressed, and a better feeling of use can be obtained. Can be granted.
• the present invention provides the following liquid oral composition and a method for improving the freeze-restoration thereof.
• the oily component contains an emulsion (A) composed of a liquid fat 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. % Liquid oral composition characterized by the above-mentioned.
• the oily component is one or more oils and fats selected from olive oil, camellia oil, castor oil, and trifatty acid glyceryl having 6 to 12 carbon atoms.
• emulsion (A) is an O / W type emulsion in which a polyhydric alcohol and water are used as a dispersion medium and an oil component is emulsified with a nonionic surfactant.
• Oral composition [6] The liquid oral composition according to any one of [1] to [5], further comprising 0.01 to 0.2% by mass of isopropylmethylphenol (C).
• the liquid oral cavity composition comprising 0.2 to 0.8% by mass of N-acyl taurine salt (B) in a liquid oral cavity composition in which an oily component is an emulsion (A) composed of liquid oil at 25 ° C.
• a method for improving the freezing and restoring properties of a composition [11] [10] The method for improving freezing and restoring properties of a liquid oral composition according to [10], wherein the content of the oil component contained in the emulsion particles of the emulsion (A) is 0.02 to 1.0% by mass of the whole composition.
• [14] The method for improving freezing and restoring properties of a liquid oral composition according to any one of [10] to [13], wherein the total content of the surfactant is 0.1 to 2% by mass.
• [15] The method for improving freezing and restoring properties of a liquid oral composition according to any one of [10] to [14], wherein the ethanol content in the composition is 100 ppm or less.
• [16] The method for improving the freezing and restoring properties of a liquid oral composition according to any one of [10] to [15], further comprising 0.01 to 0.2% by mass of isopropylmethylphenol (C).
• the perfume (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% by mass of the whole composition.
• isopropylmethylphenol can be blended to impart high oral biofilm sterilizing power.
• composition for liquid oral cavity of the present invention contains an emulsion (A) comprising an oily fat as an oily component at 25 ° C. and an N-acyl taurine salt (B).
• Emulsion (A) is an oil component in which the oil component contained in the emulsion particles consists of liquid oil at 25 ° C.
• an O / W type (oil-in-water type) emulsion obtained by emulsifying the above fats and oils with a polyhydric alcohol, water or the like as a dispersion medium can be used. It is preferable to add and mix an O / W type emulsion.
• the oil droplet particles of the O / W type emulsion are dispersed in the liquid oral composition, and the dispersion medium is mixed with the aqueous phase of the liquid oral composition and exists as an O / W type emulsion.
• oils and fats that are liquid at 25 ° C. which are oily components, include liquid oils and fats such as olive oil, camellia oil and castor oil, and tri-fatty acid glyceryl having a carbon chain length of 6 to 12, one of these alone or two or more of them. Can be used in combination.
• the tri fatty acid glyceryl include glyceryl tricaprylate, glyceryl tricaprate, and glyceryl tri (capryl / capric acid).
• tri-fatty acid glyceryl, particularly tri (capryl / capric acid) glyceryl is particularly preferable because it is resistant to discoloration due to oxidation and is stable.
• the amount of oily component in the emulsion is preferably 10 to 60% (mass%, the same applies hereinafter) of the whole emulsion including the dispersion medium, and particularly preferably 20 to 50%.
• the oil component amount is adjusted according to the average particle size of the emulsion particles, and the stability of the emulsion is improved by decreasing the oil component amount as the average particle size decreases. When it is 10% or more, the emulsion can be sufficiently formed. When it is 60% or less, the oily component is not separated, which is suitable for preventing the appearance stability from being impaired.
• one or more nonionic surfactants such as glycerin fatty acid ester, polyoxyethylene hydrogenated castor oil, and polyoxyethylene alkyl ether can be used, and those having an HLB value of 10 to 16 are preferable.
• the glycerin fatty acid ester include decaglycerin monofatty acid ester having 12 to 16 fatty acid carbon atoms such as decaglyceryl monomyristate and decaglyceryl monolaurate.
• the average number of moles of ethylene oxide added to the polyoxyethylene hydrogenated castor oil is preferably 10 to 100 moles, more preferably 20 to 60 moles.
• the average addition mole number of ethylene oxide of polyoxyethylene alkyl ether is preferably 4 to 20 moles, particularly preferably 6 to 15 moles.
• decaglycerin monofatty acid ester and polyoxyethylene hydrogenated castor oil are preferred.
• decaglyceryl monomyristate and polyoxyethylene hydrogenated castor oil are preferred from the viewpoint of appearance stability (freezing / restoring property) during freezing and restoration. preferable.
• the amount of emulsifier added is usually preferably 5 to 30%, more preferably 5 to 20% of the whole emulsion including the dispersion medium.
• the addition amount of the emulsifier is adjusted according to the average particle size 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 size becomes smaller. When it is 5% or more, the oily component is not separated, and when it is 30% or less, it is suitable for suppressing gelation.
• the dispersion medium in addition to water, one or more kinds of polyhydric alcohols such as glycerin, propylene glycol, 1,3-butylene glycol, dipropylene glycol and polyethylene glycol having an average molecular weight of 190 to 630 can be used. .
• the above emulsion preferably has an average particle size of emulsion particles of 30 to 300 nm, particularly 40 to 250 nm.
• the average particle size is within the above range, it is more preferable to improve the appearance stability (freezing / restoring property) while suppressing the irritation in the oral cavity and giving a refreshing feeling. If the average particle size is too small, the irritation at the time of use may be strong, and if it is too large, the refreshing feeling after use may not be obtained.
• grains is as showing below.
• a dynamic light scattering photometer DLS-8000 manufactured by Otsuka Electronics Co., Ltd. the emulsion was diluted 1000 times with purified water, placed in a cell, and the average particle size at 25 ° C. was measured.
• emulsion (A) in particular, glycerin or dipropylene glycol and water are used as a dispersion medium, triglyceride glyceryl as an oil component, and average added mole number of decaglycerin monofatty acid ester or ethylene oxide having 12 to 16 fatty acid carbon atoms.
• An O / W type emulsion having an average particle size of emulsion particles of 30 to 250 nm, which is emulsified with polyoxyethylene hydrogenated castor oil having a particle size of 20 to 60 mol, can be suitably added and blended.
• a known method can be adopted as a method for preparing the emulsion. For example, after stirring a predetermined amount of a nonionic surfactant, a polyhydric alcohol as a dispersion medium, and half of water with a homomixer, an oily component is added to form an emulsion, and finally the remaining water is added. W-type emulsions can be prepared. Thereafter, the average particle size of the prepared emulsion can be adjusted using a high-pressure homogenizer. In emulsification with a high-pressure homogenizer, the average particle diameter is adjusted by the difference in shearing force. When the emulsified particles are atomized, the stability over time is further improved.
• a microfluidizer manufactured by Microfluidics International CO
• a gorin homogenizer manufactured by Runny Gorin
• an optimizer manufactured by Sugino Machine
• the pressure during emulsification is usually 30 MPa or more, preferably 30 to 100 MPa.
• the introduction of the oil phase into the aqueous phase and the emulsification operation are preferably performed under a temperature condition of about 25 to 50 ° C.
• the emulsion prepared by the above method can be added and blended as the emulsion (A), but a commercially available product can also be used.
• a commercially available product can also be used.
• NET-TE-50 manufactured by Nikko Chemicals Co., Ltd. can be used.
• the content of the oil component contained in the emulsion particles of the emulsion (A) is preferably 0.02 to 1.0%, more preferably 0.05 to 0.5% of the total composition. %.
• the emulsion (A) is preferably added and blended so that the content of the oil component in the composition is within the above range.
• the content of the oil component contained in the emulsion particles is 0.02% or more, it is possible to prevent the irritation feeling during use from becoming strong.
• it is 1.0% or less appearance stability (freezing / restoring property) at the time of freezing and thawing is improved, and a lack of refreshing feeling after use can be prevented.
• the addition amount of the emulsion (A) (the addition amount of the emulsion including the dispersion medium) is preferably 0.1 to 4%, more preferably 0.2 to 1.0% of the whole composition.
• N-acyl taurine salt as component (B) examples include cocoyl methyl taurine salt, lauroyl methyl taurine salt, myristoyl methyl taurine salt, and the like. These sodium salts are preferably used. Among these, lauroylmethyl taurine salt is preferable from the viewpoint of freezing and restoring property.
• Specific examples of N-acyl taurine salts 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.
• the content of the N-acyl taurine salt (B) is 0.2 to 0.8%, preferably 0.3 to 0.5% of the whole composition.
• the effect of this invention can be provided in content being in the said range. If it is less than 0.2%, the turbidity of the composition changes after freezing and the appearance stability (freezing and restoring properties) is impaired. Moreover, a refreshing feeling cannot be imparted to the oral cavity. If it exceeds 0.8%, the stability of the emulsion decreases after freezing and the color tone of the composition fades (transparents), and the appearance stability (freezing and restoring properties) is impaired. Moreover, a feeling of irritation is given to the oral cavity and the feeling of use is impaired.
• the content of the component (B) is preferably adjusted according to the amount of the oil component contained in the emulsion particles of the emulsion (A) within the above range, and is optimal according to the average particle size of the emulsion particles. It is more preferable to adjust the range.
• the content of the oily component contained in the emulsion particles of the emulsion (A) relative to the whole composition (hereinafter abbreviated as the amount of the oily component in the emulsion (A)), the N-acyl taurine salt
• the ratio of the content of (B) to the total composition is preferably 0.15 to 3, more preferably 0 as the mass ratio. .2 to 2.5, more preferably 0.3 to 0.9.
• the appearance stability (freezing / restoring property) particularly during freezing and thawing is further improved, and the effects of the present invention are further improved. If the ratio is too small, sufficient freeze-recoverability may not be obtained, and satisfactory appearance stability may not be imparted. On the other hand, if it is too large, a feeling of irritation is strongly developed and the feeling of use may be lowered.
• the average particle size of the emulsion (A) particles, the content of the N-acyl taurine salt of the component (B), the amount of the oil component in the emulsion (A) / the amount of the component (B) When the ratio is any one of the following combinations, the effect of the present invention is further improved.
• isopropylmethylphenol C
• isopropylmethylphenol C
• isopropylmethylphenol C
• isopropylmethylphenol is added and blended, high biofilm bactericidal power can be imparted with excellent appearance stability (freezing / restoring property).
• Isopropylmethylphenol is a bactericidal component that can be blended in oral products, is blended in liquid preparations such as commercial mouthwashes, and is known to have bactericidal power on biofilms.
• isopropylmethylphenol is poorly water-soluble, it must be solubilized with a surfactant in order to be stably blended in an aqueous solution, and it is known that the level of bactericidal power varies depending on the solubilized state.
• the liquid oral cavity composition of the present invention is prepared as a mouthwash, a liquid dentifrice, and the like, and in addition to the above components, known components according to the dosage form can be blended within a range that does not interfere with the effects of the present invention.
• known components according to the dosage form can be blended within a range that does not interfere with the effects of the present invention.
• wetting agents, thickeners, surfactants, solvents, and if necessary, pH adjusters, sweeteners, colorants, fragrances, active ingredients and the like can be contained.
• wetting agent examples include sugar alcohols such as sorbitol, xylit, malt, and lactit, and polyhydric alcohols such as glycerin and propylene glycol.
• sugar alcohols such as sorbitol, xylit, malt, and lactit
• 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.
• thickener examples include xanthan gum, sodium alginate, polyvinyl alcohol, hydroxyethyl cellulose and the like (the amount is usually 0 to 1%, particularly 0 to 0.5%).
• a surfactant other than the N-acyl taurine salt generally used in liquid oral compositions is added and blended as a surfactant.
• a surfactant other than the N-acyl taurine salt generally used in liquid oral compositions.
• a surfactant is added and blended as a surfactant.
• a surfactant other than the N-acyl taurine salt generally used in liquid oral compositions is added and blended as a surfactant.
• a surfactant other than the N-acyl taurine salt generally used in liquid oral compositions is added and blended as a surfactant.
• betaine acetate type amphoteric surfactants such as alkyldimethylaminoacetic acid betaines and fatty acid amidopropyldimethylaminoacetic acid betaines as amphoteric surfactants
• N -Imazoline type amphoteric surfactants such as fatty acid acyl-N-carboxymethyl-N-hydroxyethylethylenediamine salts
• the addition amount of these surfactants is preferably 0.1 to 2%, particularly preferably 0.1 to 1.0%.
• the total content of the surfactant including the emulsifier of the emulsion (A) is preferably in the above range, particularly from the viewpoint of the stability of the emulsion. If the addition amount of the surfactant is too small, the freeze-recovery property may be deteriorated, and if it is too much, the emulsion may be dissolved.
• Anionic surfactants other than N-acyl taurine salts particularly alkyl sulfates such as sodium lauryl sulfate and acyl sarcosine salts such as sodium lauroyl sarcosine may not be added, but the effects of the present invention are not hindered. You may add in the range. When added, the addition amount is preferably 0.2% or less, particularly preferably 0.1% or less of the entire composition.
• purified water is generally used, and the blending amount is usually 60% or more.
• pH adjusters include phthalic acid, phosphoric acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid, carbonic acid, and potassium salts, sodium salts, ammonium salts, ribonucleic acid or salts thereof, sodium hydroxide, etc. Is mentioned.
• the composition of the present invention preferably has a pH of 5.5 to 8.5 at 25 ° C.
• a pH adjuster in the vicinity thereof a combination of citric acid and sodium citrate, phosphoric acid and its sodium salt (especially phosphorous) A combination of sodium dihydrogen acid and sodium monohydrogen phosphate is preferred.
• sweetening agent examples include saccharin sodium, stevocytes, sucralose, reduced palatinose, erythritol and the like.
• coloring agent water-soluble pigments having high safety such as Blue No. 1, Green No. 3, Yellow No. 4, Red No. 105 and the like can be added.
• Perfumes include 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 oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, grapefruit oil, sweetie Natural fragrances such as oil, coconut oil, Iris concrete, absolute peppermint, absolute rose, orange flower, and processing of these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder Perfumes, etc.) and menthol, Rubon, Anethole, Cineol, Methyl salicylate, Synamic aldehyde, Eugenol, 3-l-Mentoxy
• fragrances are preferably 0.00001 to 3% in the composition as long as the effects of the present invention are not hindered.
• a clove oil and / or thyme oil is contained as a fragrance, preferably in the range of 0.00001 to 0.01%, more preferably 0.0001 to 0.003%, The irritation feeling is further suppressed, and the usability of the preparation is further improved.
• flavor (D) containing a clove oil and / or thyme oil so that content of the clove oil and / or thyme oil in a composition may become the said range.
• the pungent taste derived from the N-acyl taurine salt (B) is suppressed, the irritation caused by the pungent taste is also suppressed, and the feeling of use is further improved.
• fungicides such as triclosan, cetylpyridinium chloride, benzethonium chloride, anti-inflammatory agents such as tranexamic acid, epsilon-aminocaproic acid, dextranase, amylase, protease, mutanase, lysozyme , Enzymes such as lytic enzyme, lytechenzyme, fluorides such as sodium fluoride, sodium monofluorophosphate, stannous fluoride, vitamin C such as aluminum chlorohydroxy allantoin, allantoin, azulene, lysozyme chloride, ascorbic acid, Tocopherol acetate, dihydrocholesterol, glycyrrhetin salts, glycyrrhetinic acid, hydrocholesterol, chlorophyll, copper chlorophyllin sodium, thyme, hornon, butterfly Plant extract
• the liquid oral composition of the present invention is preferably substantially free from ethanol from the viewpoint of stabilizing the emulsion.
• 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 whole composition.
• the liquid oral composition may contain a small amount of raw material-derived ethanol in the fragrance blended in the composition even if it is not blended with ethanol, in consideration of these reasons, It is desirable not to contain ethanol in addition to ethanol contained in trace amounts in perfumes.
• Liquid oral compositions (mouthwashes) shown in Tables 1 to 4 were prepared by conventional methods. Appearance stability when freeze-thawed (freezing / restoring) by the following methods, refreshing feeling after use in the oral cavity, when used The lack of irritation was evaluated. Moreover, about the composition for liquid oral cavity which mix
• An O / W type emulsion having the following composition was prepared by the following method. Stirring with a homomixer was carried out at a known high-pressure homogenizer (pressure condition 30 to 100 MPa), charging the oil phase into the aqueous phase, and emulsifying operation at 25 to 50 ° C. The average particle size of the emulsion particles was obtained by diluting the emulsion 1000 times with purified water using a dynamic light scattering photometer DLS-8000 manufactured by Otsuka Electronics Co., Ltd. Was measured.
• Embodision composition > [Emulsion A1 (average particle size 50 nm)] Decaglyceryl monolaurate 20% Tri (capryl / capric acid) glyceryl 20 Glycerin 15 Water 45 Total 100% After pre-stirring glycerin, half amount of water, and decaglyceryl monolaurate, tri (capryl / capric acid) glyceryl was added, stirred with a homomixer, and finally the remaining water was added.
• Embodision A4 (average particle size 100 nm)] Polyoxyethylene (60) hydrogenated castor oil 20% Tri (capryl / capric acid) glyceryl 30 Propylene glycol 10 Water 40 Total 100% After pre-stirring propylene glycol, half amount of water, polyoxyethylene (60) hydrogenated castor oil, tri (capryl / capric acid) glyceryl was added, and the mixture was stirred with a homomixer, and finally the remaining water was added.
• Embodision A5 (average particle size 50 nm)] Polyoxyethylene (20) hydrogenated castor oil 20% Tri (capryl / capric acid) glyceryl 20 Dipropylene glycol 10 Water 50 Total 100% Dipropylene glycol, half amount of water, polyoxyethylene (20) hydrogenated castor oil was pre-stirred, tri (capryl / capric acid) glyceryl was added, stirred with a homomixer, and finally the remaining water was added. .
• the external appearance of the composition for liquid oral cavity of the present invention becomes light cloudy when the particle size of the emulsion is small, and becomes cloudy as the particle size increases.
• the obtained freeze-thawed product was visually observed in accordance with the following criteria in terms of appearance stability (white turbidity of the liquid due to the dispersed emulsion) in comparison with a control product that was allowed to stand at ⁇ 5 ° C. for 24 hours and then at 25 ° C. for 24 hours. Judged. The samples with ⁇ and ⁇ were judged to have good appearance stability (freezing / restoring property). Evaluation criteria for appearance stability (freezing and restoring properties): ⁇ : No change in the turbidity of the liquid ⁇ : A slight change in the turbidity of the liquid is observed ⁇ : A change in the turbidity of the liquid is observed ⁇ : The turbidity of the liquid is greatly changed
• the oral bacteria used for the production of the model biofilm were all purchased from American Type Culture Collection (ATCC). Streptococcus gordonii ATCC 51656 strain and Actinomyces naeslandi ATCC 51655 strain were used as oral resident bacteria, and Porphysis as pathogenic bacteria. Romonas gingivalis strain ATCC33277 was used. These three bacterial species were inoculated into the above culture solution so as to be 2 ⁇ 10 7 cfu / mL (cloning forming units), respectively, and 37 ° C. and anaerobic conditions (80 vol% nitrogen, 10 vol% dioxide dioxide) together with the saliva-treated HA carrier. Carbon (10 vol% hydrogen) was continuously cultured for 2 weeks (the replacement rate of the culture solution was 10 vol%) to form a model biofilm with a mixture of three bacterial species on the HA surface.
• ATCC American Type Culture Collection
• model biofilm was immersed in 2 mL of an evaluation drug (liquid oral composition) for 3 minutes and washed 6 times with 1 mL of sterile physiological saline. Then, model biofilm is dispersed by sonication (200 ⁇ A, 10 seconds) with 4 mL of sterilized physiological saline, smeared on Bacteroides agar plate (blood agar plate with kanamycin added), and anaerobic until colonies can be confirmed with the naked eye. Culture (80 vol% nitrogen, 10 vol% carbon dioxide, 10 vol% hydrogen) was performed.
• Comparative Examples 1 to 3 lacking the component (B) are inferior in appearance stability (freezing / restoring property) even when they contain anionic surfactant sodium lauryl sulfate and sodium lauroyl sarcosine.
• Comparative Example 4 with a small amount of component was also inferior in appearance stability (freezing / restoring property).
• Comparative Example 5 in which there are too many components (B), the color of the liquid that became cloudy after freezing and restoration was faded (transparent), appearance stability (freezing and restoring properties) was inferior, and a sense of irritation derived from component (B) was expressed. .
• Example 19 to 24 The liquid oral compositions (mouthwashes) of Examples 19 to 24 shown in Table 5 were prepared in the same manner as described above, and the appearance stability (freezing / restoring property) during freezing and thawing was used in the same manner as above. The refreshing feeling later, lack of irritation at the time of use, and biofilm sterilizing power were evaluated, and the lack of pungent taste at the time of use was evaluated by the following method. Moreover, the nonpungency of Example 10 shown in Table 3 was evaluated similarly, and the said result was written together in Table 5 with this result.
• the fragrances a to f used in Examples 19 to 24 all contain clove oil and thyme oil. Table 5 shows the contents of clove oil and thyme oil in the compositions of each example. It is shown.
• a prescription example is shown below.
• the raw materials used are the same as described above.
• Mouthwash A) Emulsion A1 (average particle size 50 nm) 0.5% Content of oily component in emulsion (A) 0.10% (B) Lauroylmethyl taurine sodium 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% Perfume containing clove oil and thyme oil 0.2% Content of clove oil in the composition 0.00001% Content of thyme oil in the composition 0.00001% Water remaining Total 100%
• Mouthwash A) Emulsion A1 (average particle size 50 nm) 0.5% Content of oily component in emulsion (A) 0.10% (B) Lauroylmethyl taurine sodium 0.3% (C) Isopropyl methylphenol 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% Perfume containing clove oil and thyme oil 0.2% Content of clove oil in the composition 0.00001% Content of thyme oil in the composition 0.00001% Water remaining Total 100%

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