JP5066850B2 - O / W type emulsion composition - Google Patents

Description

  The present invention relates to an O / W emulsion composition that is safe and excellent in the feeling of use, with less irritation when formulated with urea and used on the skin.

  Conventionally, O / W emulsion compositions have been used in creams, lotions, ointments, gels, sprays and the like applied to the skin. In order to stably store the O / W emulsion composition, it is common to use a surfactant, but the surfactant has been suggested to irritate the skin.

  Many products, such as creams and lotions that are applied to urea-containing skin, are already on the market and are generally used. As a cream containing urea, for example, a cream containing urea and a surfactant is disclosed (see Patent Document 1).

  Polyvinyl alcohol and carboxyvinyl polymer are disclosed for use in creams, lotions, ointments and the like applied to the skin. For example, a cream for massage cosmetics for eyes containing polyvinyl alcohol, a carboxyvinyl polymer and a surfactant is disclosed (Patent Document 2).

  Creams, ointments and the like are used by filling tubes made of metal such as aluminum, aluminum laminated tubes, or candy containers as pharmaceuticals, quasi drugs, cosmetics, and the like. The inner surface of a tube made of a metal such as aluminum is coated with an epoxy resin added with phenol resin, melamine resin, etc., and the inner tube coated with epoxy phenol resin is particularly common. is there.

JP-A-11-349472 JP 2001-39851 A

  The present inventors have found that when a urea compounding agent is filled in a tube internally coated with a general epoxy phenol-based resin, it is colored over time and the commercial value is lowered.

  An object of the present invention is to provide a preparation containing urea, which contains substantially no surfactant and prevents coloration when filled in a container which is internally coated with an epoxy phenol resin.

  As a result of intensive studies to solve the above problems, the present inventors have found that specific oil components of urea, partially saponified polyvinyl alcohol having a saponification degree of 70 to 96 mol%, and carboxyvinyl polymer of 40 wt% or less based on the total amount of the composition. O / W emulsion composition obtained by adjusting pH to 3.5 to 8.5 prevents coloring over time even when filled in an epoxy phenolic resin-coated container The present invention was completed by finding out what can be done.

That is, the present invention comprises (1) a) urea b) partially saponified polyvinyl alcohol having a saponification degree of 70 to 96 mol%,
c) a carboxyvinyl polymer, and d) an oil component that is 40% by mass or less based on the total amount of the content, and 60% by mass or more of the oil component contained is a liquid oil,
O / W emulsion-containing preparation characterized in that a content of O / W emulsion having a pH of 3.5 to 8.5 is filled in a container coated with an epoxy phenol resin on the inner surface. .
(2) The O / W emulsion-containing preparation according to (1), wherein the compounding amount of urea is 1 to 30% by mass of the total amount of the composition.
(3) The O / W emulsion-containing preparation according to (1) or (2), which is substantially free of a surfactant.
(4) The O / W emulsion-containing preparation according to (1), wherein the liquid oil is a polar liquid oil.
(5) The O / W emulsion-containing preparation according to (4), wherein the polar liquid oil is a synthetic oil having an IOB value of 0.1 or more.
(6) The O / W emulsion-containing preparation according to (4), wherein the polar liquid oil is a vegetable oil mainly composed of fatty acid triglycerides.
(7) The O / W emulsion-containing preparation according to any one of (1) to (6), which is a composition for external use.
(8) The O / W emulsion-containing preparation according to any one of (1) to (7), further comprising a polyol.
It is.

  The preparation of the present invention is a urea that is excellent in preparation preparation, has a good feeling of use, does not substantially contain a surfactant, and can prevent coloring even when filled in a container internally coated with an epoxy phenol resin. It was a blended formulation.

  The “partially saponified polyvinyl alcohol” in the present invention means a partially saponified polyvinyl acetate obtained by polymerizing vinyl acetate. For example, the viscosity of a 4% aqueous solution is 4.8 to 5.8 mPa · s. There are several types with different viscosities, such as 20.5 to 24.5 mPa · s, 27.0 to 33.0 mPa · s, 40.0 to 46.0 mPa · s. Regardless of the viscosity, if a saponification degree generally used is 70 to 96 mol%, a stable O / W emulsion can be produced. From the viewpoints of formulation and usability, partially saponified polyvinyl alcohol having a saponification degree of 78 to 96 mol% is preferable, and partially saponified polyvinyl alcohol having a saponification degree of 85 to 90 mol% is particularly preferable. Polyvinyl alcohol having a saponification degree of 97 mol% or more, which is generally referred to as fully saponified polyvinyl alcohol, is distinguished from partially saponified polyvinyl alcohol in the present invention.

  The amount of the partially saponified polyvinyl alcohol is 0.1 to 4.0% by mass, preferably 0.2 to 3.0% by mass, based on the total amount of the composition. The blending amount of partially saponified polyvinyl alcohol can be appropriately adjusted and blended depending on other blending components and purpose of use. For example, in the case of an external cream or lotion for skin, 0.5 to It is preferable to mix | blend so that it may become 2.0 mass%.

  The “carboxyvinyl polymer” in the present invention means a copolymer of acrylic acid. For example, a 0.5% aqueous solution has a viscosity of 4000 to 10000 mPa · s, 40000 to 60000 mPa · s, etc. There are types, but in the present invention, they can be properly used depending on the purpose of use. For example, when making an external cream for skin, it is preferable to mainly use a type having a high viscosity, and when using a lotion, it is preferable to mainly use a type having a low viscosity.

  The blending amount of the carboxyvinyl polymer is 0.1 to 3.0% by mass with respect to the total amount of the composition, and preferably 0.3 to 2.0% by mass in terms of the formulation. A highly resistant O / W emulsion can be obtained.

  The compounding quantity of the oil component of this invention is 40 mass% or less with respect to the whole quantity of the content, and 60 mass% or more of the oil component to contain needs to be liquid oil. If the oil component exceeds 40 wt% with respect to the total amount of the composition, the oil component is separated and an emulsion cannot be prepared. Furthermore, when the ratio of the liquid oil in the oil component is less than 60 wt%, properties and stability are deteriorated. In terms of formulation, the oil component is more preferably 35 wt% or less based on the total amount of the composition.

  As a compounding quantity of urea, it is 1-30 mass% of the whole composition amount, Preferably it is 3-20 mass%.

  In addition, the “oil component” in the present invention means any of liquid oil, solid fat, and a mixture thereof, preferably liquid oil. “Liquid oil” means both non-polar and polar oils that are liquid at 25 ° C. The liquid oil is preferably a polar liquid oil. The polar liquid oil is preferably a synthetic oil having an IOB value (Inorganic Organic Balance value) of 0.1 or more, or a vegetable oil mainly composed of fatty acid triglycerides.

  The IOB value here is calculated based on [Yoshio Koda, “Organic Conceptual Diagram-Fundamentals and Applications”, Sankyo Publishing (1984)], and it is calculated by inorganic value / organic value. It is a numerical value.

  The oil component includes, for example, liquid paraffin and synthetic squalane as nonpolar liquid oil, and examples of polar liquid oil include medium chain fatty acid triglyceride, octyldodecyl myristate, cetyl isooctanoate, isopropyl myristate, Diglyceryl triisostearate, glyceryl tri (capryl / caprate), glyceryl tri-2-ethylhexanoate, diisopropyl sebacate, tri-2-ethylhexyl citrate, diisopropyl adipate, propylene glycol monocaprylate, diethyl sebacate, isostearic acid 2-hexyldecyl, isopropyl palmitate, isopropyl linoleate, ethyl linoleate, triethylhexanoin, propylene glycol dicaprylate, butylethylpropane ethylhexanoate Diol, isocetyl myristate, butyl myristate, cetyl ethyl hexanoate, ethyl oleate, ethyl hexyl palmitate, isopropyl istearate, ethyl hexyl stearate, octyldodecyl neopentanoate, propylene glycol dicaprate, pentaerythrityl tetraethyl hexanoate, dicaprylic acid Propylene glycol, trimethylolpropane triethylhexanoate, trimethylolpropane triisostearate, dibutyloctyl sebacate, diisostearyl malate, isocetyl stearate, isostearyl palmitate, octyldodecanol, hexyldecanol, oleyl alcohol, isostearyl alcohol, Olive oil, almond oil, safflower oil, castor oil, corn oil Avocado oil, persic oil, cucumber nut oil, grape seed oil, pistachio seed oil, hazelnut oil, macadamia nut oil, meadow foam oil, rosehip oil, sunflower oil, soybean oil, jojoba oil or oleic acid, solid fat Examples thereof include solid paraffin, white petrolatum, myristyl myristate, cetyl palmitate, stearyl alcohol, cetanol, cetostearyl alcohol, behenyl alcohol, stearic acid, myristic acid, hard fat, jojoba wax, and cocoa butter.

  The oil component is particularly preferably cetyl isooctanoate, isopropyl myristate, diglyceryl triisostearate, glyceryl tri (capryl / caprate), glyceryl tri-2-ethylhexanoate, diisopropyl sebacate, tri-2-ethylhexyl citrate, Diisopropyl adipate, propylene glycol monocaprylate, diethyl sebacate, 2-hexyldecyl isostearate, isopropyl palmitate, isopropyl linoleate, ethyl linoleate, triethylhexanoin, propylene glycol dicaprylate, butylethylpropanediol ethylhexanoate , Isocetyl myristate, butyl myristate, cetyl ethylhexanoate, ethyl oleate, ethyl hexyl palmitate, ethyl isostearate Propyl, ethylhexyl stearate, octyldodecyl neopentanoate, propylene glycol dicaprate, pentaerythrityl tetraethylhexanoate, propylene glycol dicaprylate, trimethylolpropane triethylhexanoate, trimethylolpropane triisostearate, dibutyloctyl sebacate and dibutyl malate A liquid synthetic oil having an IOB value of 0.1 or more selected from isostearyl, or olive oil, almond oil, safflower oil, castor oil, corn oil, avocado oil, persic oil, kukui nut oil, grape seed oil, pistachio seed oil, It is a liquid vegetable oil mainly composed of fatty acid triglycerides selected from hazelnut oil, macadamia nut oil, meadow foam oil, rosehip oil, sunflower oil and soybean oil.

  These oil components can be used alone or in combination of two or more.

  The O / W emulsion of the present invention preferably has a pH adjusted to 3.5 to 8.5. When the pH value is less than 3.5, the emulsion stability is deteriorated and the desired O / W emulsion cannot be obtained. Further, when the O / W emulsion of the present invention is used for skin, there is a concern that irritation to the skin may occur when the pH exceeds 8.5, which is not suitable for skin. From the viewpoint of formulation, it is more preferable to adjust the pH to 4.5 to 8.0.

  The pH adjuster is not particularly limited, and a basic compound blended in ordinary pharmaceuticals and cosmetics can be used. Examples thereof include diisopropanolamine, triisopropanolamine, sodium hydroxide, monoethanolamine, diethanolamine, triethanolamine, triethylamine, potassium hydroxide, and sodium citrate. In adjusting the pH, these pH adjusting agents can be used alone or in combination of two or more.

  The “external composition” in the present invention can be a dosage form generally used when an O / W emulsion is applied to the skin, such as cream, lotion, ointment, gel, aerosol and the like.

  Furthermore, when a polyol is further added to the O / W emulsion of the present invention, the excellent feeling of use of the emulsion can be maintained. The polyol that can be used in the present invention is not particularly limited, and for example, 1,3-butylene glycol, propylene glycol, dipropylene glycol, glycerin, and polyethylene glycol can be used. When blending a polyol with the O / W emulsion of the present invention, one or more of these polyols can be blended.

  Further, in the present invention, “substantially does not contain a surfactant” means that a surfactant is not added or an amount that does not sufficiently exert a surfactant effect is added. .

  Here, the surfactant means a compound having a hydrophilic group and a hydrophobic group, which usually dissolves in water and greatly changes properties such as surface tension, and at the same time forms aggregates such as micelles in water. .

  The O / W emulsion of the present invention can be produced according to a general emulsion production method. For example, carboxyvinyl polymer is dispersed in purified water and heated. Separately, polyvinyl alcohol is dissolved in purified water and urea is further dissolved. These two aqueous solutions are combined into an aqueous phase. Separately, polar oil (add polyol if necessary) is heated and dissolved to obtain an oil phase. The target O / W emulsion composition can be obtained by adding the oil phase to the aqueous phase, further adding purified water and stirring until uniform, and further cooling to room temperature while stirring. When blending a pH adjuster, a suitable amount is dissolved in the oil phase or the final purified water.

  The O / W emulsion composition of the present invention can be stored stably for a long period of time and does not need to contain a surfactant even when it is filled in a container whose inner surface is coated with an epoxyphenol resin. Therefore, it can be made into an emulsion with little irritation when used on the skin. Furthermore, the extension is light and the feel after use is excellent.

  In addition, the O / W emulsion composition of the present invention may contain an active ingredient other than urea and various base ingredients that can be contained in pharmaceuticals, quasi-drugs, and cosmetics as long as the intended effect is not impaired. it can.

  Active ingredients include, for example, anti-inflammatory agents (indomethacin, piroxicam, diclofenac sodium, felbinac, hydrocortisone acetate, dexamethasone acetate, etc.), analgesics, antihistamines (diphenhydramine, chlorpheniramine maleate, isothipentyl hydrochloride, etc.), local anesthetics ( Lidocaine, procaine, dibucaine, lidocaine hydrochloride, procaine hydrochloride, dibucaine, etc.), tissue repair agents, antipruritic agents (crotamiton, etc.), moisturizers (hyaluronic acid, ceramide, etc.), cooling agents (menthol, camphor, etc.), vitamins and Derivatives (vitamin A, vitamin B, vitamin C, vitamin E, etc.), vasoconstrictors (tetrahydrozoline hydrochloride, phenylephrine hydrochloride, etc.), whitening agents, antibacterial agents, antiallergic agents, antiviral agents, antifungal agents (miconazo nitrate) , Terbinafine hydrochloride, bifonazole, hydrochloric neticonazole, butenafine hydrochloride, Riranafutato, luliconazole, etc.), oxygen scavenger, ultraviolet absorbers or ultraviolet light scattering agents.

  Examples of the base component include solubilizing agents such as lower alcohols (ethanol, isopropanol, etc.), hydrocarbons, wax components, antioxidants (dibutylhydroxytoluene, etc.), emulsion stabilizers, gelling agents (methylcellulose, Hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, sodium alginate, xanthan gum, polyvinylpyrrolidone, etc.), thickeners, adhesives, extracts from various animals and plants, preservatives (parahydroxybenzoic acid esters, benzyl alcohol, phenoxyethanol) Etc.), chelating agents (such as sodium edetate), fragrances, dyes or liquefied gases.

Examples Hereinafter, the present invention will be described in more detail with reference to Examples, Comparative Examples, and Test Examples. Unless otherwise specified, Carbopol 980 manufactured by Noveon is used as the carboxyvinyl polymer, Panacet 810 manufactured by Nippon Oil & Fats is used as the medium chain fatty acid triglyceride, and Gohsenol EG-05 manufactured by Nippon Synthetic Chemical Industry is used as the partially saponified polyvinyl alcohol. (Saponification degree: 86.5 to 89.0 mol%) was used.

Urea 10w / w%
Medium chain triglyceride 13w / w%
Carboxyvinyl polymer 0.5w / w%
Partially saponified polyvinyl alcohol 1w / w%
1,3-butylene glycol 10w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
pH 7.5
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.0 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 10 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 13 g of medium chain fatty acid triglyceride and 10 g of 1,3-butylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. An oil phase was added to the aqueous phase, and further diisopropanolamine (appropriate amount) dissolved in the remaining purified water was added. After stirring until uniform, the mixture was cooled to room temperature with stirring to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 10w / w%
Octyldodecyl myristate 13w / w%
Carboxyvinyl polymer 0.5w / w%
Partially saponified polyvinyl alcohol 1w / w%
1,3-butylene glycol 10w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
pH 7.5
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.0 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 10 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 13 g of octyldodecyl myristate and 10 g of 1,3-butylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. An oil phase was added to the aqueous phase, and further diisopropanolamine (appropriate amount) dissolved in the remaining purified water was added. After stirring until uniform, the mixture was cooled to room temperature with stirring to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 10w / w%
Liquid paraffin 13w / w%
Carboxyvinyl polymer 0.5w / w%
Partially saponified polyvinyl alcohol 1w / w%
1,3-butylene glycol 10w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
pH 7.5
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.0 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 10 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 13 g of liquid paraffin and 10 g of 1,3-butylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. An oil phase was added to the aqueous phase, and further diisopropanolamine (appropriate amount) dissolved in the remaining purified water was added. After stirring until uniform, the mixture was cooled to room temperature with stirring to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 10w / w%
Stearyl alcohol 2w / w%
Medium chain triglyceride 14w / w%
Carboxyvinyl polymer 0.5w / w%
Partially saponified polyvinyl alcohol 1w / w%
1,3-butylene glycol 10w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
pH 7.3
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.0 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 10 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 2 g of stearyl alcohol, 14 g of medium chain fatty acid triglyceride and 10 g of 1,3-butylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. An oil phase was added to the aqueous phase, and further diisopropanolamine (appropriate amount) dissolved in the remaining purified water was added. After stirring until uniform, the mixture was cooled to room temperature with stirring to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 30w / w%
Medium chain triglyceride 12w / w%
Carboxyvinyl polymer 0.5w / w%
Partially saponified polyvinyl alcohol 1w / w%
1,3-butylene glycol 5w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
pH 7.1
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.0 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 30 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 12 g of medium chain fatty acid triglyceride and 5 g of 1,3-butylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. An oil phase was added to the aqueous phase, and further diisopropanolamine (appropriate amount) dissolved in the remaining purified water was added. After stirring until uniform, the mixture was cooled to room temperature with stirring to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 20w / w%
Hexyl decanol 3w / w%
Isopropyl myristate 12w / w%
Carboxyvinyl polymer 0.8w / w%
Partially saponified polyvinyl alcohol 1.2w / w%
Propylene glycol 5w / w%
Sodium hydroxide appropriate amount purified water 100w / w%
pH 6.0
Carboxyvinyl polymer 0.8g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.2 g of polyvinyl alcohol was dissolved in 20 g of purified water heated to about 70 ° C., and 20 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 12 g of isopropyl myristate, 3 g of hexyldecanol and 5 g of propylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. After adding the oil phase to the aqueous phase and stirring, a solution in which sodium hydroxide (appropriate amount) was dissolved in the remaining purified water was added, and the mixture was cooled to room temperature while stirring until further uniform to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 20w / w%
Isopropyl myristate 12w / w%
Carboxyvinyl polymer 0.4w / w%
Partially saponified polyvinyl alcohol 1.0 w / w%
Propylene glycol 7w / w%
Triethanolamine appropriate amount purified water 100w / w%
pH 5.0
0.4 g of carboxyvinyl polymer was dispersed in 20 g of purified water and heated to about 70 ° C. Separately, 1.0 g of polyvinyl alcohol was dissolved in 20 g of purified water heated to about 70 ° C., and 20 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 12 g of isopropyl myristate and 7 g of propylene glycol were heated to about 70 ° C. and dissolved to obtain an oil phase. After adding the oil phase to the aqueous phase and stirring, a mixture of triethanolamine (appropriate amount) mixed with the remaining purified water was added, and the mixture was cooled to room temperature while stirring until it became more uniform to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 5w / w%
Isopropyl myristate 12w / w%
Squalane 1w / w%
Carboxyvinyl polymer 0.5w / w%
Partially saponified polyvinyl alcohol 1.0 w / w%
Triethanolamine appropriate amount purified water 100w / w%
pH 7.0
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.0 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 5 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 12 g of isopropyl myristate and 1 g of squalane were heated to about 70 ° C. and dissolved to obtain an oil phase. After adding the oil phase to the aqueous phase and stirring, a solution in which triethanolamine (appropriate amount) was dissolved in the remaining purified water was added, and the mixture was cooled to room temperature while stirring until further uniform to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 10w / w%
l-Menthol 1w / w%
Medium chain triglyceride 11w / w%
Diisopropyl adipate 4w / w%
Carboxyvinyl polymer 0.5w / w%
Hydroxypropyl methylcellulose 0.05w / w%
Partially saponified polyvinyl alcohol 1.2w / w%
1,3-butylene glycol 10w / w%
Sodium hydroxide appropriate amount purified water 100w / w%
pH 6.5
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC. Separately, 1.2 g of polyvinyl alcohol was dissolved in 15 g of purified water heated to 70 ° C., and 10 g of urea was further dissolved. Further, 0.05 g of hydroxypropylmethylcellulose was swollen in 10 g of purified water heated to 70 ° C., and the three aqueous solutions were combined to form an aqueous phase. Separately, 11 g of medium chain fatty acid triglyceride, 4 g of diisopropyl adipate and 10 g of 1,3-butylene glycol were heated to about 70 ° C., and 1 g of 1-menthol was dissolved to obtain an oil phase. The oil phase was added to the aqueous phase, and sodium hydroxide (appropriate amount) dissolved in the remaining purified water was added. The mixture was stirred until uniform, and then cooled to room temperature with stirring to obtain a cream. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Urea 20w / w%
Isopropyl methylphenol 0.1w / w%
dl-Camphor 0.5w / w%
Medium chain triglyceride 12w / w%
Liquid paraffin 1w / w%
Carboxyvinyl polymer 0.6w / w%
Partially saponified polyvinyl alcohol 1.2w / w%
1,3-butylene glycol 8w / w%
Ethyl parahydroxybenzoate 0.1w / w%
Propyl parahydroxybenzoate 0.1 w / w%
Dibutylhydroxytoluene 0.1w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
pH 7.0
0.6 g of carboxyvinyl polymer was dispersed in 25 g of purified water and heated to about 70 ° C. Separately, 1.2 g of polyvinyl alcohol was dissolved in 25 g of purified water heated to about 70 ° C., and 20 g of urea was further dissolved. The two aqueous solutions were combined into an aqueous phase. Separately, 12 g of medium-chain fatty acid triglyceride and 1 g of liquid paraffin were heated to about 70 ° C., and 0.5 g of dl-camphor, 0.1 g of dibutylhydroxytoluene and 0.1 g of parahydroxybenzoate were dissolved to obtain an oil phase. Further, 8 g of 1,3-butylene glycol was heated to about 70 ° C., and 0.1 g of isopropylmethylphenol was dissolved to obtain a polyol phase. After adding the oil phase and polyol phase to the aqueous phase in this order, add diisopropanolamine (appropriate amount) and 0.1 g of ethyl parahydroxybenzoate dissolved in the remaining purified water, and stir until uniform. While cooling to room temperature, a cream was obtained. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Comparative Example 1
Urea 10w / w%
Medium chain triglyceride 13w / w%
Carboxyvinyl polymer 0.5w / w%
Polysorbate 60 1w / w%
1,3-butylene glycol 10w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
A cream was obtained in the same manner as in Example 1. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Comparative Example 2
Medium chain triglyceride 13w / w%
Carboxyvinyl polymer 0.5w / w%
Polysorbate 60 1w / w%
1,3-butylene glycol 10w / w%
Diisopropanolamine appropriate amount purified water 100w / w%
A cream was obtained in the same manner as in Example 1. The cream agent was filled in an aluminum tube (Z-1: Ikeda Kogyo Co., Ltd.) coated on the inner surface with an epoxy phenol resin.

Test Example 1 Stability Test Polysorbate 60 (polyoxyethylene monostearate) as a surfactant instead of the creams of Examples 1 to 3 of the present invention and the polyvinyl alcohol (partial saponification) of Example 1 as Comparative Example 1 Aluminum tube (Z-1: Ikeda) in which each cream was internally coated with an epoxy phenol resin using a cream prepared using sorbitan) and a cream obtained by removing urea from the formulation of Comparative Example 1 as Comparative Example 2. The properties (appearance) were evaluated immediately after production and after storage at a temperature of 65 ° C. for 2 weeks. The results are shown in Table 1.

  Immediately after production, each cream was white. After storage at a temperature of 65 ° C. for 2 weeks, the creams of Examples 1 to 3 of the present invention remained white and were not colored. However, the cream of Comparative Example 1 was changed to yellowish. The cream of Comparative Example 2 containing no urea was white even after storage.

  In the following reference test examples, the type of compounding component in the base formulation and the change in the formulation due to the change in the blending amount were observed.

Reference Test Example 1 (Prototype test for changing oil component of base formulation)
0.5 g of carboxyvinyl polymer was dispersed in 25 g of purified water and heated to about 70 ° C. to obtain an aqueous solution. Further, 1 g of partially saponified polyvinyl alcohol (saponification degree: 86.5 to 89.0 mol%) was dissolved in 25 g of purified water heated to about 70 ° C. to obtain an aqueous solution. The two aqueous solutions were combined into an aqueous phase. Separately, a mixture of 13 g of medium chain fatty acid triglyceride and 10 g of 1,3-butylene glycol was heated to about 70 ° C., and diisopropanolamine (appropriate amount) was dissolved to obtain an oil phase. The oil phase was added to the aqueous phase, the remaining purified water was further added, and the mixture was stirred until uniform, and then cooled to room temperature with stirring to obtain a cream. This was the basic prescription. The pH was adjusted to 5-7.

(1) Medium chain fatty acid triglyceride modified formulation The medium chain fatty acid triglyceride in the above basic formulation is paraffin, white petrolatum (semi-solid), liquid paraffin, synthetic squalane, cetyl palmitate, myristyl myristate, behenyl alcohol, cetanol, batyl alcohol, Octyldodecyl myristate, cetyl isooctanoate, isopropyl myristate, diglyceryl triisostearate, glyceryl tri (capryl / caprate), glyceryl tri-2-ethylhexanoate, diisopropyl sebacate, tri-2-ethylhexyl citrate, diisopropyl adipate , Propylene glycol monocaprylate, olive oil, almond oil or castor oil were replaced with creams by the same operation as the above basic formula .

(2) Extraction prescription In the above basic prescription, a modified prescription excluding medium chain fatty acid triglycerides was prepared in the same manner as the above basic prescription.

  In these modified formulations, it was confirmed whether it was possible to prepare a uniform preparation with a good feeling of use. Visual confirmation work was performed by three people. The results are shown in Table 2. The 65 ° C / 2W term confirmed the properties after 65 ° C 2W.

  The uncut formulation failed to prepare an emulsion composition.

Reference Test Example 2 (Base-form compounding amount change test)
0.5 g of carboxyvinyl polymer was dispersed in 25 g of purified water and heated to about 70 ° C. to obtain an aqueous solution. Further, 1 g of partially saponified polyvinyl alcohol (saponification degree: 86.5 to 89.0 mol%) was dissolved in 25 g of purified water heated to about 70 ° C. to obtain an aqueous solution. The two aqueous solutions were combined into an aqueous phase. Separately, a mixture of 13 g of medium chain fatty acid triglyceride and 10 g of 1,3-butylene glycol was heated to about 70 ° C., and diisopropanolamine (appropriate amount) was dissolved therein to obtain an oil phase. The oil phase was added to the aqueous phase, the remaining purified water was further added, and the mixture was stirred until uniform, and then cooled to room temperature with stirring to obtain a cream. This was the basic prescription. The pH was adjusted to 5-7.

Next, the following recipe for changing the blending amount was prepared.
(1) Partially saponified polyvinyl alcohol (saponification degree 86.5 to 89.0 mol%) blending amount change test The modified prescription of the partial saponified polyvinyl alcohol (saponification degree 86.5 to 89.0 mol%) blending amount in the above basic formulation is the same as the above basic formulation To make a cream.

  It was confirmed whether or not it was possible to prepare a uniform preparation with a good feeling of use in the partially modified polyvinyl alcohol blending amount changing formulation. Visual confirmation work was performed by three people. The results are shown in Table 3. “◯” in the “preparation” section in the table indicates that a uniform preparation could be prepared, “Δ” indicates that slight separation was observed, and “x” indicates that uniform preparation was not possible. ○ in the term of use feeling indicates that the preparation has good elongation and good use feeling, and Δ indicates that the product is slightly sticky.

  The 65 ° C / 2W term confirmed the properties after 65 ° C 2W. ○ indicates that there was no change immediately after preparation.

(2) Carboxyvinyl polymer blending amount change test The modified formulation of the carboxyvinyl polymer blending amount in the basic formulation was treated in the same manner as the basic formulation to obtain a cream.

  In the carboxyvinyl polymer blending amount changing formulation, it was confirmed whether or not it was possible to prepare a uniform preparation with a good feeling of use. Visual confirmation work was performed by three people. The results are shown in Table 4. In the preparation section of the table, ○ indicates that it was able to be prepared uniformly, Δ indicates that slight separation was observed, and × indicates that it was not possible to prepare uniformly. ○ in the term of use feeling indicates that the preparation has good elongation and good use feeling, and Δ indicates that the product is slightly sticky.

  The 65 ° C / 2W term confirmed the properties after 65 ° C 2W. ○ indicates that there was no change immediately after preparation, and Δ indicates that it was slightly non-uniform.

(3) Oil blending amount change test A modified formulation of the oil component blending amount in the basic formulation was made into a cream by the same operation as the basic formulation.

  It was confirmed whether or not it was possible to prepare a uniform preparation with a good feeling of use in the oil blending amount changing formulation. Visual confirmation work was performed by three people. The results are shown in Table 5. ○ in the section of preparation / use feeling in the table indicates that the preparation can be uniformly prepared and has good elongation and good use feeling. Δ indicates that a slight separation was observed and a slight stickiness was felt. X shows that it was not able to prepare uniformly.

  As a result of the 65 ° C./2 W transformation test for the preparations with all the items ○, all the properties were not changed.

Reference Test Example 3 (pH test for base formulation)
Carboxyvinyl polymer 0.5g was disperse | distributed to 25g of purified water, and it heated to about 70 degreeC, and obtained the water solution. Further, 1 g of partially saponified polyvinyl alcohol (saponification degree: 86.5 to 89.0 mol%) was dissolved in 25 g of purified water heated to about 70 ° C. to obtain an aqueous solution. The two aqueous solutions were combined into an aqueous phase. Separately, a mixture of 13 g of medium chain fatty acid triglyceride and 10 g of 1,3-butylene glycol was heated to about 70 ° C., and diisopropanolamine (appropriate amount) was dissolved therein to obtain an oil phase. The oil phase was added to the aqueous phase, the remaining purified water was further added, and the mixture was stirred until uniform, and then cooled to room temperature with stirring to obtain a cream. This was the basic prescription.

  Next, the blending amount of diisopropanolamine was changed to change the pH of the preparation.

  In these formulations, it was confirmed whether it was possible to prepare a uniform preparation with a good feeling of use. Visual confirmation work was performed by three people. The results are shown in Table 6. In the table, “◯” in the “preparation” section indicates that the preparation was uniform, and “×” indicates that the preparation was not uniform.

  The 65 ° C / 2W term confirmed the properties after 65 ° C 2W. ○ indicates that there was no change immediately after preparation.

Reference Test Example 4 (Liquid oil blending amount change test with respect to total oil content of base formulation)
0.5 g of carboxyvinyl polymer was dispersed in 25 g of purified water and heated to about 70 ° C. to obtain an aqueous solution. Further, 1 g of partially saponified polyvinyl alcohol (saponification degree: 86.5 to 89.0 mol%) was dissolved in 25 g of purified water heated to about 70 ° C. to obtain an aqueous solution. The two aqueous solutions were combined into an aqueous phase. Separately, a mixture of 13 g of medium chain fatty acid triglyceride and 10 g of 1,3-butylene glycol was heated to about 70 ° C., and diisopropanolamine (appropriate amount) was dissolved therein to obtain an oil phase. The oil phase was added to the aqueous phase, the remaining purified water was further added, and the mixture was stirred until uniform, and then cooled to room temperature with stirring to obtain a cream. This was the basic prescription. The pH was adjusted to 5-7.

  Using the medium chain triglyceride as the liquid oil and the solid fat cetanol as the remaining oil component, the liquid oil in the total oil component The same procedure as in the above basic formulation was performed to obtain a cream.

  In these modified formulations, it was confirmed whether it was possible to prepare a uniform preparation with a good feeling of use. Visual confirmation work was performed by three people. The results are shown in Table 7. ○ in the section of preparation in the table indicates that preparation was uniform. ○ in the item of the property indicates that a uniform preparation was obtained, Δ indicates that it was slightly non-uniform, and x indicates that it was non-uniform. ○ in the feeling of use indicates that the preparation had good usability, Δ indicates that a slight roughness was felt, and × indicates that a roughness was felt.

  The 65 ° C / 2W term confirmed the properties after 65 ° C 2W. ○ indicates that there was no change immediately after preparation.

  Since the preparation of the present invention can be sealed in containers such as general tubes, bottles, and aerosol cans, it can be used for pharmaceuticals, quasi drugs, cosmetics, and the like.

Claims (7)

a) urea of 3 to 20% by mass of the total amount of the composition b) partially saponified polyvinyl alcohol having a saponification degree of 70 to 96 mol% of 0.2 to 3.0% by mass of the total amount of the composition ,
c) 0.3 to 2.0% by mass of the total amount of the carboxyvinyl polymer, and d) 40% by mass or less based on the total amount of the contents, and 60% by mass or more of the oil component contained Oil components that are liquid oils,
O / W emulsion-containing preparation characterized in that a content of O / W emulsion having a pH of 3.5 to 8.5 is filled in a container coated with an epoxy phenol resin on the inner surface. .   2. The O / W emulsion-containing preparation according to claim 1, which is substantially free of a surfactant. The O / W emulsion-containing preparation according to claim 1 or 2 , wherein the liquid oil is a polar liquid oil. The O / W emulsion-containing preparation according to claim 3 , wherein the polar liquid oil is a synthetic oil having an IOB value of 0.1 or more. The O / W emulsion-containing preparation according to claim 3 , wherein the polar liquid oil is a vegetable oil containing fatty acid triglyceride as a main component. It is an external composition, The O / W type emulsion containing formulation of any one of Claims 1-5 . Furthermore, the O / W type emulsion containing formulation of any one of Claims 1-6 which mix | blended the polyol.