JP2017078055A - Water-in-oil emulsion composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a water-in-oil emulsion composition having high emulsion stability, free from release oil, and having a good feeling in use.SOLUTION: The present invention provides a water-in-oil emulsion composition comprising (A)-(E): (A) lipophilic surfactant, (B) lecithin, (C) oily gelator, (D) high polymer silicone, and (E) oil solution.SELECTED DRAWING: None

Description

  The present invention relates to a water-in-oil emulsion composition having excellent stability and usability.

It is known that poly (12-hydroxystearic acid) ester of polyhydric alcohol is suitable for the production of a low-viscosity emulsion composition having excellent fluidity at high and low temperatures (Non-Patent Document 1: FRAGRANCE JOURNAL September 1999). Since the poly (12-hydroxystearic acid) ester of polyhydric alcohol itself is not light and sticky, the oily water-in-oil emulsion composition for cosmetics, which tends to be avoided in any case because it is oily and heavy. It is widely used as an emulsifier. Patent Document 1 (Japanese Patent No. 4146969) discloses a multi-layer emulsifier type skin external preparation containing a poly (12-hydroxystearic acid) ester of a polyhydric alcohol.
In general, in a water-in-oil emulsion composition, dispersed water phase particles do not have an electric charge, so that coalescence is prevented by electrostatic repulsion between emulsified particles and stabilization cannot be achieved. For this reason, for the problem of precipitation and separation in the emulsion composition, the outer phase (oil phase) is thickened with a thickener, or the interface is strengthened by using a plurality of emulsifiers (the increase in viscosity is not much). That cannot be expected).

As an example of blending a thickener, an oil containing water containing a poly (12-hydroxystearic acid) ester and triacylglycerol 1 to 50% by mass and a fructooligosaccharide fatty acid ester as a thickening gelling agent, and water A water-in-water emulsified composition has been proposed (Patent Document 2: Japanese Patent No. 4676634). However, this emulsified composition still has problems in use feeling such as stickiness.
In addition, poly (12-hydroxystearic acid) ester of polyhydric alcohol, water-in-oil emulsified cosmetics using phospholipid as a different type of emulsifier and glyceryl (behenic acid / eicosanedioic acid) glyceryl as an oily gelling agent A fee has been proposed (Patent Document 3: Japanese Patent No. 5572356). Although this emulsified cosmetic partially improves the feeling of use, the skin feel and firmness are not sufficient as a cosmetic. Furthermore, the stability at high temperatures is unknown.
A water-in-oil emulsified cosmetic containing an oil component, poly (12-hydroxystearic acid) ester of a polyhydric alcohol, a specific silicone oil, and an organically modified clay mineral that is an oily gelling agent has also been proposed. (Patent Document 4: Japanese Patent No. 3993505). It is described that this emulsified cosmetic was stable at 50 ° C. However, nothing is described about oil release in cream form, and the feeling of use is not sufficient.
Further, Non-Patent Document 1 shown above shows water in oil when poly (12-hydroxystearic acid) ester of polyhydric alcohol is excessively mixed to increase the volume ratio of the inner aqueous phase (90%). It is described that the viscosity of the mold emulsion composition increases. However, the water-in-oil emulsified composition with a high inner water phase is a composition that has a unique splash feeling (feeling that the inner water phase bounces at the time of application) and does not have a natural feeling of conforming to the skin, and has an excellent feeling of use. It's hard to say.

  Among water-in-oil emulsion compositions, cream-type cosmetics and external preparations are sold in tube containers or jar containers. However, a cream type with a high viscosity often entrains air when the emulsified composition is filled in a tube container or a jar container, resulting in a void inside. When the cream type with such voids is stored at high temperature or when stored for a long period of time, the oil contained in the oil phase separates and accumulates in the voids (hereinafter referred to as “oil separation”). May occur. Unlike the emulsion stability, this oil separation is due to the instability of the structure and composition constituting the oil phase. The oil separation generated in the gap is easily recognized as a defective product, which causes a problem in design quality.

The basic composition of a water-in-oil emulsified cream is an oil, an emulsifier, an oily gelling agent, and water. In cosmetics, an oily gelling agent is blended not only for the purpose of increasing the viscosity of the composition but also for improving the feeling of use. In cosmetics used locally, such as a cream for the eyes, use feelings such as “feeling of firmness”, “feeling of skin familiarity”, and “feeling of thickness” are important design items. In order to realize the feeling of use, the combination of the oily gelling agent, the emulsifier and the oil becomes complicated.
The oil separation occurs when the compatibility of these components is not good. In the oil phase, various oil agents are present together with the oily gelling agent. At this time, if the oil agent is held in a network having a network structure formed by the oily gelling agent, the composition is stable and does not cause quality problems. However, when the oily gelling agent particles and molecules are attracted to each other under high temperature and long-term storage, the network structure network is disturbed, and if the mesh interval becomes close, the oil agent can no longer be held in the network structure network. . Then, the oil agent that can no longer be held is pushed out of the network structure of the oil phase, resulting in “oil separation”. Therefore, in terms of quality design, it also has a “feeling of smoothness”, a “feeling of stickiness”, and a “feeling of thickness” while also having a “feeling of smoothness” and “feeling of non-stickiness” that are the basic feeling of use of cosmetics. To achieve this, combining multiple different oil phase components such as oil-based gelling agents, silicone and hydrocarbon oils to achieve a complex feeling of use, the balance in the oil phase is lost, and "oil separation" tends to occur. Become. In particular, the preferred feeling of use required for topical water-in-oil emulsified creams and the suppression of “oil separation” were difficult problems for cosmetic formulation designers.
As prior art for solving such oil separation, there are, for example, Patent Document 5 (Japanese Patent Laid-Open No. 2007-153812) and Patent Document 6 (Japanese Patent Laid-Open No. 2013-107827).

Japanese Patent No. 4146969 Japanese Patent No. 4676634 Japanese Patent No. 5572356 Japanese Patent No. 3993505 JP 2007-153812 A JP 2013-107827 A

Fragrance JOURNAL September 1999 pages 83-86

The present applicant has been continuously developing a water-in-oil emulsion composition having excellent usability and stability using poly (12-hydroxystearic acid) ester of a polyhydric alcohol. In particular, the present inventor, as a cosmetic for topical use such as a cream for the eyes, has a preferable basic feeling of use such as “a feeling of smoothness” and “a feeling of non-stickiness”, and further, as a cream for the eyes. We are conducting research and development of water-in-oil cream type emulsified compositions that have the essential feelings of “feeling of firmness”, “feeling of skin familiarity”, and “thickness”. In this process, the present inventor made a polyhydric alcohol poly (12-hydroxystearic acid) ester, a water-in-oil emulsified composition comprising a combination of lecithin, a gelling agent and a highly polymerized silicone in a filled container. Thus, even when voids are formed, oil separation does not occur, and it has been found that the cosmetics have excellent storage stability and usability, and the present invention has been completed.
That is, the present invention has high emulsification stability and excellent basic feel as a cosmetic material, and further has a “feel of firmness”, “feel of skin familiarity”, and “thickness”, and does not cause oil separation. It is an object to provide an aqueous emulsion composition.

The main configuration of the present invention is as follows.
(1) A water-in-oil emulsion composition containing (A) to (E).
(A) Lipophilic surfactant (B) Lecithin (C) Oily gelling agent (D) Highly polymerized silicone (E) Oil agent (2) (A) Poly (12-hydroxy) whose lipophilic surfactant is a polyhydric alcohol The water-in-oil emulsion composition according to (1), which is a stearic acid ester.
(3) (D) When the highly polymerized silicone is dispersed in dimethylpolysiloxane having a kinematic viscosity of 20 mm ² / s by the capillary method at a concentration of 20% by mass, the viscosity by the rotation method is 40000 to 50000 mPa · s. The water-in-oil emulsion composition according to (1) or (2), which is dimethylpolysiloxane.
(4) The water-in-oil emulsion composition according to any one of (1) to (3), wherein (D) the degree of polymerization of the highly polymerized silicone is 8000.
(5) The water-in-oil emulsion composition according to any one of (1) to (4), wherein (C) the oily gelling agent is an organically modified clay mineral.
(6) The water-in-oil emulsion composition according to (5), wherein the organically modified clay mineral is dimethyl distearyl ammonium hectorite.
(7) The water-in-oil emulsion composition according to (5) or (6), further comprising (C) an inulin fatty acid ester and / or a dextrin fatty acid ester as an oily gelling agent.
(8) (E) The oil agent contains at least one from the group consisting of silicone oil and volatile silicone oil, and at least one from the group consisting of ester oil, fat and hydrocarbon oil (1) to (7) The water-in-oil emulsion composition according to any one of the above.
(9) The water-in-oil emulsion composition according to any one of (1) to (8), wherein the viscosity of the composition measured at 25 ° C. with a B-type viscometer is 20000 to 50000 mPa · s.
(10) The water-in-oil emulsion composition according to any one of (1) to (9), which is a cream for the eyes.

  The composition of the present invention has a high emulsification stability and is excellent in a basic feeling of use as a cosmetic, and also has a “feel of firmness”, “feel of skin familiarity”, and “feel of thickness”, and further oil separation occurs. No water-in-oil emulsion composition. Furthermore, the composition of the present invention does not separate in a cycle test (twice 12 hours cycle) at −20 ° C. and room temperature (25 ° C.), and oil is released in the voids even after long-term storage (storage at 50 ° C. for 1 month). It is a composition in which no occurs. In addition, since oil separation does not occur in the gap, the tube container in which there is a risk of occurrence of the gap can be filled and provided. Furthermore, the water-in-oil emulsion composition obtained by the composition of the present invention is “nobita smooth”, “no stickiness”, “smoothness”, “skin feel”, “thickness” Since the feeling of use required for the cream is excellent, it is particularly excellent as a cosmetic for topical use such as the eyes.

The present application relates to a water-in-oil emulsion composition containing (A) a lipophilic surfactant, (B) lecithin, (C) an oily gelling agent, (D) a highly polymerized silicone, and (E) an oil. It is.
Below, the component of this invention is demonstrated.

Essential component [(A): Lipophilic surfactant]
The composition of the present invention is a water-in-oil emulsion composition and needs to contain a lipophilic surfactant. As the lipophilic surfactant, it is preferable to use poly (12-hydroxystearic acid) ester of a polyhydric alcohol from the viewpoint of use feeling.
Poly (12-hydroxystearic acid) ester of polyhydric alcohol used in the present invention is obtained by reacting poly (12-hydroxystearic acid) with a halogenating agent such as thionyl chloride in the presence of an alkali such as polyethylene glycol. It can be obtained by reacting the acid chloride prepared above.
Preferred examples of the polyhydric alcohol include propylene glycol, butanediol, pentanediol, (poly) glycerin, (poly) propylene glycol, and polyethylene glycol. Among these, polyethylene glycol is particularly preferable. The polyethylene glycol in this case preferably has an average molecular weight of 400 to 6000. On the other hand, the poly (12-hydroxystearic acid) serving as a hydrophobic group preferably has an average molecular weight of 1000 to 3000.
The di (12-hydroxystearic acid) ester of polyethylene glycol preferably has the INCI name listed as dipolyhydroxystearic acid PEG-30, and commercially available products include ARACEL P-135, COLDA JAPAN There is cis roll DPHS manufactured by Co., Ltd.
When blending a poly (12-hydroxystearic acid) ester of a polyhydric alcohol, the blending amount is preferably 0.1 to 5% by mass, particularly preferably 1 to 5% by mass. If it is less than 0.1% by mass, emulsification may be insufficient. If it exceeds 5 mass%, there is a risk of having a sticky feel.

[(B): Lecithin]
As the lecithin used in the present invention, natural phospholipids such as egg yolk lecithin and soybean lecithin, hydrogenated soybean lecithin obtained by changing the unsaturated carbon chain in lecithin to a saturated bond by hydrogenation, hydrogenated egg yolk lecithin and the like can be used. In the present specification, these hydrogenated products are collectively referred to as hydrogenated lecithin (hydrogenated lecithin). In the present invention, hydrogenated lecithin is preferably used. In the present invention, lecithin is preferably blended in an amount of 0.1 to 1% by mass.

[(C): Oily gelling agent]
Examples of the oily gelling agent used in the present invention include organically modified clay minerals, dextrin fatty acid esters, inulin fatty acid esters, fine particle silica, hydrogenated castor oil and the like. Among these, it is preferable to mix organically modified clay minerals. In addition, when organic dextrin fatty acid ester and inulin fatty acid ester are used in combination with organically modified viscosity minerals, “thickness”, “smooth feeling of smoothness”, “feel of non-stickiness”, “feeling of skin comfort”, “feeling of firmness” "Is improved, which is preferable. The organically modified clay mineral is obtained by modifying a clay mineral with a quaternary ammonium salt type cationic surfactant. For example, organic modified bentonite, organic modified hectorite, etc. can be used. More specifically, dimethyl distearyl ammonium hectorite, dimethyl alkyl ammonium hectorite, benzyl dimethyl stearyl ammonium hectorite, distearyl dimethyl ammonium chloride-treated aluminum magnesium silicate and the like can be mentioned. In the present invention, a premix product containing an organically modified clay mineral may be used as the organically modified clay mineral. For example, 12.5% by mass of distearyldimonium hectorite, 37.5% by mass of PEG-10 dimethicone, 49.95% by mass of cyclopentasiloxane, 0.05% tocopherol, such as Nikomurus WO manufactured by Nippon Surfactant Co., Ltd. A composition consisting of% by mass can be exemplified. In the composition of the present invention, it is preferable to add 0.05 to 2% by mass, more preferably 0.1 to 1% by mass as the organically modified clay mineral.
Moreover, in this invention, it is preferable to mix | blend any one or both of inulin fatty acid ester and dextrin fatty acid ester in addition to an organic modified clay mineral. When an inulin fatty acid ester and / or a dextrin fatty acid ester is further blended in the composition, the feeling of use such as “feeling of smoothness of spreading” and “feeling of thickness”, which is felt when applied, is further improved. Examples of inulin fatty acid esters include inulin stearate. Inulin stearate is obtained by esterifying stearic acid to inulin. An example of a commercially available product is Leo Pearl ISL2 manufactured by Chiba Flour Milling Co., Ltd. Moreover, as dextrin fatty acid ester, dextrin palmitate can be illustrated. Dextrin palmitate is an ester bond between dextrin and palmitic acid. An example of a commercially available product is Leopard KL manufactured by Chiba Flour Milling Co., Ltd. The blending amount of the inulin fatty acid ester and / or the dextrin fatty acid ester may be set as appropriate, but by blending 0.1 to 1% by mass in a total amount, “a feeling of smoothness”, “a feeling of thickness”, “ This is preferable because the feeling of non-stickiness, the feeling of skin familiarity, and the feeling of firmness are further improved.

[(D): highly polymerized silicone]
The highly polymerized silicone used in the present invention is a viscosity of 40,000 to 50,000 mPa · s when the highly polymerized silicone is dispersed at a concentration of 20% by mass in dimethylpolysiloxane having a kinematic viscosity of 20 mm ² / s by the capillary method. A silicone having the following characteristics. The degree of polymerization of this highly polymerized silicone is about 8000 when calculated from the weight average molecular weight based on gel permeation chromatography.
In this invention, it is preferable to mix | blend this highly polymerized silicone so that it may contain 0.1-0.5 mass% per composition, More preferably, 0.2-0.4 mass%. The highly polymerized silicone having such characteristics is commercially available as a composite product and can be used. An example of such a commercial product is MK-15H manufactured by Shin-Etsu Chemical Co., Ltd. MK-15H is a mixture of a highly polymerized methylpolysiloxane having a polymerization degree of 8000 and a low-viscosity methylpolysiloxane having a viscosity of 20 mm ² / s as measured by a capillary method in a ratio of 2: 8. When using this MK-15H, it is preferable to mix | blend 0.5-2.5 mass% per composition, More preferably, 1-2 mass%.
In addition, MK-15H containing this highly polymerized silicone has a viscosity of 45000 mPa · s when measured at 25 ° C. using a B-type viscometer.
By blending such a highly polymerized silicone with the poly (12-hydroxystearic acid) ester of polyhydric alcohol and lecithin, the water-in-oil emulsion composition of the present invention has a “feeling of a smooth and smooth” It becomes a composition having both an excellent feeling of use such as “thickness” and an effect of suppressing oil separation.
When the viscosity of the highly polymerized silicone is dispersed in dimethylpolysiloxane having a kinematic viscosity of 20 mm ² / s by capillary method at a concentration of 20% by mass, the viscosity of the highly polymerized silicone is 40000 mPa · s at 25 ° C. when measured with a B-type viscometer. When it is less than s or more than 50000 mPa · s, oil separation occurs in the gap, which is not preferable.

[(E): Oil agent]
Examples of the oil that can be used in the present invention include ester oils, fats and oils, hydrocarbon oils, silicone oils, and volatile silicone oils. Liquid oil or pasty oil is preferred.
Examples of ester oils include cetyl ethylhexanoate, 1,3-butylene glycol diisononanoate, 1,3-butylene glycol di-2-ethylhexanoate, dipropylene glycol diisononanoate, dipropylene glycol di-2-ethylhexanoate, Isononyl isononanoate, glyceryl tri-2-ethylhexanoate, glyceryl tricaprate, glyceryl triisostearate, neopentyl glycol dicaprate, ethylhexyl palmitate, isostearyl neopentanoate, myristoylmethyl-β-alanine (phytosteryl / decyltetradecyl), etc. Is mentioned.
Examples of fats and oils include camellia oil, evening primrose oil, macadamia nut oil, olive oil, rapeseed oil, corn oil, sesame oil, jojoba oil, germ oil, wheat germ oil, liquid oil and fat, cocoa butter, palm oil, palm oil, palm Examples include nuclear oil.
Examples of the hydrocarbon oil include liquid paraffin, squalene, squalane and the like.
Examples of silicone oil include dimethylpolysiloxane and methylphenylpolysiloxane. Examples of the volatile silicone oil include decamethylcyclopentasiloxane and cyclopentasiloxane. Instead of these, a composition containing the highly polymerized silicone may be blended.
In particular, pentaerythrityl tetraethylhexanoate, squalane, isostearyl isostearate, ethylhexyl palmitate, methylphenylpolysiloxane, methylpolysiloxane, cyclopentasiloxane, olive oil, jojoba oil, myristoylmethyl-β-alanine (phytosteryl / decyltetradecyl) ) Are preferably used in combination from the viewpoint of usability. Although the compounding quantity of the oil agent in this invention is not specifically limited, Preferably it is 20-50 mass% with respect to a composition. Further, in order to realize good elongation (“feel of smoothness”) and “feel of skin familiarity”, an oil agent selected from the group consisting of silicone oil and volatile silicone oil is used in an amount of 40 to 60 with respect to the total amount of oil agent. It is preferable to mix so that it may become the mass%. Since ester oils, fats and oils, and hydrocarbon oils can give a moist feel, they are preferably blended so as to be 60 to 40% by mass with respect to the total amount of the oil agent.

  The viscosity of the water-in-oil emulsified composition of the present invention is No. 1 after storage for 1 week at room temperature (25 ° C.). When a B-type viscometer equipped with 4 rotors is used and measurement is performed under the conditions of a measurement temperature of 25 ° C., a rotor rotation speed of 6 rpm, and 30 seconds after the start of measurement, it is preferably in the range of 20000 to 50000 mPa · s. This viscosity is a preferable range as the viscosity of the cream filled in the tube container, even if the 6K bottle (standard bottle) is tilted and the content does not flow down.

[Optional ingredients]
In the water-in-oil emulsion composition of the present invention, components that are usually used in cosmetics, for example, nonionic surfactants, anionic surfactants, as long as the effects of the present invention are not impaired as optional components Agent, cationic surfactant, amphoteric surfactant, oil agent, moisturizer such as polyhydric alcohol, antioxidant, ultraviolet absorber, salt, pH adjuster, preservative, ascorbic acid derivative, antibacterial agent, chelating agent Coloring agents, fragrances and the like can be blended. In addition, cosmetic ingredients such as ceramide and plant extract can be blended.

Examples of the humectant include glycerin, diglycerin, 1,3-butylene glycol, dipropylene glycol, and pentylene glycol.
Examples of the salts include sodium chloride and magnesium sulfate.
Examples of the pH adjusting agent include citric acid, sodium citrate, phosphoric acid, sodium phosphate, potassium hydroxide and the like.
Examples of the preservative include phenoxyethanol and paraben.
Examples of the ascorbic acid derivative include L-ascorbic acid phosphate magnesium salt, L-ascorbic acid phosphate sodium salt, 2-O-α-D-glucopyranosyl-L-ascorbic acid and the like.
Examples of ceramide include cetyl PG hydroxyethyl palmitate, cerebroside and the like.

  The water-in-oil emulsion composition of the present invention can be used as a quasi-drug or pharmaceutical product as a cosmetic or a skin external preparation. The dosage form is particularly preferably a creamy dosage form, which is suitable for topical cosmetics such as the eyes and external preparations.

The features and effects of the present invention will be described in more detail with reference to examples and comparative examples.
The water-in-oil emulsion compositions (cream type) of Comparative Examples 1 to 8 having the compositions shown in Table 1 and Examples 1 to 6 and Table 2 were prepared.
In addition, the compounding component which attached | subjected * 1-4 to Table 1 and Table 2, and was marked is as follows.
* 1: Nikomulus WO, manufactured by Nippon Surfactant Kogyo Co., Ltd .: 12.5% by mass of distearyldimonium hectorite, 0.05% by mass of tocopherol, 37.5% by mass of PEG-10 dimethicone, 49.95% by mass of cyclopentasiloxane. %
* 2: MK-15H, manufactured by Shin-Etsu Chemical Co., Ltd .: Highly polymerized methylpolysiloxane (polymerization degree 8000) at a concentration of 20% by mass to low polymerized methylpolysiloxane (dimethylpolysiloxane having a kinematic viscosity of 20 mm ² / s) Dispersed dispersion (viscosity is 45000 mPa · s)
* 3: BY11-040 manufactured by Toray Dow Corning Co., Ltd .: A dispersion in which highly polymerized dimethylpolysiloxane (polymerization degree 2800, viscosity is 4 million mPa · s) is dispersed in cyclopentasiloxane at a concentration of 15% (viscosity is 1500mPa · s)
* 4: KF-96H-1 million mPa · s (manufactured by Shin-Etsu Chemical Co., Ltd., polymerization degree 2200) at a concentration of 20% by mass with a low viscosity silicone (kinematic viscosity 20 mm ² / s when measured by capillary method) Dispersion) (viscosity is 1700 mPa · s)

(Preparation method)
Ingredients (A) to (E) are heated to 90 ° C. and mixed thoroughly with stirring to prepare an oil phase. Water phase components such as water and polyhydric alcohol are heated to 80 ° C. and sufficiently stirred and mixed to prepare an aqueous phase. While the adjusted aqueous phase is gradually added to the oil phase, the mixture is stirred and emulsified at 6000 rpm for 2 minutes using a homomixer, and then cooled to room temperature while stirring to obtain a water-in-oil emulsion composition.

(Evaluation method)
Measurement and sensory evaluation were performed on the following evaluation items.
<Viscosity>
The obtained water-in-oil emulsion composition was filled in a glass container having a diameter of about 4 cm and stored in a heat-reserving bath at 25 ° C. and 50 ° C. for 1 week, 2 weeks, and 1 month. After elapse of the storage days, No. A B-type viscometer equipped with 4 rotors was used, and measurement was performed under the conditions of a measurement temperature of 25 ° C., a rotor rotation speed of 6 rpm, and 30 seconds after the start of measurement. Immediately before measuring the viscosity, the presence or absence of an oil separation layer (oil separation) was confirmed on the surface of the emulsion. The evaluation of oil separation was performed based on the following <Confirmation of oil separation into voids>.

<Emulsification stability>
The emulsification stability was evaluated by the following cycle test. The cycle test is a test for evaluating the emulsion stability. Those in which separation occurs in this test are judged as “poor emulsion state”.
<< Cycle test >>
The obtained water-in-oil emulsion composition was filled into glass containers (6K bottles) each having a diameter of about 4 cm, and the low temperature (−20 ° C.) and room temperature were alternately repeated for 12 hours each, and this was repeated for 2 cycles. The emulsified state was visually observed.
Evaluation was made in the following two stages.
○: Not separated ×: Separated (water and aqueous phase components are separated)

<Confirmation of oil separation>
The obtained water-in-oil emulsified composition is placed in a glass container (6K bottle) each having a diameter of about 4 cm, and a narrow mouthed bag (with the tip of a plastic bag cut) on the filling surface in contact with the glass. Was observed, and the container was sealed tightly. This was stored in a 40 ° C. and 50 ° C. thermal insulation bath for one month, and the occurrence of oil separation in the voids formed so as to contact the glass was visually observed. Oil separation is different from separation of an emulsified composition with water separation. Oil release may be observed on the surface of the composition filled in the 6K bottle, but since the oil spreads over the entire surface, if the amount is small, it may be overlooked by the visual appearance observation method. However, it can be confirmed by a test method that created voids. This test is an effective test as a method for confirming quality deterioration due to early oil separation.
The visual evaluation criteria under each temperature condition were the following two stages.
○: No oil separation in the gap
X: There is oil separation in the gap. In this test, visual observation of the surface was also performed at the same time. The evaluation criteria in this case are as follows.
○: No oil separation on the surface
×: There is oil separation on the surface

<Sensory evaluation>
Regarding the feeling of use, two professional sensory evaluators evaluated the following criteria for each evaluation item: “Thickness”, “Smoothness of smoothness”, “Smoothness of stickiness”, “Feeling of skin”, and “Feeling” It was evaluated by. The evaluation results in the table were consistent with each other. The history of the sample was evaluated blindly by the sensory evaluator.

<< Thickness >>
◎: Very thick
〇: Feel the thickness
Δ: Somewhat thick
×: Does not feel thickness

<< Smoothness of Noby >>
◎: Feels very smooth and smooth. ○: Feels smooth and smooth.
Δ: Feels a little smooth and smooth
×: Does not feel smooth and smooth

<< Non-sticky feeling >>
〇: Does not feel sticky
Δ: Somewhat sticky
×: Sticky

<< Skin familiarity >>
〇: Feel skin familiarity
Δ: Slightly familiar with skin
×: Does not feel skin familiarity

<< Harness >>
〇: Feeling firm
Δ: Slight tension
×: Does not feel tension

(Evaluation results)
As shown in the lower part of Tables 1 and 2, the water-in-oil emulsion compositions of Examples 1 to 6 have no oil separation in the voids even when visually confirmed after storage at high temperature (50 ° C.) for 1 month. All the evaluation items of “feeling of smoothness”, “feeling of stickiness”, “feeling of thickness”, “feeling of skin familiarity”, “feeling of firmness”) are realized. I was able to confirm that. That is, it turned out that it is a stable composition which has all the feelings of use required for an eye cream.
On the other hand, the emulsified state of the compositions of Comparative Examples 1 to 5 was confirmed to be good by a cycle test in some test examples (Comparative Examples 1 and 2), but oil separation into the voids was observed ( Comparative Examples 1-4). In Comparative Example 5, although no oil separation occurred, the feeling in use was quite poor. In Comparative Examples 6 to 8, oil separation occurred and it was judged that the quality of the cream type filling the tube container was unsuitable.
Focusing on the viscosity, Example 4 had no oil separation even when the viscosity after storage at 50 ° C. decreased to 7000 mPa · s, but Comparative Example 6 had a viscosity of 38900 mPa · s after storage at 50 ° C. The viscosity was 5 times higher than 4, but oil separation was observed. That is, it was confirmed that the phenomenon of “oil separation” was not suppressed by the viscosity.
In addition, when dimethyl distearyl ammonium hectorite was first selected as the oily gelling agent, and when dextrin palmitate or inulin stearate was used in combination, “feeling of skin familiarity” and “feeling of firmness” were excellent. In particular, it was confirmed that “thickness” and “smoothness and smoothness” were excellent when blended with inulin stearate in combination.
The structure of the present invention has no “oil-releasing” and all of the feelings of use (“smoothness of smoothness”, “feel of non-stickiness”, “feel of thickness”, “feel of skin familiarity”, “feel of firmness”) It was found that the item can be realized.

  Summarizing the above evaluation, the water-in-oil emulsion composition of the present invention has a “feel of smoothness”, “feel of non-stickiness”, “feel of thickness”, “feel of skin familiarity”, and “feel of firmness”. All can be realized, and oil separation does not occur even at high temperatures, so it can be said that it is optimal as a cream for the eyes when filled in a tube container.

Below, the prescription | regulation of a water-in-oil emulsion composition which employ | adopted the structure of this invention, a manufacturing method, and a characteristic are shown.
Formulation Example 1 High moisturizing cream formulation
(Compounding ingredients) (mass%)
1. Dipolyhydroxystearic acid PEG-30 2
2. Hydrogenated lecithin 1
3. Myristoylmethyl-β-alanine (phytosteryl / decyltetradecyl) 2
4). Olive oil 5
5. Jojoba oil 4
6). Glyceryl tri-2-ethylhexanoate 3
7). Cyclopentasiloxane 5
8). Methylphenylpolysiloxane 5
9. (Dimethicone / Vinyl Dimethicone) Cross Polymer 1
10. Dimethyl distearyl ammonium hectorite 1
11. MK-15H (manufactured by Shin-Etsu Chemical Co., Ltd.) 2
12 Glycerin 5
13. 1,2-Pentanediol 2
14 Phenoxyethanol 0.2
15. Sodium hyaluronate 0.1
16. Purified water residue

(Manufacturing method)
The oil phase (components 1 to 11) and the water phase (components 12 to 16) were separately heated to 80 to 90 ° C. and sufficiently stirred to prepare an aqueous phase and an oil phase. The obtained aqueous phase was added to the oil phase, emulsified by stirring at 6000 rpm for 2 minutes with a homomixer, and then cooled with stirring to room temperature to obtain a water-in-oil emulsion composition.

(Characteristic evaluation)
Viscosity, emulsion stability, oil separation, and feeling of use were evaluated in the same manner as described above.
The high moisturizing cream of Formulation Example 1 has an appropriate viscosity, good emulsification stability, no oil separation, and a feeling of use (“feeling of smoothness”, “feeling of non-stickiness”, “thickness” Feeling ”,“ feeling of skin familiarity ”, and“ feeling firmness ”), and excellent storage stability.

Claims (10)

A water-in-oil emulsion composition containing (A) to (E).
(A) lipophilic surfactant (B) lecithin (C) oily gelling agent (D) highly polymerized silicone (E) oil agent   The water-in-oil emulsion composition according to claim 1, wherein (A) the lipophilic surfactant is a poly (12-hydroxystearic acid) ester of a polyhydric alcohol. (D) A dimethylpolysiloxane having a viscosity of 40,000 to 50,000 mPa · s by a rotation method when a highly polymerized silicone is dispersed in dimethylpolysiloxane having a kinematic viscosity of 20 mm ² / s by a capillary method at a concentration of 20% by mass. The water-in-oil emulsion composition according to claim 1 or 2.   (D) The polymerization degree of highly polymerized silicone is 8000, The water-in-oil emulsion composition in any one of Claims 1-3.   (C) The oily gelling agent is an organically modified clay mineral, The water-in-oil emulsion composition according to any one of claims 1 to 4.   The water-in-oil emulsion composition according to claim 5, wherein the organically modified clay mineral is dimethyl distearyl ammonium hectorite.   The water-in-oil emulsion composition according to claim 5 or 6, further comprising (C) an inulin fatty acid ester and / or a dextrin fatty acid ester as an oily gelling agent.   (E) Oil agent contains 1 or more types from the group which consists of silicone oil and volatile silicone oil, and 1 or more types from the group which consists of ester oil, fats and oils, and hydrocarbon oil in any one of Claims 1-7 characterized by the above-mentioned. A water-in-oil emulsion composition.   The water-in-oil emulsion composition according to any one of claims 1 to 8, wherein the viscosity of the composition measured at 25 ° C with a B-type viscometer is 20000 to 50000 mPa · s.   It is a cream for eyes, The water-in-oil emulsion composition in any one of Claims 1-9.