KR20100039937A - Preparation of microcapsule loaded with active materials and cosmetic composition containing the microcapsule - Google Patents

Abstract

PURPOSE: A method for manufacturing solid waxa microcapsule is provided to stabilize soluble or/and insoluble active ingredients by capsulation and to last activation of the product. CONSTITUTION: A cosmetic composition contains 7-dihydrocholesterol, retinol, or active ingredient of Glycyrrhiza uralensis extract thereinside, and candelilla wax, behenyl alcohol, batyl alcohol, glyceryl stearate se, or ceresin wax. The solid wax is 0.1-10 weight% based on oil phase. The cosmetic composition is used in the form of skin lotion, milk lotion, massage cream, pack, gel, essence, lip stick, makeup base, foundation, lotion, cream, or spray.

Description

Preparation method of a solid wax microcapsule containing a functional material and a cosmetic composition containing the same {Preparation of microcapsule loaded with active materials and cosmetic composition containing the microcapsule}

The present invention relates to a method for producing a solid wax microcapsules containing a functional material and a cosmetic composition containing the solid wax microcapsules.

Unstable bioactive substances are rapidly degraded by the external environment. Therefore, encapsulation techniques for stabilizing these materials are very important. 7-Dihydrocholesterol (hereinafter referred to as "7-DHC"), a precursor of vitamin D3, is known to increase the expression of Heat Shock Protein at the level of protein and mRNA in epidermal keratinocytes of the general public. Vitamin D is the only vitamin that is synthesized in the skin. In fact, starting with a precursor called 7-DHC (7-dihydrocholesterol) in the basal layer of the epidermis, the synthesis of vitamin D occurs under the influence of ultraviolet radiation. Vitamin D skin synthesis is controlled by natural self-regulatory mechanisms, especially to prevent excessive production of vitamin D, especially when exposed to ultraviolet light. Excessive exposure to UV light causes the cells that make up the skin to die, so that each skin cell loses its own function and can cause abnormal skin defense and immune mechanisms. Vitamin D3 and its precursors have been reported to protect the skin from ultraviolet radiation and to restore skin cells exposed to ultraviolet radiation. However, the use of 7-DHC as a topical skin preparation has been limited due to its low solubility and chemical instability.

Retinoids include retinol, retinal, retinyl acetate, and the like. Among these, retinol is an endogenous compound and is essential for the differentiation and growth of epithelial tissue. Retinoids play an important role in maintaining the original function of epidermal cells, and have been applied to the treatment of skin cancer, beginning to be used to treat various diseases with abnormal changes in keratinogenesis. By making the epidermal cells younger, they can inhibit skin aging and prevent pigmented skin diseases. In particular, the retinoid is one of the substances that can penetrate to the dermis, which is below the skin, from the outside of the skin and act on the collagen and elastin of the dermis. The penetrating action of retinoids increases collagen and elastin, increases elasticity and softens the skin. Cosmetic compositions containing retinoids are formulated as oil-in-water (o / w) emulsion compositions, but the retinoids contained in these compositions are chemically unstable and easily lose their activity.

Oil-soluble licorice extract is derived from dried herbal medicines from the root or stem of licorice. Glabridin, an oil-soluble licorice extract, is a hydrophobic main ingredient, which is easier to penetrate into the skin than other whitening substances, and inhibits the production of tyrosinase, a melanin pigment-forming enzyme, resulting in excellent whitening and inflammation. It shows the effect of suppressing. However, although the glybridine component is useful in its chemical structure, it also has solubility in water, so that even after stabilization, the glabridine component comes out of the particles, browns the color of the cosmetic, and loses activity.

Vitamin D is known to be effective in skin aging and whitening effects, and Korean Patent No. 10-03222081 stabilizes using a porous lipophilic polymer resin to improve the safety problem in the existing application in cosmetics. It states that it could. In addition, the use of vitamin A in cosmetics has been well known for a long time, but skin irritation, reducing irritation and encapsulation methods have already been introduced. Korean Patent No. 10-0271315 discloses a method of encapsulating D-α-tocopherol with retinol or its derivative using marine collagen and chitosan as a matrix. Glybridine is very effective in preventing skin aging by promoting fibroblast and keratinocyte proliferation, improving skin wrinkles by promoting collagen synthesis, improving skin elasticity, improving moisture, and enhancing skin immunity. Because of its small size, a technique for liposomeizing a cosmetic composition having no side effects on the skin is disclosed in Korean Patent No. 10-0570096.

However, the vitamin D and oil-soluble licorice extract having such efficacy are difficult to apply to the formulation because it is a poorly soluble substance, and vitamin A is unstable and the efficacy is rapidly decreased when exposed to external environment such as light, especially cosmetic formulation In the case of inclusion in the formulation, it is liable to be denatured by the surfactant, water, oil, etc. present in the formulation. Therefore, vitamin D and oil-soluble licorice extract should be easily solubilized, and in order to use unstable vitamin A as a cosmetic raw material, there is a problem that the various stimuli must be blocked.

Accordingly, the present invention solves the above problems in formulating a functional active ingredient in cosmetics, and easily solubilizes poorly soluble substances such as vitamin D, oil-soluble licorice extract, and the unstable substance such as vitamin A has its activity and color in the cosmetic It is intended to be formulated so as not to denature.

In addition, an object of the present invention is to prepare a stabilized and solubilized cosmetics vitamin D, oil-soluble licorice extract or unstable vitamin A in the functional active ingredient.

In order to achieve the above object, the present inventors collect a functional active ingredient such as vitamin D, oil-soluble licorice extract or vitamin A in solid wax and prepare it as microcapsules by using phase separation of the oil phase containing the aqueous phase and the functional active ingredient. The invention was invented.

Hereinafter, the present invention will be described in detail. The present invention secured stability by preparing microcapsules using solid wax to increase the solubilization of poorly soluble functional materials and the stability of unstable functional active ingredients, and used them in cosmetic compositions.

In the present invention, the size of the capsule can be controlled by the stirring speed and the stirring time in the process of preparing microcapsules using the phase separation of the oil phase containing the water phase and the functional active ingredient, and the feeling of use can also be adjusted according to the properties of the solid wax. have.

In order to effectively deliver a functional active ingredient to the skin, the first thing to do is stabilization and solubilization of the functional active ingredient. Therefore, it is necessary to solubilize and stabilize poorly soluble functional active ingredients and apply them to cosmetic compositions easily and simply. In preparing the solid wax microcapsules, the stirring speed and the stirring time should be adjusted in order to adjust the capsule particle size. Solid waxes such as CANDELILLA WAX, BEHENYL ALCOHOL, BATYL ALCOHOL, GLYCERYL STEARATE SE, and Ceresin Wax have a content of 0.1 to It is preferably adjusted to 10.0% by weight, and the content of poorly soluble and / or unstable functional active ingredient is used by mixing 0.1 to 5.0% by weight with respect to the total oil phase component. If the wax is used less than the above range, there is a problem that it is difficult to form a capsule by capturing a functional active ingredient, and when used too much, the size of the particles is too large to cause agglomeration. In addition, when poorly soluble and / or unstable functional active ingredients are used in less than the above range, it is difficult to expect a sufficient efficacy effect in consideration of titer and the like, and when excessively used, there is a problem in that the stability of the capsule cannot be secured.

In addition, among the solid wax components of the group consisting of candelilla wax (CANDELILLA WAX), beyl alcohol (BEHENYL ALCOHOL), batyl alcohol (BATYL ALCOHOL), glyceryl stearate SE (CELYIN WAX) The use of one or more selected is because these waxes can form voids in capsule formation, and when other solid waxes are used, it is not easy to create voids.

The microcapsules made of the solid wax component can adjust the size by controlling the stirring speed and time, increase the stability of the functional active ingredient, and finally play a role of enhancing the penetration efficiency in the skin. In addition, according to the present invention, if the stirring speed is increased and the stirring time is lengthened, small particles may be formed to further increase the stability of the functional active ingredient.

The present invention is a mixture of purified water, butylene glycol (BUTYLENE GLYCOL), dimethicone (DIMETHICONE), carbomer and triethanolamine 30 to 50: 1 to 10: 1 to 5: 0.1 to 3: 0.1 to 1 by weight A water phase is produced and is included in the group consisting of CANDELILLA WAX, BEHENYL ALCOHOL, BATYL ALCOHOL, GLYCERYL STEARATE SE, and CRESIN WAX. Oil phase mixed with at least one functional active ingredient selected from the group consisting of one or more selected solid waxes, SQUALANE, retinol, 7-DHC and oil-soluble licorice extract in a weight ratio of 0.1 to 10: 1 to 5: 0.1 to 5.0 After heating to 80 ° C. and stirring, the functional active ingredient and the solid wax are mixed, and a solid wax capsule is formed during the cooling process to collect the functional active ingredient therein. Thus prepared is a solid wax microcapsules, which is a cosmetic formulation commonly referred to in the art as an essence.

The formulation of the microcapsules cosmetic composition provided by the present invention may be any formulation that can be prepared as an external preparation for skin, and may include basic cosmetics such as flexible lotion, nutrition lotion, massage cream, nutrition cream, pack, gel, essence, lipstick, makeup base, It can also be widely applied to external cosmetics or quasi-drugs such as color cosmetics and cleaning agents such as foundations, hair dressings, wool, hair dyes, and lotions, ointments, creams, gels, patches or sprays.

The present invention solves the problems of poor solubility and instability caused by applying the active ingredient to cosmetics by stabilizing micro-encapsulated and insoluble functional active ingredients such as 7-DHC, retinol, oil-soluble licorice extract using solid wax. It could be improved and the activity of the product could last long. Therefore, the cosmetic composition of the present invention is useful in applying poorly soluble and / or unstable functional active ingredients to skin cosmetics.

One or more functional active ingredients selected from the group consisting of 7-dihydrocholesterol, retinol and oil-soluble licorice extracts are collected therein, candelilla wax (CANDELILLA WAX), benzyl alcohol (BEHENYL ALCOHOL), batyl alcohol ( BATYL ALCOHOL), GLYCERYL STEARATE SE and CERESIN WAX selected from the group consisting of one or more solid waxes, which are formed by stirring in an aqueous phase or in an oily phase as an active ingredient. It provides a cosmetic composition.

In addition, the present invention provides a cosmetic composition, characterized in that the solid wax is 0.1 to 10% by weight relative to the oil phase.

In addition, the present invention provides a cosmetic composition, characterized in that the functional active ingredient is 0.1 to 5% by weight relative to the oil phase.

In addition, the present invention, the cosmetic composition is a flexible lotion, nourishing lotion, massage cream, nourishing cream, pack, gel, essence, lipstick, makeup base, foundation, cleaning agent, hair dressing, wool, hair dye, lotion, cream or spray formulation It provides a cosmetic composition characterized in that.

The present invention is also selected from the group consisting of CANDELILLA WAX, BEHENYL ALCOHOL, BATYL ALCOHOL, GLYCERYL STEARATE SE, and CRESIN WAX. Mixing at least one solid wax with at least one functional active ingredient selected from the group consisting of 7-dihydrocholesterol, retinol and oil-soluble licorice extract, completely dissolving it, and then mixing it with a warm water phase;

Stirring the aqueous, oily mixture;

And cooling after stirring;

It provides a cosmetic composition manufacturing method containing a microcapsules containing as an active ingredient.

In another aspect, the present invention provides a method for producing a cosmetic composition containing a microcapsule as an active ingredient, characterized in that the heating range of the oil phase and the water phase is 40 ~ 90 ℃. If the heating range is too low, the oil phase is not dissolved and the water phase and the oil phase are not mixed, and thus the microcapsules are not formed, and the active ingredient is destroyed at an excessively high temperature.

In addition, the present invention provides a method for producing a cosmetic composition containing the microcapsules as an active ingredient, characterized in that the stirring is 300 to 1,000 rotations for 30 seconds to 10 minutes. If the stirring time is too short, the capsule size becomes large, and in case of skin lotion, precipitation may occur and the skin penetration rate decreases. In addition, if the stirring is excessively long, the size of the capsule becomes too small, making it difficult to collect the functional material in the capsule, and the collection rate is lowered.

Hereinafter, the configuration of the present invention will be described in more detail based on the following examples. However, it will be apparent to those skilled in the art that the scope of the present invention is not limited only to the description of the following examples.

Example 1 Preparation of Solid Wax Microcapsules and Essence Cosmetics  Produce

To prepare microcapsules, an aqueous phase containing purified water, butylene glycol, dimethicone, carbomer and triethanolamine was warmed to 80 ° C.

The oil phase is selected from the group consisting of squalene and candelilla wax, BEHENYL ALCOHOL, BATYL ALCOHOL, GLYCERYL STEARATE SE, and ceresin wax. At least one solid wax and at least one functional active ingredient selected from the group consisting of 7-DHC, retinol and oil-soluble licorice extract were added to complete dissolution and then mixed into the warm water phase (see Table 1). This mixed solution was stirred for 1 minute at 300 rpm / min using a Haydon mixer. Cooling after stirring to prepare a solid wax microcapsules.

 Awards  Paid a Purified water: 83.9% Butylene Glycol: 7.0% Dimethicone: 1.0% Carbomer: 0.1% Triethanolamine: 0.1% Squalene; 2.0% Candelilla Wax: 0.7% 7-DHC 0.5% b Retinol 0.5% c Soluble Licorice Extract 0.5% d Benyl Alcohol: 0.7% 7-DHC 0.5% e Retinol 0.5% f Soluble Licorice Extract 0.5% g Batyl alcohol: 0.7% 7-DHC 0.5% h Retinol 0.5% i Soluble Licorice Extract 0.5% j Glyceryl Stearate SE: 0.7% 7-DHC 0.5% k Retinol 0.5% l Soluble Licorice Extract 0.5% m Ceresin Wax: 0.7% 7-DHC 0.5% n Retinol 0.5% o Soluble Licorice Extract 0.5%

Comparative Example 1

The same conditions as in Example 1 were prepared in the same manner, but the functional active ingredient was prepared by adding the microcapsules after the preparation.

Test Example 1: Microcapsules Size and Functional Substance Content

In order to measure the size of the prepared microcapsules and the content of functional substances, the microcapsules prepared in Example 1 were checked for particle size using a light scattering apparatus [ELS-8000, OTUSKA Electronics Co., Japan]. The content of functional material was measured using HPLC. The results are shown in Table 2.

 Revolutions / hour (minutes)  300 times / 1 minute  400 times / 2 minutes  500 times / 3 minutes  No.  Particle size (㎛)  % Loading  Particle size (㎛)  % Loading  Particle size (㎛)  % Loading  a  250.1  92.0  30.0  91.3  5.3  91.9  b  260.3  91.3  34.1  89.3  3.5  89.0  c  255.0  90.6  33.8  93.0  6.1  91.2  d  261.3  91.3  33.7  92.5  4.9  92.5  e  258.1  89.3  32.6  91.2  5.7  90.9  f  250.8  93.0  32.0  92.5  5.3  93.0  g  252.3  92.5  33.8  90.9  4.5  92.5  h  256.4  91.9  34.7  91.4  6.5  91.3  i  255.8  89.0  32.4  92.0  3.1  90.6  j  258.4  91.2  33.5  91.3  2.3  91.4  k  254.1  92.5  33.6  90.6  6.1  91.3  l  263.1  90.9  37.5  91.4  5.8  89.3  m  259.1  91.4  39.4  91.8  4.7  93.0  n  260.0  91.8  35.4  91.0  6.0  92.5  o  253.7  92.3  33.5  92.1  5.5  91.2

As shown in Table 2, when the size of the microcapsules according to the present invention is 300/1 minutes 250.1 ~ 263.1㎛, 400/2 minutes 30.0 ~ 39.4㎛ when 500/3 minutes It was confirmed that the 2.3 ~ 6.5㎛, the content of the functional material was found to be 89.0 ~ 93.0% without significant difference even if the number of revolutions and time. Therefore, it was confirmed that the size of the particles can be adjusted according to the rotation speed and time when preparing the microcapsules using the solid wax.

Test Example 2: Microcapsules Size and Functional Contents after 6 Months

In order to measure the change in particle size and the change in the content of the functional material after 6 months of the preparation of the microcapsules, the size of the microcapsules prepared in Example 1 was confirmed by using a light scattering apparatus, and the content of the functional material Was measured using HPLC.

 300 times / 1 minute> 6 months later  400 times / 2 minutes> 6 months later  500 times / 3 minutes> 6 months later  No.  Particle size (㎛)  % Loading  Particle size (㎛)  % Loading  Particle size (㎛)  % Loading  a  255.1  85.3  31.0  84.3  5.6  84.3  b  263.3  84.2  34.7  85.1  3.7  85.1  c  257.1  86.0  34.8  84.9  6.1  84.9  d  263.7  84.3  34.0  85.0  5.2  83.2  e  259.3  85.1  32.8  84.2  5.8  84.2  f  258.7  84.9  33.2  85.6  5.7  85.6  g  259.1  83.2  34.5  84.4  5.0  84.4  h  256.4  83.9  35.1  83.7  6.8  83.7  i  255.7  84.0  33.2  84.7  3.7  86.0  j  258.7  82.9  34.1  84.2  2.9  84.3  k  255.3  83.4  34.7  86.0  6.4  83.7  l  263.3  85.6  38.3  84.3  5.9  84.7  m  260.2  84.4  40.2  85.1  4.9  84.2  n  261.4  83.7  36.7  84.9  6.3  86.0  o  255.7  84.7  34.5  83.2  5.7  84.8

As shown in Table 3, the size of the microcapsules according to the present invention after six months is a capsule prepared under the condition of 300/1 minutes. 255.1 ~ 263.3㎛, capsules manufactured under the conditions of 400/2 minutes 31.0 ~ 40.2㎛ capsules manufactured under 500/3 minutes It was confirmed that the 2.9 ~ 6.8㎛, the content of the functional material was also found to be 82.9 ~ 86.0%. That is, after 6 months, the particle size and loading rate were almost unchanged, which confirms that the functional material was stabilized by encapsulation of the solid wax.

Test Example 3: Stabilized 7- DHC Wrinkle Relief Effect Test

In order to verify the anti-wrinkle effect of stabilized 7-DHC in women aged 30 to 40 years, 20 subjects were selected and tested as follows. The microcapsules containing stabilized 7-DHC were stored at 45 ° C. for 4 weeks in the microcapsules of Example 1 and then the product of Example 1 was applied twice a day around the woman's right eye for 4 weeks. Comparative Example 1 was applied around the other eye for comparison. After 4 weeks, the wrinkle relief effect was visually observed and the results are summarized in Table 4.

 A noticeable effect  Mitigating effect  no effect  Example 1  12  8  0  Comparative Example 1  One  3  16

As shown in Table 4, when the Example 1 product stabilized with 7-DHC was applied, all 20 women showed a mitigating effect, and in particular, 12 showed a significant mitigating effect such that 7-DHC was not stabilized. Compared to 1 showed a breakthrough results. Thus, it was proved that the effect of the microcapsules stabilized with 7-DHC with solid wax was superior to that without stabilization.

Test Example 4: Test for skin elasticity effect of microcapsules containing retinol

Dividing 60 healthy women (average age 29.5 years) into 6 groups at a temperature of 22-24 ° C and 55% RH, apply the cosmetic compositions of Example 1 and Comparative Example 1 for 12 weeks, centered around the eyes, respectively. After (2 times / day) skin elasticity was measured using a skin elasticity measuring instrument (Cutometer SEM 575, C + K Electronic Co., Germany). The test results are described as ΔR5 values, ie, R5 (12 weeks) -R5 (0 weeks), which are average values of the respective test groups of the Cutometer SEM 575 shown in Table 5 below. The closer it is, the better the elasticity is.

In addition, the degree of improvement was calculated by the following equation 1 and the calculation results are shown in Table 5.

% Improvement = △ R5 / (R5 before application) * 100

 Before application  After application  Skin elasticity enhancing effect (△ R5)  % Improvement  Example 1  0.75  1.19  0.44  58.6  Comparative Example 1  0.73  0.82  0.09  12.3

According to Table 5, when using Example 1, the skin elasticity was increased by 46.3% compared to Comparative Example 1. Therefore, it can be seen that the cosmetic containing the microcapsules stabilized functional material according to the present invention effectively enhances skin elasticity.

Test Example 5: Whitening effect experiment of oil-soluble licorice extract microcapsules

The whitening effect of the cosmetic composition of the present invention was measured in 30 Korean women aged 19 to 40 with dark skin. 9 parts of the arms were measured by 1 cm in length and width, and the cosmetics of Example 1 and Comparative Example 1 were applied to each of two places, and the other one was used as a control for comparison. Each cosmetic was applied steadily for 8 weeks at intervals of 2 weeks, after 8 weeks to measure the skin color (L value) using Minolta CR 300 and calculated the degree of change of skin color (ΔL) using the following equation 2, The results are shown in Table 6 below.

Skin color change (ΔL) = L value before cosmetic application-L value after cosmetic application

 Example 1  Comparative Example 1  Control  ΔL  1.75  0.25  0.00

As can be seen from the results of Table 6, looking at the ΔL value after 8 weeks, cosmetic Example 1 of the present invention was significantly higher than Comparative Example 1 and the control group. Therefore, it can be seen that the cosmetic composition of the present invention shows a very good whitening effect.

Claims (7)

One or more functionally active ingredients selected from the group consisting of 7-dihydrocholesterol, retinol and oil-soluble licorice extracts are collected therein, candelilla wax (BEHENYL ALCOHOL), batyl alcohol (BATYL ALCOHOL) Cosmetic composition comprising a microcapsule produced by stirring at least one solid wax selected from the group consisting of glyceryl stearate SE (GLYCERYL STEARATE SE) and ceresin wax (CERESIN WAX) in the aqueous phase, oil phase mixed state as an active ingredient. The method of claim 1, The solid wax is a cosmetic composition, characterized in that 0.1 to 10% by weight relative to the oil phase. The method of claim 1, The functional active ingredient is a cosmetic composition, characterized in that 0.1 to 5% by weight relative to the oil phase. The method of claim 1, The cosmetic composition is a flexible lotion, nourishing lotion, massage cream, nourishing cream, pack, gel, essence, lipstick, makeup base, foundation, cleaning agent, hair dressing, wool, hair dye, lotion, cream or spray formulation Cosmetic composition. At least one solid wax selected from the group consisting of CANDELILLA WAX, BEHENYL ALCOHOL, BATYL ALCOHOL, GLYCERYL STEARATE SE, and CRESIN WAX. Mixing one or more functionally active ingredients selected from the group consisting of 7-dihydrocholesterol, retinol and oil-soluble licorice extracts, completely dissolving them, and then mixing them into a warm water phase; Stirring the aqueous, oily mixture; And cooling after stirring; Cosmetic composition containing a microcapsules containing as an active ingredient. The method of claim 5, The heating range of the water phase is a cosmetic composition manufacturing method containing a microcapsule as an active ingredient, characterized in that 40 ~ 90 ℃. The method of claim 5, The stirring method for producing a cosmetic composition containing the microcapsules as an active ingredient, characterized in that 300 to 1,000 rotations for 30 seconds to 10 minutes.