KR19990058599A - Cosmetic composition containing a double capsule - Google Patents

Abstract

The present invention is intended to improve the stability of cosmetic active ingredients that are easily oxidized or decomposed in water, oil or air, liposomes of water-soluble or oil-soluble actives for cosmetics, and then encapsulated in a matrix using chitosan to form a double capsule structure. The present invention relates to a cosmetic double capsule and a cosmetic composition containing the same.

Description

Cosmetic composition containing a double capsule

The present invention is water-soluble or soluble by a second matrix encapsulation by chitosan gum in which nano-sized particles encapsulated in liposomes, which are two-molecule membranes, are encapsulated in two-molecule liposomes which are thermodynamically unstable and easily oxidized in air or air. The present invention relates to a cosmetic double capsule having improved stability of an oil-soluble active substance and a cosmetic composition containing the same.

Generally used components such as retinol, retinic acid, retinaldehyde and derivatives thereof, unsaturated fatty acids and tocopherol belonging to water-soluble vitamin C derivatives and oil-soluble retinoids are easily oxidized in the air, aqueous solutions, or oil-soluble solutions. Worse Conventionally, in using these components, it is a reality that the product is stabilized in an oil-in-water (O / W) type of emulsion. In addition, in order to further increase the stability of the water-in-oil-in-water (W / O / W) type of multi-phase emulsion form is stabilized and partly commercialized, it is simply used by combining various antioxidants. In this case, there is a problem that can not be widely used because the activity of the component is changed over time to change to another substance or a specific odor is generated to irritate the skin.

Recently, liposome capsules that are actively applied in the cosmetic field are used in some functional cosmetics, but there are drawbacks that cannot be used because of difficulty in formulation. Although there are many types of liposomes, soybean phospholipids are used the most, and the method of solvent extraction, ultrasonic method, homogenizer method, and microfluidizer are used. How to do it.

The purpose of the application of the medial in the cosmetic field is to increase the fluidity of the biofilm of phospholipids to facilitate metabolism of the substance, and to increase the skin absorption of cosmetic ingredients. As a result, it has been reported that the cell survival time has been increased as a result of the liposome formation of the active ingredient on the skin and the experiment of the cell tissue culture. In epidermis, concentrations have been reported to increase more than five times. Recently, some cosmetics-related companies have introduced liposome theory and applied it to cosmetics, but the actual situation appears to be insignificant.

In general, as the components used in the matrix capsule, sodium alginate, collagen, chitosan, gelatin derivatives, agar and the like are prepared using the coating agent or used as a thickener or gelling agent. Here, collagen is coiled, so the use of the structure is increased, regardless of pH or ionic strength of the solvent, there is a feature that can be easily used in a wide range regardless of temperature, but it is difficult to be a complete capsule . On the other hand, sodium alginate is widely applied in the manufacture of hard capsules and is a raw material hardened by polyvalent metal ions. Although the stability is relatively good, there is a risk of breaking when the capsule is pressurized. I also have Since agar has a characteristic of dissolving at high temperature and hardening at low temperature, it must be encapsulated at high temperature, and thus, a high temperature unstable active ingredient may have a big disadvantage. Gelatin is inconvenient to dissolve in a solvent and then used through a capillary tube, and the method is difficult, and is mainly applied to soft capsules in pharmaceuticals.

Accordingly, the present inventors have repeatedly studied to solve the above problems, by first encapsulating a water-soluble or oil-soluble active substance for cosmetics into liposomes and then encapsulating a second matrix using chitosan to form a double multicapsule structure. It has the advantage of increasing the stability of water-soluble or oil-soluble active substances, and its efficacy in making functional cosmetics for protecting the skin is superior to existing products, and also freely controlling the particle size of the capsule in various formulations. It has been found that the product can be commercialized to complete the present invention.

Accordingly, an object of the present invention is to increase the stability of water and oil-soluble active ingredients by encapsulating cosmetic active ingredients which are easily oxidized or decomposed in aqueous solution, oil-soluble solution or air into MLV (Multi-Lamellar Vesicles) liposomes and chitosan. It is to provide a double capsule that can be formulated.

Still another object of the present invention is to provide a cosmetic composition containing the cosmetic double capsule.

1 is a schematic diagram of a double capsule manufacturing apparatus used in the present invention,

2 is a graph showing the results of analyzing the stability of vitamin A palmitate by HPLC,

3 is a graph showing the results of analyzing the stability of the vitamin C derivatives by HPLC,

4 is a graph showing the results of analyzing the stability of vitamin A acetate by HPLC,

5 is a graph showing the results of analyzing the stability of the retinol by HPLC,

Figure 6 is a graph showing the results of analyzing the stability of retinic acid by HPLC.

Explanation of symbols on the main parts of the drawings

1 pressure gauge, 2 N ₂ springs,

3 homogenizers, 4 chitosan-containing MLV liposomes,

5 nozzles, 6 10% sodium hydroxide solution,

7 MLV liposome primary capsule, 8 chitosan matrix secondary capsule.

Cosmetic double capsule of the present invention for achieving the above object is characterized in that it is prepared by liposomes of water-soluble or oil-soluble active substance, and then formed a matrix double capsule film using chitosan.

EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.

Matrix double capsules of liposomes and chitosan of the present invention can be prepared by the following method. First, MLV liposomes are made because they can most effectively increase the affinity with the skin. In addition, minimizing the particle size of MLV liposomes is of paramount importance to increase penetration of the skin. A proper amount of phospholipids, ceramides, and vegetable oils obtained from soybeans are mixed and dissolved at a melting point or higher, and the aqueous phase in which glycerin and diethanolaminecetyl phosphate is dissolved is wetted at 80 to 100 ° C., cooled and cooled to form a water-soluble active ingredient, vitamin C derivatives. A suitable amount of the active ingredient, vitamin A palmitate, is added and dispersed homogeneously, and then passed through a microfluidizer to form a liposome base (primary capsule). Here, since the particle size of the capsule may vary depending on the number of times and the pressure passed through the microfluidizer, an appropriate condition should be set. Therefore, the proper conditions in the present invention are preferably 1 to 5 times of passage times and 300 to 500 psi of passage pressures. When mixing water and oil-soluble active ingredients at high temperatures, it is most preferable to use an ultrasonic method or a microfluidizer in order to stably reduce the unstable substances having low titers to the particle size.

To make secondary matrix capsules with primary MLV liposome capsules, first dissolve 1 to 10% by weight of chitosan in lactic acid, malic acid, tartaric acid, and glycolic acid, and then first MLV liposomes from 1% to as much as 10% in an amount. Mix with the capsule. Dropping this mixture into a pre-made 10% NaOH solution produces a microscopic spherical capsule. This can be made up to 0.01mm ~ 5mm or more depending on the size of the nozzle, and the change in the hardening of the film is determined according to the content of chitosan, so the NaOH content should be properly adjusted.

Cosmetic double capsule of the present invention can be manufactured in a capsule manufacturing apparatus or a similar manner as shown in Figure 1, when explaining the manufacturing process as follows. When nitrogen is bombarded and pressurized in the tank containing MLV liposome base through a certain nozzle (Φ: 100-300μm) and the contents are dropped into sodium hydroxide solution, the chitosan inside the liposome is changed to basic. While hardened to chitosan membrane. Thus, retinol derivatives and vitamin C derivatives in liposomes are stably present in ceramides and phospholipids in small sizes (100-200 nm), and the second matrix encapsulation method with chitosan membrane to protect the liposomes once more and increase the stability. to be. This technology is not yet known, and it is expected that many studies will be made in cosmetics as well as in the future.

There are many ways to make liposomes, but the method used here is a difficult technique compared to the general method, but it has excellent advantages in terms of quality and safety. Many raw materials are commercialized by encapsulating only liposomes, but there are still many problems in securing stability in aqueous solutions, useful solutions or air. When the unstable cosmetic ingredients are double matrix capsules by the method used in the present invention, it is possible to secure a good stability several times more than just stabilizing with liposomes. As a result, securing stability is consistent with enhancing efficacy.

Although the double capsule for cosmetics of this invention is not specifically limited, For example, it is preferable that raw materials, such as an unstable retinol derivative and a water-soluble vitamin C derivative, are contained in the quantity of 0.1-50 weight% in heat or air | atmosphere.

In addition, although the primary MLV liposome capsule in the cosmetic double capsule of this invention is not limited, it is suitable to contain 1-20 weight% of phospholipid components extracted from the bean, and 0.01-0.5 weight% of ceramide. Since the particle size of the liposome is different depending on the content of the vegetable ester oil, it is necessary to select an appropriate oil when applying to cosmetics. Therefore, in the present invention, jojoba oil, macadamia oil, meadow oil, rose oil, olive oil, squalene, coconut oil and the like are preferably contained in an amount of 3 to 40% by weight. In addition, a certain amount of tocopherol is excellent in the oxidation stability of the liposome base, 0.01 to 5% by weight is the most suitable content for making liposomes.

When the matrix double capsule is used for cosmetics, the most suitable ingredient is chitosan. Chitosan capsules are most preferred because they are superior in skin affinity and excellent in skin safety or skin moisturizing power than those used in general capsules such as sodium alginate, gelatin gum, agar and the like. In particular, chitosan is effective above all because it is already known as a raw material having excellent self-preservation ability. In the present invention, after special encapsulation in the form of MLV liposomes, which are not general O / W emulsion form or W / O emulsion form, chitosan using AHA as a solvent is used. Rather, it is an advanced technology.

Hereinafter, the present invention will be described in more detail with reference to Examples.

Example

(Method for preparing MLV liposome)

The raw materials 1 to 3 shown in Table 1 were weighed in a separate beaker, heated and dissolved at 90 to 105 ° C., then cooled to 80 ° C., and the raw materials 4 to 7 were heated and dissolved at 80 ° C. to prepare the raw materials 1 to 3 and After mixing, the mixture is sealed and allowed to wet for 30 minutes. It is then cooled to 40 ° C., mixed with 8-11 raw materials, dispersed for 3 minutes with a homomixer, and then passed through a microfluidizer to prepare an MLV liposome (primary capsule). At this time, when using a microfluidizer, if the appropriate optimum conditions are set, a more excellent capsule can be obtained. Therefore, the number of passages used in the present invention is 1 to 5 times, the passing pressure is a suitable condition 300 to 500 psi.

In addition to the examples in the present embodiment, it should be noted that liposomes having different composition ratios can be obtained according to separate content changes.

Table 1 Formulation Table of MLV Liposome Primary Capsules

(Unit: weight%)

Raw material name Formulation Example 1 Formulation Example 2 Formulation Example 3 Formulation Example 4 Formulation Example 5 Formulation Example 6 1. Soy Phospholipids 1.0 3.0 6.0 10.0 15.0 20.0 2. Ceramide 0.01 0.1 0.2 0.3 0.4 0.5 3. Jojoba oil 5.0 10.0 10.0 10.0 10.0 15.0 4. Glycerin 5.0 7.0 10.0 10.0 10.0 10.0 5. D. Acetylphosphate 0.5 0.8 1.0 1.0 1.0 1.0 6. Purified water to 100 to 100 to 100 to 100 to 100 to 100 7. Vitamin C Derivatives 0.5 1.0 1.0 2.0 2.0 2.0 8. Purified water 5.0 5.0 5.0 5.0 5.0 5.0 9. Vitamin A Palmitate 1.0 2.0 3.0 4.0 5.0 5.0 10. Vitamin A Acetate 1.0 2.0 3.0 4.0 5.0 5.0 11.ethanol 5.0 5.0 10.0 10.0 10.0 5.0

Liposomes were rarely generated when the content of the phospholipid base was 1.0 wt% (Formulation Example 1), and sufficient liposomes were made at 20 wt% (Formulation Example 6). Ceramide formed stable liposomes at a content of 0.01-0.5% by weight, but the multilamellar form was superior as the content increased. The content of ceramide in general cosmetics is known to be 0.05 to 0.1% by weight.

(Manufacturing method of chitosan matrix double capsule)

As shown in Table 2 below, the primary MLV liposome (raw material 1) was accurately weighed in a 1 liter beaker, mixed with chitosan and lactic acid, and then mixed with a homomixer in a range of 1 to 10 minutes to allow sufficient dispersion. Stir. At this time, the stirring speed varies depending on the amount of contents, but in general, stirring at 1,000 to 2,000 rpm is appropriate. The resulting mixture was dropped in a 10% NaOH solution stored in a separate 1 liter beaker to prepare a chitosan matrix double capsule.

[Table 2] Component Composition Table of Chitosan Matrix Secondary Capsules

(Unit: weight%)

Raw material name Example 1 Example 2 Example 3 Example 4 Example 5 1.MLV Liposomes (Formulation Example 3) 97.0 95.0 93.0 90.0 85.0 2. Chitosan (10% solution) 3.0 5.0 7.0 10.0 15.0

The preparation example of the cream in the cosmetics containing the double capsule of this invention is shown by the manufacture example below.

Production Example

As shown in Table 3 below, it is prepared in the same manner as described in the above examples to test the recovery of the chitosan double capsule as the same base by applying a certain amount of various retinol derivatives applied to the cream of cosmetics.

After dissolving the oil phase containing 10.0% by weight of phospholipid and 0.1% by weight of ceramide at 80 ° C. or higher, the components dissolved in the aqueous phase, such as glycerin and diethanolamine cetyl phosphate, are weighed and dissolved in a water phase at 80 ° C. or higher and mixed and homogenized together with the oil phase. do. Subsequently, the mixture was cooled to 40 ° C., and each vitamin derivative was mixed in amounts to pass through a microfluidizer to make a primary MLV liposome capsule, which was mixed with a chitosan solution and stirred, and then dropped in an aqueous sodium hydroxide solution to base the chitosan. Make a matrix double capsule. At this time, the inner diameter of the nozzle used was 150㎛, but the size of the nozzle can be freely adjusted to make the capsule to the desired size.

TABLE 3

(Unit: weight%)

Furtherance Preparation Example 1 Preparation Example 2 Preparation Example 3 Preparation Example 4 1. Soy Phospholipids 10.0 10.0 10.0 10.0 2. Ceramide 0.1 0.1 0.1 0.1 3. Jojoba oil 10.0 - - - 4. Glycerin 7.0 7.0 7.0 7.0 5. D. Acetylphosphate 0.5 0.5 0.5 0.5 6. Squalane - 10.0 - - 7. Macadamia Oil - - 10.0 - 8. Olive Oil - - - 10.0 9. Meadowfoam oil - - - - 10. Purified Water to 100 to 100 to 100 to 100 11.Vitamin C Derivatives 0.5 0.5 0.5 0.5 12. Vitamin A Palmitate 0.5 - - - 13. Vitamin A Acetate - 0.5 - - 14. Retinol - - 0.5 - 15. Retinic acid - - - 0.5 16. Ethanol 5.0 5.0 5.0 5.0 17. Chitosan (10% solution, solvent: lactic acid) 5.0 5.0 5.0 5.0 18. Lubrajel MS 10.0 10.0 10.0 10.0

According to the composition of Table 3, the general O / W method, W / O method and liposome method, and the chitosan double matrix method according to the present invention having a sample prepared by the stability of the vitamin derivative and retinol derivatives easily decomposed in the atmosphere The test results are shown in Table 4 below.

Comparative Production Example 1 (O / W Emulsification Method)

The composition shown in Table 3, but instead of soy phospholipid and ceramide, polysorbate 60 1.0% by weight as an emulsifier to make an emulsion with the same content, emulsified at 3,000 rpm for 3 minutes at 80 ℃ and cooled to 40 ℃ Next, water-soluble or oil-soluble retinol derivatives were added to each other to carry out the comparative experiments.

Comparative Production Example 2 (W / O Emulsification Method)

To the composition as shown in Table 3, but instead of soy phospholipids and ceramides, 1.5 wt% of sorbitan sesquioleate was used as an emulsifier to make an emulsion. The emulsion was emulsified at 3,000 rpm for 3 minutes at 80 ° C. and then cooled to 40 ° C. Then, water-soluble or oil-soluble retinol derivatives were added to each other, and then run as comparative experiments.

Comparative Production Example 3 (Liposome Method)

The composition as shown in Table 3, but was prepared only by the liposome method, not chitosan matrix capsules were tested in a comparative experiment.

[Table 4] Stabilization test results of water and oil-soluble active substances for cosmetics

(Detection content (% by weight) (recovery rate (%)))

Raw material name Content (% by weight) O / W emulsification W / O emulsification Liposome method Double Capsule Vitamin A Palmitate 0.5 0.18 (36) 0.20 (40) 0.30 (60) 0.46 (92) (Manufacturing Example 1) Vitamin A Acetate 0.5 0.22 (44) 0.24 (48) 0.32 (64) 0.47 (94) (Manufacturing Example 2) Vitamin C derivatives 0.5 0.13 (26) 0.19 (38) 0.25 (50) 0.43 (86) (Manufacturing Example 1) Retinol 0.5 0.16 (32) 0.18 (36) 0.28 (56) 0.46 (92) (Manufacturing Example 3) Retinic acid 0.5 0.20 (40) 0.22 (44) 0.31 (62) 0.43 (86) (Manufacturing Example 4)

(Note) The result is the result of quantitative analysis by HPLC after 6 weeks at 35 ℃ after sample preparation.

As shown in Table 3, unstable substances were prepared in various ways, and then stored in a 35 ° C thermostat for 6 weeks and analyzed by high performance liquid chromatography. The recoveries of cosmetic water and oil-soluble active ingredients were 26-44%, 36-48% in W / O mode and 50-64% in liposome mode. However, in the matrix double capsule method using chitosan, the overall recovery rate is 86-94%, so even if it is an unstable substance in the air, it is thought that the best effect on stability can be obtained by using this method. After storage for 30 days in a 35 ℃ thermostat, the results of HPLC analysis of the vitamin derivatives and retinol derivatives are shown in Figures 2-6.

As described above, it is considered that the cosmetic composition according to the present invention is a method for imparting many techniques for the development of functional cosmetics in cosmetics, and the stability of the vitamin derivative and the retinol derivative by the chitosan matrix double capsule method of the present invention is Compared to the general O / W, W / O, liposome method, it can be seen that it is very high. In the future, the present invention is expected to be applied to a lot of applications by appropriately utilizing the drug delivery system as well as cosmetics.

Claims (3)

Cosmetic capsules containing a water-soluble or oil-soluble active substance, wherein the water-soluble or oil-soluble active substance is prepared by liposomes to form a multi-lamellae vesicle (MLV) liposome, and then a matrix double capsule film is formed using chitosan. Cosmetic double capsule characterized in that. The cosmetic double capsule according to claim 1, wherein the chitosan is contained in an amount of 1 to 15% by weight. A cosmetic composition comprising a double capsule for cosmetic according to claim 1.