KR970000739B1 - Lakes method for coloring material extracted from fruit (vaccinium vyrtillus) - Google Patents

Abstract

The lake method consists of; a) dissolving delphinidin or cyanidin pigments extracted from the fruit of Vaccinium vyrtillus, in alcohol,water or mixtrue thereof, b) adding soluble collagen salt sol'n adjusted pH 7.0~9.0 by alkali, c) reacting by mixing, and d) fixing by adding metal ions of polyvalent metal salts. This method provides purple,pink and green pigments which have a good coloring effect,dispersibility,stability to light,inhibition of skin dyeing and excellent stability to acid or alkali.

Description

Method of Raking of Bilberry Fruit Extract Pigment

The present invention relates to a method of laking a pigment (Delphinidin) or cyanidin (Cyanidin), which is a pigment extracted from the fruit of Vaccinium vyrtillus of the present invention, more specifically, a delphinidin or cyanidin by lake water-soluble collagen Therefore, the present invention relates to a method for producing purple, pink and green pigments excellent in color effect, usability, pigment dispersibility, light stability, skin dye removal, and stability against acid alkali.

Bilberry is a perennial shrub wild in the forests of northern Europe, and its fruit has been used for food for a long time.

In addition, in percutaneous absorption, it plays a role of trauma healing, delaying skin aging by strengthening crosslinking of skin collagen fiber, active oxygen absorbent, preservative and the like. These efficacies are attributed to anthocanoses, collectively referred to as flavonoids, which act as pigments capable of vivid colors and various color expressions in addition to the efficacies. However, these substances have been difficult to use as pigments because of their instability to acid alkali and instability to light.

Collagen, on the other hand, is an index of aging of skin as a protein in the body. Collagen in young people contains a lot of moisture, so it maintains elastic and smooth skin condition, but as it ages, the cross-linkage between collagen fibers increases and the water content decreases, which leads to rough and wrinkled skin.

On the other hand, there has been a method to rake the pigments commonly used in cosmetics with cellulose, but there has been no proposal to rake the pigments extracted from bilberry, and no proposal to rake the pigments using collagen. .

The present invention improves the problems such as instability to acid alkali, instability to light, dyeing on skin while maintaining excellent color of pigment (hereinafter referred to as delphinidin pigment) itself extracted from bilberry fruit. During the intensive study, the collagen is treated with alkali and the delphinidin pigment is adsorbed and quenched to solve the above problems, as well as the dispersibility of the pigment in the aqueous and oil phases, and the effect of delaying skin aging by water-soluble collagen. At the same time, the present invention has been found to be able to obtain cosmetic pigments of violet, pink, and green color with excellent usability.

Hereinafter, the present invention will be described in more detail.

Preferably, in the present invention, an aqueous solution of a water-soluble animal collagen salt in which a bilberry fruit extract pigment delfininidine or cyanidin is dissolved in alcohols, water or a mixture thereof, and an alkali such as sodium hydroxide is added thereto to adjust the pH to 7.0-9.0. It is added, and the resulting mixture is reacted under stirring, and then the method of lake bilberry fruit extract pigments comprising the step of immobilizing by adding a metal ion of a metal salt of a polyvalent metal salt.

The solvent used to dissolve the bilberry extract pigment in the present invention is not particularly limited, but alcohols such as ethanol, propanol, isopropanol, water, or mixtures thereof may be used. Particularly preferably a 70:30 to 30:70 weight ratio mixture of water and alcohol is used.

According to the method of the present invention, the delphinidin pigment is added to the above-described solvent to stir well to prepare a saturated solution, and then a small amount of alkali such as sodium hydroxide is added thereto to add an aqueous solution of the collagen salt having a pH above the isoelectric point, followed by stirring. React to bond. The amount of the collagen salt used at this time is preferably an amount of the ratio of the equivalent ratio of the delphinidin pigment to the collagen salt of 1: 1-5. The ionic compound obtained in the reaction varies in color depending on the pH. As the pH increases, violet, pink, and green colors can be obtained. That is, the pH ranges from about 7.0 to 8.0, which is purple, and is about 8.0 to 8.5. It is pink in the range and green in the range of 8.5 ~ 9.0.

The polyvalent metal salt was added to the ionic complex of delphinidin and collagen thus obtained and stirred to allow the metal ions to be ion-bonded to the unreacted ions in the ionic complex, followed by immobilization. Make up. The amount of water-soluble polyvalent metal salt added at this time is in the range of the ratio of the equivalent ratio of water-soluble collagen salt to metal salt is 1: 1.

Bilberry dry extract pigment used in the present invention is an Italian Indena (Indena) product commonly used as a pigment in the art, the trade name is BILBERRY DRY EXTRACT, the general formula is as follows :

Wherein R is OH or OMe, R ₁ is OH, R ₂ is H, OH or OMe and Glyc is glycoside.

In addition, the bilberry fruit extract pigment used in the present invention can be obtained as a powder by a conventional method such as dipping for a predetermined period of time using purified water, ethanol or a mixture thereof as a solvent and then evaporated to dry, optionally, It can be purified by conventional solvent extraction method or chromatography method.

As the polyvalent metal salt that can be used in the present invention, water-soluble polyvalent metal salts, such as calcium chloride, aluminum sulfate, barium chloride, and the like, which can undergo an ion-bonding reaction with the same equivalent as delphinidin-collagen ion binder, are used. When it is added to excess water and stirred, the polyvalent metal salt dissolves in water and dissociates and the metal ions are adsorbed onto the collagen surface.

The water-soluble collagen used in the present invention is a water-soluble collagen under the trade name ATELLO COLLAGEN as a product of KOKEN, which is commonly used in the art.

Purple, pink, and green pigments produced by the present invention have the following advantages over the bilberry extract pigments of the type.

First, when delphinidin itself is dissolved in water or an organic solvent, reddish-brown dark and dull undesirable color is expressed, but the rake pigmented pigment has a vivid and beautiful color.

Second, the pigments laked by the present invention is excellent in water dispersibility and oil dispersibility as compared to delphinidin, and there is no phenomenon that the pigments aggregate together.

Third, depending on the pH of the solution in the ion bonding reaction, it is possible to lake the violet, pink, green pigments, and the produced lake has no color change because of improved acid, temperature and light stability compared to delphinidin.

Fourth, it does not dissolve in oil or water and does not dye on the skin.

Fifth, collagen's aging retardation effect is maintained as it is, and has a unique feeling of use, so that the feeling is soft and the skin affinity is excellent.

The present invention will be described in more detail with reference to the following Examples, but the present invention is not limited to these Examples.

EXAMPLE

1 g of delphinidin is added to 300 g of a mixture of water and ethanol at a weight ratio of 70:30, and dissolved well. In addition, 20 g of commercially available water-soluble collagen (2%) is dispersed in 200 g of water, and then a small amount of caustic soda is added so that the pH is 7.0-9.0. Here, depending on the pH range, i.e., violet-based products in the pH range of about 7.0-8.0, pink-based products in the range of about 8.0-8.5, and green-based products in the range of about 8.5-9.0 are obtained.

The two solutions are mixed and stirred well. Then, ₄ g of aluminum sulfate (Al ₂ (SO ₄ ) ₃ , 16-8H ₂ O) 4g was added to excess warm water (50 ° C.), followed by stirring for about 30 minutes, followed by mixing of the dye and the collagen salt previously stirred therein. The precipitate formed by the addition of the solution was filtered, washed and dried to prepare a lake.

The rake pigment of the present invention prepared as described above and the existing pigments are delfinidine and cyanidin pigments used as raw materials in the present invention, and are products of SUN CHEMICAL of the United States of America. The physical properties of Red No. 202 were compared with Table 1 according to the method described below.

Evaluation standard

◎: Extremely good, ○: Good, △: Normal, X: Poor

Evaluation test method of Table 1 in the experiment is as follows.

1) Light stability: After dispersing a suitable amount of sample in an aqueous solution containing a small amount of polyoxyethylene sorbitan lauryl ester of pH 7.0, observe the color difference and state change while standing for a few days in sun and shade. .

2) Safety against acid alkali: After dispersing the sample in the above aqueous solution of pH 4.0-10.0 and shaking it, observe the change of color or smell of the sample dispersion.

3) Safety against Skin Dyeing: Dissolve or disperse the sample in the same amount, and apply a small amount to the skin. After a few hours, observe and evaluate the state of washing.

4) Dispersibility: Disperse the sample in water or oil under the same conditions and evaluate the degree of dispersion under a microscope.

Claims (4)

Dissolve the bilberry fruit extract delfinidin or cyanidin in alcohol, water or a mixture thereof, add an aqueous solution of a water-soluble animal collagen salt in which alkali is added to adjust the pH to 7.0-9.0, and the resulting mixture is reacted under stirring, Then, the method of lake raking the bilberry fruit extract, characterized in that the immobilized by adding a metal ion of a polyvalent metal salt. The method of claim 1, wherein the mixing ratio of water and alcohols is 70: 30-30: 70. The method according to claim 1, wherein the equivalent ratio of the bilberry fruit extract pigment and the water-soluble animal collagen is 1: 1-5. The method of claim 1, wherein the equivalent ratio of the salt of water-soluble animal collagen and the water-soluble polyvalent metal salt is 1: 1.