JP2014527989A - Microemulsion containing button extract and its preparation method and application - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a microemulsion containing a button extract and a preparation method and application thereof. SOLUTION: A method for preparing a microemulsion containing a button extract, wherein the button extract is mixed with water, hydrogenated lecithin and an oil phase at a weight ratio of 1: 5 to 1:12. The mixed hydrogenated lecithin is mixed at a shear rate of 100 to 800 m / s for 10 to 60 minutes under a concentration of 1 to 50 wt% and 50 to 500 atm. The microemulsion obtained by this method has good stability, is easy to use, and can be used for the production of cosmetics and skin care products. [Selection figure] None

Description

  The present invention relates to plant extracts, and in particular to microemulsions containing button extracts that can be used for gene regulation and also in cosmetics.

  The button is a traditional Chinese medicine, and according to the description of the Chinese Pharmacy, the roots, leaves and flowers of the button can also be used as a Chinese medicine. The operation in the beauty skin care aspect can also be traced back to the age. For example, beauty prescriptions containing button skins, button flower slices, etc. are written in old books, such as 《Outside Secret Secretary》 and 《Gion Essentials》. ing.

  The button is still used for cleaning cosmetics such as shampoo (Patent Document 1) and whitening cream (Patent Document 2), but there are defects in the extraction process, stability protection, effect verification, etc. doing.

  Button oil-soluble and water-soluble extracts have different effects and differ in solubility, making it difficult to add simultaneously to the formulation of a cosmetic or skin care product. Or they must be added in different steps in the process of preparing cosmetics and skin care products.

  The present invention is designed for systematic processes and verification methods to extract all the active ingredients of buttons, and to protect the stability by using physical technology to facilitate the use in cosmetics. In addition, the DNA microarray technology can quickly and accurately confirm the action of the button extract and other active substances on the gene regulation surface, and can find the optimum blending range.

Chinese application 200000098833.2 Chinese application 200510000271.8

  It is an object of the present invention to provide a microemulsion containing a button extract and a method for preparing the same.

  The present invention uses a microemulsion containing the above button extract for the preparation of a gene regulatory complex.

  Another object of the present invention is to produce a microemulsion containing the above button extract for the production of cosmetics and skin care products.

  The weight ratio of the button extract to water is 1: 5 to 1:12, and the button extract, water, hydrogenated lecithin and oil phase are mixed, and the concentration of hydrogenated lecithin after mixing is 1 wt% to 50 wt%. Then, the concentration of the oil phase is 1 wt% to 50 wt%, and the mixture is mixed for 10 to 60 minutes at a shear rate of 100 to 800 m / s under 50 to 500 atm.

  The oil phase can be selected from any of silicon oil, mineral oil and hydrogenated polyisobutene.

  The method for preparing the button extract includes the step (1) of drying the water content of the button (including roots, stems, leaves and flowers) to <10% and crushing to 30-50 mesh, petroleum ether, normal Extraction by solid-liquid separation over 2-8 hours at 30-90 degrees Celsius using hexane or ethanol (2), and recovering the solvent in the liquid part (solvent residual amount <0.1%) and button The oil-soluble component is obtained, and water for solid residue is extracted by solid-liquid separation at 30 to 90 degrees Celsius for 1 to 4 hours, and the liquid part is concentrated to obtain an extract. A step (3) of obtaining, and a step (4) of mixing the oil-soluble component and the water-soluble component of the button.

  The microemulsion containing the button extract obtained by the above method has a particle size of 1000 to 2000 nm, and the content of the button extract is 1% to 25%.

  The microemulsion containing this button extract contains the extract of the water-soluble component and oil-soluble component of the button at the same time, and can be used for the manufacture of skin care products and cosmetics. High stability as skin care products and cosmetics. The amount of microemulsion containing the button extract used in skin care products and cosmetics is 0.1 wt% to 10 wt%.

  By blending this button extract with a microemulsion and other substances, genes that form melanin, genes that are related to the moisturizing ability of the skin, genes that are related to the improvement of skin aging, and to the skin It is possible to regulate the expression level of genes related to relaxation of stimulation.

  An advantage of the present invention is that the water-soluble component and oil-soluble component of the button are prepared in a microemulsion to improve stability and ease of use. Using this microemulsion to produce cosmetics and skin care products can effectively moisturize, reduce melanin, improve skin aging, and alleviate skin irritation.

  Hereinafter, in order to make the features and effects of the present invention clearer and easier to understand, examples will be described along with examples.

  The moisture content of the buttons (including roots, stems, leaves, flowers) was dried to <7% and ground to 20 mesh.

  Extraction was performed by solid-liquid separation using ethanol as a solvent at 60 degrees Celsius for 6 hours. The liquid portion was distilled to remove the solvent, and the solvent was recovered (residual solvent amount <0.1%) to obtain an oil-soluble component of the button.

  Water for solid residue was extracted by solid-liquid separation at 70 degrees Celsius for 3 hours, and the liquid part was concentrated to obtain an extract, thereby obtaining a water-soluble component of the button.

  The water-soluble component and oil-soluble component of the button were mixed.

  Ethanol can be replaced with petroleum ether or normal hexane, and similar results can be obtained.

  10 kg of water was added to 1 kg of a mixture of the oil-soluble component and the water-soluble component of the button obtained in Example 1. Further, 4 kg of hydrogenated lecithin and 5 kg of silicon oil were added to obtain a mixed solution. The mass concentrations in the mixed solution of hydrogenated lecithin and silicone oil were 20% and 25%, respectively.

  The mixed solution was put into a stainless steel container, a pressure of 500 atm was applied, and the mixture was mixed at a shear rate of 500 m / s for 40 min to form a microemulsion, and a microemulsion containing a button extract was obtained. The final product particle size ranged from 1000 to 2000 nm and the button extract content was 5 wt%. Silicone oil can be replaced by mineral oil, with similar results.

  The microemulsion obtained by the above preparation was added to the emulsion and the cream substrate to form an experimental group with an addition amount of 10%. At the same time, a commercially available button extract that was not microemulsified was added to the same emulsion and cream substrate to form a control group with an addition amount of 0.5%. A milk and cream substrate with nothing added was blank.

  Samples from the experimental group and the control group were placed in transparent plastic bottles, irradiated with light for 24 hours, and subjected to a load test at 40 degrees Celsius for 4 weeks. The blank was stored in a cool shade. Forty volunteers evaluated the color and smell. All volunteers compared the experimental group with the blank and answered “no change in tint / smell” or “slight change in tint / smell”. All the volunteers compared the blank with the control group and answered, “A great change in both color and odor”. All volunteers replied that “the appearance and smell of the experimental group was superior to the control group”.

  7.8 kg of water was added to 1.2 kg of the mixture of the oil-soluble component and the water-soluble component of the button obtained in Example 1. Further, 0.5 kg of hydrogenated lecithin and 0.5 kg of silicon oil were added to obtain a mixed solution. The mass concentrations in the mixture of hydrogenated lecithin and silicone oil were 5% and 5%, respectively.

  The mixed solution was put into a stainless steel container, a pressure of 5 atm was applied, and the mixture was mixed at a shear rate of 800 m / s for 60 minutes to form a microemulsion to obtain a microemulsion containing a button extract. The final product particle size was in the range of 1000-2000 nm, and the button extract content was 12 wt%.

  7.8 kg of water was added to 1.2 kg of the mixture of the oil-soluble component and the water-soluble component of the button obtained in Example 1. Further, 0.5 kg of hydrogenated lecithin and 0.5 kg of hydrogenated polyisobutene were added to prepare a mixed solution. The mass concentrations in the mixed solution of hydrogenated lecithin and hydrogenated polyisobutene were 5% and 5%, respectively.

  The rest of the procedure was the same as in Example 3, and a microemulsion containing button extract was obtained. The final product particle size was in the range of 1000-2000 nm, and the button extract content was 12 wt%.

When a human epidermal keratinocyte (HEK) culture is inoculated into a 6-well plate, the density is about 20000 cells / cm ² , and when the cell fusion rate reaches 70%, dividing into at least two groups (1).

  One of these is added with an active ingredient containing button extract and treated for 24 hours. Add the microemulsion containing the button extract of Example 3 or 4 and undecylenoylphenylalanine (product of SEPPIC), dilute using DMEM and finally the microemulsion containing the button extract in the cell line Step (2) in which the concentration of the solution is 3 wt%, undecylenoylphenylalanine is 1 wt%, and the other is the control (add blank medium).

  After collecting the cells, RNA is isolated, RNA is transformed into cDNA, the resulting cDNA is amplified with T7 RNA polymerase, and cytidine triphosphate using anthocyanin-3 or anthocyanin-5 fluorescent labels The labeled cDNA is hybridized onto a DNA microarray slide, and the DNA microarray slide is scanned using Agilent's dual channel laser detection DNA microarray scanner system. The laser wavelength for Cy3 labeling is 532 nm. The laser wavelength of Cy5 label is 633 nm, the fluorescence intensity is recorded, and data analysis is performed (3).

  As a result, GM-CSF (reducing expression 20 times), glutaredoxin (raising expression 38 times), thioredoxin reductase 1 (raising expression 24 times), etc. Could be adjusted.

  The cell culture and detection method is the same as in Example 5. In step (2), the microemulsion containing the button extract of Example 3 or Example 4 and vitamin C are added, and finally the button is extracted from the cell line. The concentration of the microemulsion containing the product is 3 wt% and vitamin C is 0.5 wt%.

  As a result, GM-CSF (reducing expression 30 times), glutaredoxin (raising expression 16 times), thioredoxin reductase 1 (raising expression 10 times), and the like, the expression level of genes related to melanogenesis is effectively reduced. Could be adjusted.

  The cell culture and detection method was the same as in Example 5. In step (2), the microemulsion containing the button extract of Example 3 or Example 4 and the pansy extract (product of Silab, France) were added. The concentration of the microemulsion containing the button extract in the cell line is 1 wt%, and the pansy extract is 1 wt%.

  As a result, effectively regulate the expression level of genes related to skin moisturizing ability, such as Desmocollin3 (Raise expression 18 times), Filagrin (Raise expression 4 times), AQP3 (Raise expression 2 times) I was able to.

  The cell culture and detection method is the same as in Example 5. In step (2), the microemulsion containing the button extract of Example 2 and Inond extract (BASF product) are added, and finally the button in the cell line is added. The concentration of the microemulsion containing the extract is 3 wt%, and the inondo extract is 1 wt%.

  As a result, MMP1 (reducing expression by 30%), MMP2 (reducing expression by 90%), LOXL-8 (raising expression by 2 times), COL1A2 (raising expression by 60%), etc. The expression level of a gene could be effectively controlled.

  The cell culture and detection method was the same as in Example 5. In step (2), a microemulsion containing the button extract of Example 2, dipotassium glycyrrhizinate and bisabolol was added, and finally the button extract in the cell line. The concentration of the microemulsion containing 1.5 wt%, dipotassium glycyrrhizinate 0.5 wt%, and bisabolol 0.5 wt%.

  As a result, it was possible to effectively regulate the expression level of genes such as IL-18 (reducing expression by 90%), Caspase1 (reducing expression by 4 times), and the like, which are related to relaxation of skin irritation.

  Examples 10 to 15 are used for the production of cleansing products, beauty products, cream products and lotions using the microemulsions containing the button extracts obtained in Examples 2 to 4, respectively.

  Preparation of cleansing products

  Beauty product preparation

  Cream product preparation

  Cream product preparation 2

  Preparation of lotion

  Preparation of emulsion

Claims (7)

  The weight ratio of the button extract to water is 1: 5 to 1:12, and the button extract, water, hydrogenated lecithin and oil phase are mixed, and the concentration of hydrogenated lecithin after mixing is 1 wt% to 50 wt%. A method for preparing a microemulsion containing a button extract, characterized in that the oil phase concentration is 1 wt% to 50 wt% and mixing is performed at a shear rate of 100 to 800 m / s under 50 to 500 atm for 10 to 60 minutes .   The method for preparing a microemulsion containing a button extract according to claim 1, wherein the oil phase is one of silicon oil, mineral oil, or hydrogenated polyisobutene. (1) drying the button moisture content to <10% and crushing to 30-50 mesh;
(2) a step of extracting by solid-liquid separation using petroleum ether, normal hexane or ethanol at 30 to 90 degrees Celsius for 2 to 8 hours;
The solvent in the liquid part is recovered (solvent residual amount <0.1%) to obtain an oil-soluble component of the button, and water for solid residue is obtained by solid-liquid separation at 30 to 90 degrees Celsius for 1 to 4 hours. Extracting and concentrating the liquid portion into an extract to obtain a water-soluble component of the button (3);
A step (4) of mixing the oil-soluble component and the water-soluble component of the button;
A method for preparing a microemulsion comprising a button extract according to claim 1.   A microemulsion containing a button extract, characterized by being prepared by the method according to any one of claims 1 to 3.   The microemulsion containing the button extract according to claim 4, wherein the microemulsion is applied to the manufacture of skin care products and cosmetics.   The microemulsion containing a button extract according to claim 5, wherein the amount of the microemulsion containing the button extract is 0.1 wt% to 10 wt%.   Prepare a gene regulatory complex that is the expression level of genes that form melanin, genes that are related to the skin's moisturizing ability, genes that are related to improving skin aging, and genes that are related to alleviating skin irritation A microemulsion comprising the button extract according to claim 4, wherein the microemulsion comprises a button extract.