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CN-122011797-A - Method for preparing morin from black rose and application of morin in whitening cosmetics

CN122011797ACN 122011797 ACN122011797 ACN 122011797ACN-122011797-A

Abstract

The invention provides a method for preparing morin from black rose and application of morin in whitening cosmetics, and belongs to the technical field of extraction of active ingredients. The method comprises the steps of (1) weighing black rose sample powder, adding ethanol for water bath extraction, centrifuging after extraction is finished to obtain supernatant, (2) drying the supernatant to obtain black rose crude extract, (3) carrying out column elution separation on the black rose crude extract, carrying out rotary evaporation and drying to obtain macroporous resin extract, and (4) purifying the macroporous resin extract to obtain the black rose purified product, namely the morin.

Inventors

  • ZHANG HUIMIN
  • SHAO QI
  • ZHANG XUEQIN
  • SONG SHUANGSHUANG
  • ZHANG LIMEI
  • ZOU PENGFEI
  • XING YAN

Assignees

  • 国珍健康科技（北京）有限公司

Dates

Publication Date
20260512
Application Date
20260202

Claims (10)

  1. 1. A method for preparing morin from black rose is characterized by comprising the following steps: (1) Weighing the black rose sample powder, adding ethanol for water bath extraction, and centrifuging after the extraction is finished to obtain a supernatant; (2) Drying the supernatant obtained in the step (1) to obtain a crude extract of black-red rose; (3) Re-dissolving the crude extract of black rose obtained in the step (2) by using ethanol, eluting and separating by a column, and performing rotary evaporation and drying to obtain a macroporous resin extract; (4) Adding ethanol into the macroporous resin extract prepared in the step (3) for redissolving, and then purifying to obtain an ink red rose purified product, namely the morin; The column separation in the step (3) is carried out by adopting AB-8 as macroporous resin column and adopting water-ethanol as mobile phase, the elution is carried out by adopting water, 30% ethanol, 60% ethanol, 80% ethanol and 100% ethanol respectively for gradient elution, and 60% ethanol eluent is collected.
  2. 2. The method according to claim 1, wherein the ethanol in step (1) has a volume fraction of 55-65%, preferably 60%.
  3. 3. The method according to claim 1, wherein the ratio of the sample powder to ethanol in step (1) is 1g:10-20mL, preferably 1g:15mL.
  4. 4. The method according to claim 1, wherein the water bath extraction temperature in step (1) is 55-70deg.C, the extraction time is 60-100min, and the number of extraction times is 1-3.
  5. 5. The method according to claim 1, wherein the centrifugation in step (1) is carried out at a rate of 4000 to 6000 r/min for a period of 8 to 15min.
  6. 6. The method according to claim 1, wherein the ethanol in the step (3) has a volume fraction of 55 to 65%.
  7. 7. The method according to claim 1, wherein the purification in the step (4) is performed by: PrePulite XP C18 is taken as a semi-preparation chromatographic column; Acetonitrile is taken as a mobile phase A,0.2 percent phosphoric acid is taken as a mobile phase B for gradient elution ,0-1 min,5% A;1-2 min,5% →10% A;2-8 min,10% →11% A;8-11 min,11% →15% A;11-14 min,15% A;14-16 min,15% →19% A;16-19 min,19% A;19-25 min,19%→40% A; The flow rate is 5 mL/min; the column temperature is 35 ℃; The detection wavelength is 254 nm; the sample injection volume is 500 mu L; collecting the eluent with retention time of 19-20 min, and blowing and drying the eluent with liquid nitrogen to obtain the morin.
  8. 8. A morin obtainable by the process of any one of claims 1 to 7.
  9. 9. Use of the morin prepared by the method of any one of claims 1 to 7 in the preparation of whitening cosmetics.
  10. 10. A cosmetic with whitening effect is characterized by comprising the morin prepared by the method of any one of claims 1-7 and acceptable auxiliary materials in cosmetics.

Description

Method for preparing morin from black rose and application of morin in whitening cosmetics Technical Field The invention belongs to the technical field of extraction of active ingredients, and particularly relates to a method for preparing morin from black rose and application of morin in whitening cosmetics. Background Skin pigmentation and melanin overproduction are core problems to be solved in the field of whitening and skin care. Tyrosinase is used as a key speed limiting enzyme in the melanin synthesis process, so that the tyrosinase becomes a key action target point for developing a whitening product, and searching for a safe and efficient tyrosinase inhibitor becomes a main research and development strategy in the field. The main stream of the current market comprises whitening components such as vitamin C and derivatives thereof, arbutin, nicotinamide and the like, but the main stream of the current market still has the limitations of poor stability, slow effect, easy skin irritation under high concentration and the like. Glabridin is taken as a high-efficiency whitening component extracted from glabra liquorice, and is known as whitening gold due to the excellent tyrosinase inhibition effect, but the glabridin is expensive and limited in source, so that the industrial application of glabridin is severely restricted. Therefore, developing a novel natural whitening ingredient with a stable source and controllable cost, which has a better effect than glabridin, becomes a technical bottleneck that the art is urgent to break through. The rose flowers are used as traditional medicinal and edible plants, are rich in flavonoids, polyphenol compounds, vitamins and the like, are often added in the form of an extract in cosmetics, and mainly play the roles of fragrance, moisture preservation and basic antioxidation. For example, chinese patent CN120391663A discloses a preparation method and application of rose extract, which utilizes microbial fermentation technology to increase the content of water-soluble vitamins in rose. The method selects lactobacillus plantarum, saccharomyces cerevisiae and bacillus subtilis as strains, adjusts the proportion of the strains to ensure that the proportion of the viable count of the lactobacillus plantarum, the saccharomyces cerevisiae and the bacillus subtilis is (1-3): (1-2): (1-2), forms a composite microbial inoculum, and adds pretreated rose to carry out sectional fermentation. Finally, the content of water-soluble vitamins in the rose extract is improved, so that the total antioxidant activity is improved by about 35 percent while the rose polysaccharide substances are reserved. The flos Rosae Rugosae extract is suitable for providing raw materials for functional food, health product and cosmetics. However, the prior researches have obvious limitations that firstly, the exploration of the whitening efficacy of the roses is stopped at the level of crude extracts, systematic comparison of efficacy differences among different varieties is lacking, secondly, core whitening efficacy factors of the roses cannot be deeply separated and identified, so that the efficacy of the products is undefined and the quality is uncontrollable, and finally, the efficacy evaluation system is imperfect, and the system verification from tyrosinase inhibition to cell-level melanin production inhibition is lacking, so that the whitening potential of the roses is difficult to convincingly prove. The prior art fails to disclose whether specific components which are comparable to glabridin exist in rose flowers or not, and also lacks a technical scheme for systematically screening and accurately positioning core whitening substances from multiple varieties. Therefore, there is a need to develop a method for preparing morin from black rose and its application in whitening cosmetics. Disclosure of Invention Based on the defects existing in the prior art, the invention provides a method for preparing morin from black rose and application of morin in whitening cosmetics. According to the invention, an activity tracking separation strategy is adopted, the black rose extract is directionally separated and purified by a modern preparation liquid chromatography technology, the key whitening active ingredient which is morin is successfully enriched and purified step by step from a complex matrix and is structurally identified, the primary definition of the morin is a core material foundation of the whitening effect of the black rose, and the comprehensive whitening effect of the morin from the black rose in inhibiting tyrosinase activity and blocking melanin generation is proved to be obviously superior to that of a positive control glabridin by an in-vitro melanoma cell model evaluation system, so that a scientific basis is provided for developing a glabridin alternative scheme with high efficiency and commercial feasibility. In order to achieve the above purpose, the present invention adopts the follo