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CN-118078699-B - Pinus parviflora extract and preparation method and application thereof

CN118078699BCN 118078699 BCN118078699 BCN 118078699BCN-118078699-B

Abstract

The invention provides a pinus tenuifolia extract and a preparation method and application thereof, wherein the preparation method comprises the following steps of extracting pinus tenuifolia powder with alcohol, and concentrating the obtained extract under reduced pressure to obtain crude extract; centrifuging the crude extract, collecting a supernatant I, re-dissolving the precipitate, centrifuging, collecting a supernatant II, combining the supernatant I and the supernatant II to obtain a solution to be purified, carrying out sectional elution on the solution to be purified by using macroporous resin, collecting the eluent of the last section, concentrating and drying to obtain the lycopodium clavatum extract. The preparation method provided by the invention can effectively enrich saponins, flavonoids, polyphenols and lycoclavanin (pinocembrin) in pinocembrin, the active ingredients can be precisely controlled, the content is stable, and the prepared pinocembrin extract has good antioxidant effect and relieving effect and can be applied to cosmetics.

Inventors

  • CHEN WENJUN
  • YUAN YONGLEI
  • WU JIAHUI
  • LI JINGJING
  • QU LIPING
  • WANG FEIFEI
  • MA XIAO
  • GUO ZHENYU

Assignees

  • 云南贝泰妮生物科技集团股份有限公司
  • 云南云科特色植物提取实验室有限公司

Dates

Publication Date
20260505
Application Date
20240308

Claims (16)

  1. 1. A method for preparing a pinus tenuifolia extract, which is characterized by comprising the following steps: (1) Extracting the lycopodium clavatum powder by alcohol, and concentrating the obtained extracting solution under reduced pressure to obtain a crude extracting solution; (2) Centrifuging the crude extract, collecting a supernatant I, re-dissolving the precipitate, centrifuging, collecting a supernatant II, and combining the supernatant I and the supernatant II to obtain a solution to be purified; (3) The solution to be purified is subjected to sectional elution by macroporous resin, the eluent of the last section is collected, concentrated and dried, and the lycopodium clavatum extract is obtained; the extraction agent is ethanol water solution, the material-liquid ratio during extraction is 1 (5-10), the mass percentage of ethanol in the ethanol water solution is 60-80%, the extraction is independently carried out for 1-3 times, and the extraction time is respectively and independently 1-3 h; the macroporous resin is D-101 type macroporous resin; The sectional elution is sequentially carried out by adopting a solvent I, a solvent II and a solvent III; The solvent I is water, and the volume of the column is eluted for 2-5 times; The solvent II is ethanol water solution, the mass percentage of ethanol in the ethanol water solution is 15-25%, and the volume of the column is eluted by 3-8; The solvent III is ethanol water solution, the mass percentage of ethanol in the ethanol water solution is 80-90%, and the elution is carried out for 5-10 column volumes.
  2. 2. The method of claim 1, wherein the particles of the pinus parvifolia powder are 70-100 mesh in size.
  3. 3. The method according to claim 1, wherein the pinus radiata is a dried whole plant of pinus radiata of pinus genus of pinaceae family.
  4. 4. The method according to claim 1, wherein the reduced pressure concentration is at a temperature of 45 to 65 ℃.
  5. 5. The preparation method according to claim 1, wherein the mass ratio of the crude extract to the pinus parviflora powder is (0.5-1.5): 1.
  6. 6. The method according to claim 1, wherein in the step (2), the rotational speeds of the centrifugation are each independently 3000 to 16000 rpm.
  7. 7. The process according to claim 1, wherein the reconstitution is carried out using a solvent to crude extract volume ratio of (0.8-1.2): 1.
  8. 8. The preparation method according to claim 1, wherein the mass ratio of the macroporous resin to the pinus cassiabarka powder is (3-5): 1.
  9. 9. The method according to claim 1, wherein the loading rate at the time of the stepwise elution is 0.4 to 0.6 column volume/h.
  10. 10. The preparation method according to any one of claims 1 to 9, characterized in that the preparation method comprises the steps of: (1) Alcohol extraction is carried out on 70-100 meshes of larch powder, the feed liquid ratio is1 (5-10), the extractant is ethanol water solution with the mass percentage of 60-80%, the extraction is independently carried out for 1-3 times, the time of each extraction is 1-3 h, the obtained extract is decompressed and concentrated at 45-65 ℃ to obtain crude extract, and the mass ratio of the crude extract to the larch powder is (0.5-1.5): 1; (2) Centrifuging the crude extract 3000-16000 rpm, collecting supernatant I, re-dissolving the precipitate with 0.8-1.2 times of solvent, centrifuging 3000-16000 rpm, collecting supernatant II, and mixing the supernatant I and the supernatant II to obtain the solution to be purified; (3) The solution to be purified is subjected to sectional elution by adopting D-101 macroporous resin, the mass ratio of the macroporous resin to the spidroa casserosa powder is (3-5), the loading speed is 0.4-0.6 column volume/h, 2-5 column volumes are sequentially eluted by adopting water during sectional elution, 3-8 column volumes are eluted by adopting an ethanol aqueous solution with the mass percentage of 15-25%, 5-10 column volumes are finally eluted by adopting an ethanol aqueous solution with the mass percentage of 80-90%, the last section of eluent is collected, concentrated and dried, and the spidroa casserosa extract is obtained.
  11. 11. An extract of pinus parviflora, characterized in that it is prepared by the preparation method according to any one of claims 1-10.
  12. 12. The extract of pinus parviflora according to claim 11, wherein the mass percentage of saponins in the extract of pinus parviflora is up to 42.96%.
  13. 13. The extract of pinus parviflora according to claim 11, wherein the mass percentage of polyphenols in the extract of pinus parviflora is up to 12.67%.
  14. 14. The extract of pinus parviflora according to claim 11, wherein the extract of pinus parviflora comprises up to 10.48% by mass of flavonoids.
  15. 15. The extract of pinus parviflora according to claim 11, wherein the amount of lycoclavanin% by mass of the extract of pinus parviflora is up to 14.76%.
  16. 16. Use of an extract of pinus parviflora according to any one of claims 11 to 15 for the preparation of a cosmetic having antioxidant or soothing effect.

Description

Pinus parviflora extract and preparation method and application thereof Technical Field The invention belongs to the technical field of plant extraction, and particularly relates to a lycopodium clavatum extract and a preparation method and application thereof. Background Pinus parviflora (PALHINHAEA CERNUA (l.) et Franco) is a medium to large-sized earthy plant of pinus parviflora (PALHINHAEA FRANCO ET, vasc. Ex Vasc. Et Franco.) of the family pinaceae (Lycopodiaceae p. Beauv. Ex mirb.). Mainly distributed in south China, southwest and eastern China, etc., and the origin is China. In China, the plant mainly grows under forests, bushes or rocks with the altitude of 100-1800 m, and is distributed in regions such as Yunnan, guizhou, jiangxi, hunan and the like. The shisong is a traditional medicine, is one of plants from which the traditional Chinese medicine lycopodium clavatum is derived, can be used as the whole herb and spores, and has the effects of diminishing inflammation, stopping bleeding, clearing liver and improving vision according to the record of Luchuan herbal. Modern pharmacological researches have shown that Pinus koraiensis has effects of relieving fever, promoting blood circulation, removing liver-fire, removing toxic substances, promoting intestinal peristalsis, and improving sleep, and can be used for treating numbness of limbs, hematochezia, infantile convulsion, scald due to fire and water, traumatic injury, hepatitis, and rubella. It is also commonly used in clinic for treating acute gastroenteritis, rheumatic arthritis, etc. However, there is less research on stone-on-tassel. At present, the research of the stone pine is mainly focused on the research of chemical components, and the active components in the stone pine are mainly alkaloids such as the stone pine alkali, the hydroxy stone pine alkali, nicotine and the like, and flavone and triterpene compounds, and 34 chemical components are identified. Compound lycoclavanin has not been previously reported in pinus plants. The research on the lycopodium clavatum is relatively few, reagents harmful to the environment and the body such as ethyl acetate, petroleum ether and the like are used for separating and purifying chemical components of the lycopodium clavatum, the environment protection and the sustainable research are not facilitated, and the application research on the lycopodium clavatum extract in the field of skin care products is not published at present. Therefore, developing a pinus parviflora extract with simple process, definite active ingredients and clear quality standard is the research focus in the field. Disclosure of Invention Aiming at the defects of the prior art, the invention aims to provide a pinus cassiabarktree extract, a preparation method and application thereof, the preparation method has simple process, the obtained extract has definite effective components, and can be applied in cosmetics to exert antioxidant, antiinflammatory and relieving effects. In order to achieve the aim of the invention, the invention adopts the following technical scheme: In a first aspect, the invention provides a method for preparing a pinus parviflora extract, which is characterized by comprising the following steps: (1) Extracting the lycopodium clavatum powder by alcohol, and concentrating the obtained extracting solution under reduced pressure to obtain a crude extracting solution; (2) Centrifuging the crude extract, collecting a supernatant I, re-dissolving the precipitate, centrifuging, collecting a supernatant II, and combining the supernatant I and the supernatant II to obtain a solution to be purified; (3) And (3) carrying out sectional elution on the solution to be purified by adopting macroporous resin, collecting the eluent of the last section, concentrating and drying to obtain the lycopodium clavatum extract. Preferably, the particle size of the spikenard powder is 70-100 mesh, for example, 70 mesh, 80 mesh, 90 mesh, 100 mesh, etc. Preferably, the pinus radiata is a dried whole plant of pinus radiata of pinus genus of pinaceae family. Preferably, the extracting agent adopted in the extraction is an ethanol water solution, and the mass percentage of ethanol in the ethanol water solution is 60-80%, for example, 65%, 70%, 75%, 80% and the like, and preferably 70%. Preferably, the ratio of the feed liquid in the extraction is 1 (5-10), for example, 1:6, 1:7, 1:8, 1:9, 1:10, and the like, preferably 1:10. Preferably, the extraction is performed independently 1-3 times, for example, 1, 2 or 3 times, preferably 2 times. Preferably, the extraction times are each independently 1-3 hours, for example, 1.5 hours, 2 hours, 2.5 hours, etc. Preferably, the reduced pressure concentration is at a temperature of 45-65 ℃, which may be 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃, 60 ℃, 62 ℃, 64 ℃, etc., for example. Preferably, the mass ratio of the crude extract to the spidroa casweight powder is (0.5-1.5): 1, for example, 0.6:1, 0.8: