CN103030673B - Method for extracting myricetin-3-O-rutinose from taxus mairei leaves - Google Patents
Method for extracting myricetin-3-O-rutinose from taxus mairei leaves Download PDFInfo
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- CN103030673B CN103030673B CN201210588681.9A CN201210588681A CN103030673B CN 103030673 B CN103030673 B CN 103030673B CN 201210588681 A CN201210588681 A CN 201210588681A CN 103030673 B CN103030673 B CN 103030673B
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- Prior art keywords
- rutinose
- extract
- extraction
- ampelopsin
- elutriant
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Saccharide Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting myricetin-3-O-rutinose from taxus mairei leaves. The method comprises the steps of using a supercritical extraction kettle to extract, using methyl alcohol to absorb, using AB-8 resin to conduct chromatography, using 100-mesh polyamide to conduct the chromatography, collecting an eluent at 6-9min, concentrating and drying, and obtaining a white crystallized compound of myricetin-3-O-rutinose. The extracting method is simple and easy to implement, and the purity of myricetin-3-O-rutinose in the extracted white crystallized compound reaches 99.76%.
Description
Technical field
The present invention relates to the extractive technique of plant flavone, be specifically related to a kind of method extracting ampelopsin-3-O-rutinose from leaves of Taxus mairei.
Background technology
Containing efficacy components such as taxol, Japanese yew flavones and yew amyloses in Taxus leaf, Japanese yew flavones contains common parent nucleus C
6-C
3-C
6structure, have regulate cardiovascular system effect, anti-inflammatory and anti-immunization, anti-microbial effect, to the effect of peptide ulceration and antitumor action etc.Grant number is extract and the extracting method that the Chinese invention patent of ZL200910157034.0 discloses a kind of southerm yew blade, and extract major ingredient comprises rutin-3-O-Quercetin, rutin-3-O-kaempferol, rutin-3-O-myricetin, kaempferol-7-O-glucose and glucose-7-O-Quercetin; Extracting method comprises that blade is dried, pulverizes and sieves, immerses alcohol solvent, stirred lower supersound extraction, extracting solution concentrating under reduced pressure goes alcohol, chloroform extraction degreasing, aqueous phase concentrate drying step, the mixture of what the method obtained is various Japanese yew flavones.Ampelopsin molecular formula is C
15h
10o
8, chemical name: 3,5,7-trihydroxy--2-(3,4,5-trihydroxy-phenyl)-4H-1-benzopyran-4-one, has antithrombotic, resists myocardial ischemia, improves microcirculation, hypoglycemic effect of Denging.Rutinose molecular formula is C
12h
22o
10.There is not the report extracting ampelopsin-3-O-rutinose monomer from leaves of Taxus mairei at present.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method extracting ampelopsin-3-O-rutinose from leaves of Taxus mairei, and the method can be extracted and obtain the higher ampelopsin-3-O-rutinose monomer of purity.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of method extracting ampelopsin-3-O-rutinose from leaves of Taxus mairei, and its step is as follows:
1, fresh southerm yew blade is dried 24h at 50 DEG C of temperature, pulverize, crossing No. 8 sieves is powder, loads in supercritical extraction reactor;
2, in supercritical extraction reactor, be 28 DEG C in extraction temperature, CO
2hydrodynamicpressure is 30MPa, under entrainment agent ethanol flow velocity 0.27 ml/min, and extraction 1.5h, extraction is extracted thing;
3, in extract, add methanol absorption is absorption liquid, the addition of described methyl alcohol is add methyl alcohol 1ml in the extract of above-mentioned powder 5g, absorption liquid AB-8 resin chromatography, then be the ethanol elution of 80% by mass percentage concentration, obtain the first elutriant, first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, first concentrated solution, 100 order polyamide chromatography, be the ethanol elution of 60% by mass percentage concentration again, collect the elutriant of 6 ~ 9 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is ampelopsin-3-O-rutinose.
The invention has the advantages that a kind of method extracting ampelopsin-3-O-rutinose from leaves of Taxus mairei, extracted by supercritical extraction reactor, methanol absorption, after AB-8 resin chromatography, then use 100 order polyamide chromatography, collect the elutriant of 6 ~ 9 min, concentrate drying obtains ampelopsin-3-O-rutinose white crystalline compound, this simple and convenient extraction, easy to implement, in the white crystalline compound of extraction, the purity of ampelopsin-3-O-rutinose reaches 99.76%.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment
From leaves of Taxus mairei, extract a method for ampelopsin-3-O-rutinose, first fresh southerm yew blade is dried 24h under 50 DEG C of conditions, pulverize, crossing No. 8 sieves is powder, and weigh 50g, loads in supercritical extraction reactor, be 28 DEG C in extraction temperature in supercritical extraction reactor, CO
2hydrodynamicpressure is 30MPa, under entrainment agent ethanol flow velocity 0.27 ml/min, extraction 1.5h obtains extract, adding 10ml methanol absorption in extract is absorption liquid, absorption liquid AB-8 resin (commercially available) chromatography, AB-8 resin is low-pole, surface-area 480 ~ 520 (m2/g), particle radii 13 ~ 14nm, water content 64%, be the ethanol elution of 80% by mass percentage concentration after chromatography, obtain the first elutriant, first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, first concentrated solution, 100 order polymeric amide (commercially available) chromatographies, be the ethanol elution of 60% by mass percentage concentration, collect the elutriant of 6 ~ 9 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is through analysis of the molecular structure, that hydroxyl on ampelopsin C3 position is combined with rutinose and the disaccharide glycosides formed, belong to ampelopsin-3-O-rutinose in flavonoid compound, adopt high effective liquid chromatography for measuring, in white crystalline compound, ampelopsin-3-O-rutinose purity reaches 99.76%, for the pharmacological research of ampelopsin-3-O-rutinose and application create condition.
Claims (1)
1. from leaves of Taxus mairei, extract a method for ampelopsin-3-O-rutinose, it is characterized in that step is as follows:
1) fresh southerm yew blade is dried 24h at 50 DEG C of temperature, pulverize, crossing No. 8 sieves is powder, loads in supercritical extraction reactor;
2), in supercritical extraction reactor, be 28 DEG C in extraction temperature, CO
2hydrodynamicpressure is 30MPa, under entrainment agent ethanol flow velocity 0.27 ml/min, and extraction 1.5h, extraction is extracted thing;
3) in extract, add methanol absorption is absorption liquid, the addition of described methyl alcohol is add methyl alcohol 1ml in the extract of above-mentioned powder 5g, absorption liquid AB-8 resin chromatography, then be the ethanol elution of 80% by mass percentage concentration, obtain the first elutriant, first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, first concentrated solution, 100 order polyamide chromatography, be the ethanol elution of 60% by mass percentage concentration again, collect the elutriant of 6 ~ 9 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is ampelopsin-3-O-rutinose.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210588681.9A CN103030673B (en) | 2012-12-31 | 2012-12-31 | Method for extracting myricetin-3-O-rutinose from taxus mairei leaves |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210588681.9A CN103030673B (en) | 2012-12-31 | 2012-12-31 | Method for extracting myricetin-3-O-rutinose from taxus mairei leaves |
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| CN103030673A CN103030673A (en) | 2013-04-10 |
| CN103030673B true CN103030673B (en) | 2015-07-22 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001062753A1 (en) * | 2000-02-25 | 2001-08-30 | Hanwha Chemical Corporation | Method and apparatus for preparing taxol using supercritical fluid from source materials |
| CN101716197A (en) * | 2009-12-30 | 2010-06-02 | 宁波泰康红豆杉生物工程有限公司 | Extractive of Taxus chinensis var.mairei leaves and preparation method |
-
2012
- 2012-12-31 CN CN201210588681.9A patent/CN103030673B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001062753A1 (en) * | 2000-02-25 | 2001-08-30 | Hanwha Chemical Corporation | Method and apparatus for preparing taxol using supercritical fluid from source materials |
| CN101716197A (en) * | 2009-12-30 | 2010-06-02 | 宁波泰康红豆杉生物工程有限公司 | Extractive of Taxus chinensis var.mairei leaves and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| Flavonoids from the Genus Taxus;Miroslawa Krauze-Baranowska;《Z. Naturforsch.》;20041231;第59c卷;43-47 * |
| 王亚飞,等.红豆杉属植物资源的研究现状与开发利用对策.《林业科学》.2012,第48卷(第5期),116-125. * |
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