CN103044378A - Method for extracting ginkgetin from leaves of taxus mairei - Google Patents
Method for extracting ginkgetin from leaves of taxus mairei Download PDFInfo
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- CN103044378A CN103044378A CN2012105885534A CN201210588553A CN103044378A CN 103044378 A CN103044378 A CN 103044378A CN 2012105885534 A CN2012105885534 A CN 2012105885534A CN 201210588553 A CN201210588553 A CN 201210588553A CN 103044378 A CN103044378 A CN 103044378A
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- Prior art keywords
- ginkgetin
- leaves
- elutriant
- methyl alcohol
- white crystalline
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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
Abstract
The invention discloses a method for extracting ginkgetin from leaves of taxus mairei. The method is characterized in that leaves of taxus mairei are extracted through a supercritical extraction kettle, methyl alcohol is added for absorption, AB-8 resin is adopted for chromatography, then 100-mesh polyamide is adopted for chromatography, eluant is collected for 15 to 17 min and is concentrated and dried to obtain ginkgetin white crystalline compounds. The extraction method is simple and convenient, is easy to implement, and the purity of the ginkgetin in the extracted white crystalline compounds is 99.52%.
Description
Technical field
The present invention relates to the extractive technique of plant flavone, be specifically related to a kind of method of from leaves of Taxus mairei, extracting Ginkgetin.
Background technology
Contain the efficacy components such as taxol, Japanese yew flavones and yew amylose in the Taxus leaf, the 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 the 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 oven dry, crushing screening, immersion alcohol solvent, the lower supersound extraction of stirring, extracting solution concentrating under reduced pressure go alcohol, chloroform extraction degreasing, water concentrate drying step, and what the method obtained is the mixture of various Japanese yew flavones.Ginkgetin has another name called ginkegetin or ginkgetin, is yellow crystal, 347～349 ℃ of fusing points (decomposition).The report that extracts the Ginkgetin monomer from leaves of Taxus mairei is not arranged at present.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of extracting Ginkgetin from leaves of Taxus mairei, and the method can obtain the higher Ginkgetin monomer of purity.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of method of from leaves of Taxus mairei, extracting Ginkgetin, and its step is as follows:
1, fresh southerm yew blade is dried 24h under 50 ℃ of temperature, pulverize, cross No. 8 sieves and be powder, in the supercritical extraction reactor of packing into;
2, in the supercritical extraction reactor, be 36 ℃ in extraction temperature, CO
2Hydrodynamicpressure is 30MPa, under entrainment agent ethanol flow velocity 0.32 ml/min, extracts 2 h, and extraction is extracted thing;
3, in extract, add methyl alcohol and be absorbed as absorption liquid, the addition of described methyl alcohol is to add methyl alcohol 1ml in the extract of above-mentioned powder 5g, absorption liquid AB-8 resin chromatography, then be 80% ethanol elution with mass percentage concentration, obtain the first elutriant, the first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, the first concentrated solution is with 100 order polymeric amide chromatographies, be the ethanol elution of 60 % again with mass percentage concentration, collect the elutriant of 15～17 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is Ginkgetin.
The invention has the advantages that a kind of method of from leaves of Taxus mairei, extracting Ginkgetin, extract by supercritical extraction reactor, methyl alcohol absorbs, behind the AB-8 resin chromatography, use again 100 order polymeric amide chromatographies, collect the elutriant of 15～17 min, concentrate drying obtains the Ginkgetin white crystalline compound, this simple and convenient extraction, easy to implement, the purity of Ginkgetin reaches 99.52% in the white crystalline compound of extraction.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment
A kind of method for preparing type separation Ginkgetin from leaves of Taxus mairei is dried 24h with fresh southerm yew blade first under 50 ℃ of conditions, pulverize, and crosses No. 8 sieves and is powder, and the 50g that weighs is in the supercritical extraction reactor of packing into; Be 36 ℃ in extraction temperature in the supercritical extraction reactor, CO
2Hydrodynamicpressure is 30MPa, under entrainment agent ethanol flow velocity 0.32 ml/min, extract 2 h, add 10ml methyl alcohol in the extract and be absorbed as absorption liquid, absorption liquid AB-8 resin (commercially available) chromatography, the AB-8 resin is low-pole, surface-area 480～520 (m2/g), particle radii 13～14nm, water content 64%; It behind the chromatography is 80% ethanol elution with mass percentage concentration, obtain the first elutriant, the first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, the first concentrated solution is with 100 order polymeric amide (commercially available) chromatographies, be the ethanol elution of 60 % again with mass percentage concentration, collect the elutriant of 15～17 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is Ginkgetin, adopts high effective liquid chromatography for measuring, and Ginkgetin purity reaches 99.52% in the white crystalline compound.
Claims (1)
1. method of extracting Ginkgetin from leaves of Taxus mairei is characterized in that step is as follows:
1) fresh southerm yew blade is dried 24h under 50 ℃ of temperature, pulverize, cross No. 8 sieves and be powder, in the supercritical extraction reactor of packing into;
2) in the supercritical extraction reactor, be 36 ℃ in extraction temperature, CO
2Hydrodynamicpressure is 30MPa, under entrainment agent ethanol flow velocity 0.32 ml/min, extracts 2 h, and extraction is extracted thing;
3) in extract, add methyl alcohol and be absorbed as absorption liquid, the addition of described methyl alcohol is to add methyl alcohol 1ml in the extract of above-mentioned powder 5g, absorption liquid AB-8 resin chromatography, then be 80% ethanol elution with mass percentage concentration, obtain the first elutriant, the first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, the first concentrated solution is with 100 order polymeric amide chromatographies, be the ethanol elution of 60 % again with mass percentage concentration, collect the elutriant of 15～17 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is Ginkgetin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210588553.4A CN103044378B (en) | 2012-12-31 | 2012-12-31 | Method for extracting ginkgetin from leaves of taxus mairei |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210588553.4A CN103044378B (en) | 2012-12-31 | 2012-12-31 | Method for extracting ginkgetin from leaves of taxus mairei |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103044378A true CN103044378A (en) | 2013-04-17 |
| CN103044378B CN103044378B (en) | 2015-04-22 |
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| CN201210588553.4A Active CN103044378B (en) | 2012-12-31 | 2012-12-31 | Method for extracting ginkgetin from leaves of taxus mairei |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003037096A1 (en) * | 2001-10-31 | 2003-05-08 | Brightwater Horticulture Limited | Improved botanical extractions process |
| CN1994507A (en) * | 2006-12-05 | 2007-07-11 | 中国海洋大学 | A low-pressure supercritical extraction process and apparatus thereof |
| CN102603482A (en) * | 2012-02-20 | 2012-07-25 | 福建华尔康生物科技有限公司 | Separation technology for multiple components in ginkgo leaf |
| CN102631379A (en) * | 2012-04-25 | 2012-08-15 | 江苏红豆杉保健品有限公司 | Preparation method of taxus chinensis active extract and application thereof in fungus resistance |
-
2012
- 2012-12-31 CN CN201210588553.4A patent/CN103044378B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003037096A1 (en) * | 2001-10-31 | 2003-05-08 | Brightwater Horticulture Limited | Improved botanical extractions process |
| CN1994507A (en) * | 2006-12-05 | 2007-07-11 | 中国海洋大学 | A low-pressure supercritical extraction process and apparatus thereof |
| CN102603482A (en) * | 2012-02-20 | 2012-07-25 | 福建华尔康生物科技有限公司 | Separation technology for multiple components in ginkgo leaf |
| CN102631379A (en) * | 2012-04-25 | 2012-08-15 | 江苏红豆杉保健品有限公司 | Preparation method of taxus chinensis active extract and application thereof in fungus resistance |
Non-Patent Citations (2)
| Title |
|---|
| 窦圣姗: "东北红豆杉枝叶抗肿瘤有效部位群及其化学研究", 《黑龙江中医药大学硕士学位论文》 * |
| 金槐: "超临界萃取银杏黄酮", 《农牧产品开发》 * |
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| CN103044378B (en) | 2015-04-22 |
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