CN101134758B - Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf - Google Patents
Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf Download PDFInfo
- Publication number
- CN101134758B CN101134758B CN2007100502421A CN200710050242A CN101134758B CN 101134758 B CN101134758 B CN 101134758B CN 2007100502421 A CN2007100502421 A CN 2007100502421A CN 200710050242 A CN200710050242 A CN 200710050242A CN 101134758 B CN101134758 B CN 101134758B
- Authority
- CN
- China
- Prior art keywords
- bilobalide
- ginkgo leaf
- ginkgolide
- monomer
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The process of extracting and separating bilobalide A, bilobalide B, bilobalide C, bilobalide J and bilobalide monomer from ginkgo leaf includes the following steps: 1. extracting ginkgo leaf with alcohol solutions of different concentrations, merging extracted solution and concentrating; 2. extracting the concentrate with ethyl acetate, recovering organic phase and concentrating to form extractum; 3. diluting the extractum, eluting in selective polar adsorption resin column with alcohol, recovering alcohol from the eluted solution and crystallizing in alcohol to obtain bilobalides; 4. eluting bilobalides crystal in silica gel column with mixed solution of n-hexane and ethyl acetate, and collecting eluted solution sectionally to obtain bilobalide monomer, bilobalide A, bilobalide B, bilobalide C and bilobalide J successively; and 5. concentrating and re-crystallizing separately to obtain bilobalide monomer, bilobalide A, bilobalide B, bilobalide C and bilobalide J.
Description
(1) technical field:
The present invention relates to from plant, extract the method for effective ingredient, be specifically related to the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer from Ginkgo Leaf.
(2) background technology:
Ginkgo claims maidenhair tree again, belongs to gymnosperm, is one of the veteran kind of unique existence of Ginkgoaceae Ginkgo, and its leaf and fruit have important pharmaceutical use.What research was maximum at present is Folium Ginkgo extract, and it comprises flavonoid compound and ginkgolide compound.Flavonoid compound has 38 kinds approximately, and total content is 22-27%; Ginkgolide compound comprises bilobalide and bilobalide, and total content is 5.4-6.6%.Bilobalide mainly comprises Ginkgolide A, B, C, J and M monomer; According to the literature, each monomeric pharmic function has certain difference in the bilobalide, and wherein, Ginkgolide A, B have significant curative effect to the treatment cardiovascular and cerebrovascular diseases; Bilobalide is to treatment nervous system disorders drug effect uniqueness then, in order to improve its medicinal result of treatment, and sometimes must be with each monomer separation purifying; Because bilobalide is the sesquiterpene material, and Ginkgolide A, B, C, J, M are the diterpenes materials, their molecular structure is comparatively similar, polarity difference is also very little, cause in the ginkgolide compound each monomeric extraction with separate the comparison difficulty, have only a little enterprise that they are separated separately, as application number is 200410065104.7, name is called the Chinese invention patent of " a kind of separation purification method of ginkgolide monomer ", disclose a kind of separation purification method of ginkgolide monomer, it is to adopt column chromatography-recrystallization-supercritical CO
2Refining purifying combination process is produced highly purified Ginkgolide A, Ginkgolide B, ginkalide C, bilobalide J, bilobalide M and bilobalide; Wherein column chromatography adopts positive or anti-phase fixedly filler, makes water, ethyl acetate, ethanol, methyl alcohol, chloroform, sherwood oil equal solvent gradient elution, supercritical CO
2Refining purifying and crystal formation finishing technique condition are: pressure≤100MPa, and temperature≤150 ℃, entrainment agent is ethyl acetate, ethanol etc.; The monomer content separating obtained by this method reaches as high as 99.8%, total recovery 〉=90%, but this method has adopted supercritical CO
2Refining purifying combination process, working condition is had relatively high expectations, and corresponding cost is also higher.
(3) summary of the invention:
The present invention will disclose a kind of high method of extraction separation Ginkgolide A, B, C, J and bilobalide monomer from Ginkgo Leaf of income rate height, each monomer purity of gained of extracting.
The method of the present invention extraction separation Ginkgolide A, B, C, J and bilobalide monomer from Ginkgo Leaf, its step is as follows:
1) get Ginkgo Leaf, extract with Different concentrations of alcohol from high to low, united extraction liquid reclaims ethanol, the extracting solution after obtaining concentrating;
Take by weighing a certain amount of Ginkgo Leaf, can be earlier be that the ethanol of 60-80% extracted 1-3 hour Ginkgo Leaf 50-70 ℃ the time with volumetric concentration, wherein, the weight that Ginkgo Leaf and alcoholic acid proportioning are pressed Ginkgo Leaf: alcoholic acid volume=1: 8-10; Ginkgo Leaf is separated, and is that the ethanol of 30-55% extracted 1-3 hour Ginkgo Leaf 50-70 ℃ the time with volumetric concentration again, wherein, and the weight that Ginkgo Leaf and alcoholic acid proportioning are pressed Ginkgo Leaf: alcoholic acid volume=1: 6-8; Ginkgo Leaf being separated, is that the ethanol of 10-25% extracted 1-3 hour Ginkgo Leaf in the time of 50-70 ℃ with volumetric concentration again, wherein, and the weight that Ginkgo Leaf and alcoholic acid proportioning are pressed Ginkgo Leaf: alcoholic acid volume=1: 5-7; United extraction liquid reclaims ethanol, extracting solution is concentrated into 8-10 times of volume of Ginkgo Leaf weight;
2) add ethyl acetate extraction in the extracting solution after concentrating, be concentrated into medicinal extract after the recovery organic phase;
Can add equal volume of ethyl acetate in concentrated solution, in general, it is better to extract the effect that is reached for 3 times;
3) with step 2) the back selective polarity atresia adsorption resin column of going up of gained medicinal extract dilution, use ethanol elution, the gained elutriant obtains ginkgolide compound with alcohol crystal after reclaiming ethanol again;
The model of described selective polarity atresia adsorption resin column can be ADS-15, or ADS-17, or ADS-F8; With step 2) gained medicinal extract, can wash with water earlier doubly to the water dilution back of its weight upper prop with 50-200, and is colourless until effluent liquid; And then be the ethanol elution of 50-70% with volumetric concentration, the 30-60 that the volumetric usage of described eluent can be above-mentioned medicinal extract weight is doubly; The elutriant that collection is obtained reclaims ethanol, is concentrated into medicinal extract, is that the ethanol of 50-80% is solvent crystallization with volumetric concentration again, and the gained crystallization is ginkgolide compound;
4) with silicagel column in the ginkgolide compound crystallization, with the mixed solution wash-out of normal hexane and ethyl acetate, the Fractional Collections elutriant obtains bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J successively respectively;
The volume ratio of normal hexane and ethyl acetate is preferably 9 in the mixed solution of described normal hexane and ethyl acetate: 1-2: 8; In the process of wash-out, with the online detection and location of light scattering detector, the Fractional Collections elutriant obtains containing the elutriant of bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J successively;
5) recycling step 4) in solvent in each elutriant of collecting, obtain bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J monomer respectively with alcohol crystal again.
Recycling step 4) solvent in the elutriant of collecting in is that the ethanol of 20-40% carries out crystallization to the bilobalide elutriant with volumetric concentration, obtains bilobalide monomer; The ethanol that with volumetric concentration is 60-80% carries out crystallization to the Ginkgolide A elutriant, obtains the Ginkgolide A monomer; The ethanol that with volumetric concentration is 30-70% carries out crystallization to the Ginkgolide B elutriant, obtains the Ginkgolide B monomer; The ethanol that with volumetric concentration is 20-40% carries out crystallization to the ginkalide C elutriant, obtains the ginkalide C monomer; The ethanol that with volumetric concentration is 20-40% carries out crystallization to the bilobalide J elutriant, obtains the bilobalide J monomer.
Advantage of the present invention:
The present invention adopts from high to low Different concentrations of alcohol that Ginkgo Leaf is extracted, and the extraction yield of ginkgolide compound has been improved more than 10%, and particularly the extraction yield of bilobalide and bilobalide J has improved 15% than prior art; Also adopt special selective polarity not have macroporous adsorbent resin among the present invention and carried out removal of impurities, can remove most of isolating impurity of silicagel column that influences, realized that a upper prop is separable Ginkgolide A, B, C, J and the bilobalide monomer of obtaining, and each monomeric purity reaches more than 99%; Compared with prior art, method technology provided by the invention is simple, production cost is low, and gained monomer purity height is easier to the production of industrialization.
(4) embodiment:
Embodiment 1
1) getting 10 kilograms of Ginkgo Leaves, is that 80% ethanol extracted 1 hour Ginkgo Leaf in the time of 50 ℃ with 100 liters of volumetric concentrations, with 200 purpose filter clothes Ginkgo Leaf is separated; Being 55% ethanol with 60 liters of volumetric concentrations again extracted 1 hour Ginkgo Leaf 70 ℃ the time, with 200 purpose filter clothes Ginkgo Leaf was separated; Being 25% ethanol with 50 liters of volumetric concentrations again extracted 1 hour Ginkgo Leaf 50 ℃ the time, with 200 purpose filter clothes Ginkgo Leaf was separated; Merge the extracting solution of three extraction gained, reclaim ethanol, extracting solution is concentrated into 100 liters of concentrated solutions;
2) in concentrated solution, add 100 liters of ethyl acetate extractions 3 times, merge the organic phase that extracting and separating goes out, concentrate after the recovery organic phase and obtain 500 gram medicinal extract;
3) with step 2) in gained medicinal extract add 50 times of volume water dilution back and go up the ADS-15 posts, wash with water earlier, colourless until effluent liquid, be 50% ethanol elution again with 15 liters of volumetric concentrations, collect elutriant, reclaim ethanol, be concentrated into medicinal extract, be 50% alcohol crystal again with volumetric concentration, obtain 70 gram ginkgolide compound crystal;
4) with silicagel column in the ginkgolide compound crystallization, carry out gradient elution with the mixed solution of normal hexane and ethyl acetate, wherein, the volume ratio of normal hexane and ethyl acetate is 9: 1-2: 8; In elution process, with the online detection and location of light scattering detector, the Fractional Collections elutriant obtains containing the elutriant of bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J successively;
5) recycling step 4) in solvent in each elutriant of collecting, be that 20% ethanol carries out crystallization to the bilobalide elutriant with volumetric concentration then, obtain 12.01 bilobalide monomers that restrain; Be that 60% ethanol carries out crystallization to the Ginkgolide A elutriant with volumetric concentration, obtain the Ginkgolide A monomers of 3.12 grams; Be that 40% ethanol carries out crystallization to the Ginkgolide B elutriant with volumetric concentration, obtain the Ginkgolide B monomers of 4.55 grams; Be that 30% ethanol carries out crystallization to the ginkalide C elutriant with volumetric concentration, obtain the ginkalide C monomers of 4.72 grams; Be that 30% ethanol carries out crystallization to the bilobalide J elutriant with volumetric concentration, obtain the bilobalide J monomers of 1.30 grams.
Embodiment 2
1) getting 50 kilograms of Ginkgo Leaves, is that 60% ethanol extracted 3 hours Ginkgo Leaf in the time of 70 ℃ with 400 liters of volumetric concentrations, with 200 purpose filter clothes Ginkgo Leaf is separated; Being 30% ethanol with 400 liters of volumetric concentrations again extracted 3 hours Ginkgo Leaf 70 ℃ the time, with 200 purpose filter clothes Ginkgo Leaf was separated; Being 10% ethanol with 300 liters of volumetric concentrations again extracted 3 hours Ginkgo Leaf 70 ℃ the time, with 200 purpose filter clothes Ginkgo Leaf was separated; Merge the extracting solution of three extraction gained, reclaim ethanol, extracting solution is concentrated into 500 liters of concentrated solutions;
2) in concentrated solution, add 500 liters of ethyl acetate extractions 3 times, merge the organic phase that extracting and separating goes out, concentrate after the recovery organic phase and obtain 1.5 kilograms of medicinal extract;
3) with step 2) in gained medicinal extract add 200 times of volume water dilution back and go up the ADS-17 posts, wash with water earlier, colourless until effluent liquid, be 70% ethanol elution again with 60 liters of volumetric concentrations, collect elutriant, reclaim ethanol, be concentrated into medicinal extract, be 70% alcohol crystal again with volumetric concentration, obtain 233 gram ginkgolide compound crystal;
4) with silicagel column in the ginkgolide compound crystallization, carry out gradient elution with the mixed solution of normal hexane and ethyl acetate, wherein, the volume ratio of normal hexane and ethyl acetate is 9: 1-2: 8; In elution process, with the online detection and location of light scattering detector, the Fractional Collections elutriant obtains containing the elutriant of bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J successively;
5) recycling step 4) in solvent in each elutriant of collecting, be that 30% ethanol carries out crystallization to the bilobalide elutriant with volumetric concentration then, obtain 5.17 bilobalide monomers that restrain; Be that 75% ethanol carries out crystallization to the Ginkgolide A elutriant with volumetric concentration, obtain the Ginkgolide A monomers of 28.71 grams; Be that 30% ethanol carries out crystallization to the Ginkgolide B elutriant with volumetric concentration, obtain the Ginkgolide B monomers of 81.90 grams; Be that 25% ethanol carries out crystallization to the ginkalide C elutriant with volumetric concentration, obtain the ginkalide C monomers of 3.47 grams; Be that 40% ethanol carries out crystallization to the bilobalide J elutriant with volumetric concentration, obtain the bilobalide J monomers of 4.01 grams.
Embodiment 3
1) getting 40 kilograms of Ginkgo Leaves, is that 70% ethanol extracted 1 hour Ginkgo Leaf in the time of 70 ℃ with 280 liters of volumetric concentrations, with 200 purpose filter clothes Ginkgo Leaf is separated; Being 50% ethanol with 280 liters of volumetric concentrations again extracted 2 hours Ginkgo Leaf 60 ℃ the time, with 200 purpose filter clothes Ginkgo Leaf was separated; Being 20% ethanol with 280 liters of volumetric concentrations again extracted 2 hours Ginkgo Leaf 70 ℃ the time, with 200 purpose filter clothes Ginkgo Leaf was separated; Merge the extracting solution of three extraction gained, reclaim ethanol, extracting solution is concentrated into 400 liters of concentrated solutions;
2) in concentrated solution, add 400 liters of ethyl acetate extractions 3 times, merge the organic phase that extracting and separating goes out, concentrate after the recovery organic phase and obtain 1.2 kilograms of medicinal extract;
3) with step 2) in gained medicinal extract add 100 times of volume water dilution back and go up the ADS-F8 posts, wash with water earlier, colourless until effluent liquid, be 60% ethanol elution again with 70 liters of volumetric concentrations, collect elutriant, reclaim ethanol, be concentrated into medicinal extract, be 80% alcohol crystal again with volumetric concentration, obtain 225 gram ginkgolide compound crystal;
4) with silicagel column in the ginkgolide compound crystallization, carry out gradient elution with the mixed solution of normal hexane and ethyl acetate, wherein, the volume ratio of normal hexane and ethyl acetate is 9: 1-2: 8; In elution process, with the online detection and location of light scattering detector, the Fractional Collections elutriant obtains containing the elutriant of bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J successively;
5) recycling step 4) in solvent in each elutriant of collecting, be that 25% ethanol carries out crystallization to the bilobalide elutriant with volumetric concentration then, obtain 44.51 bilobalide monomers that restrain; Be that 70% ethanol carries out crystallization to the Ginkgolide A elutriant with volumetric concentration, obtain the Ginkgolide A monomers of 31.76 grams; Be that 50% ethanol carries out crystallization to the Ginkgolide B elutriant with volumetric concentration, obtain the Ginkgolide B monomers of 16.72 grams; Be that 40% ethanol carries out crystallization to the ginkalide C elutriant with volumetric concentration, obtain the ginkalide C monomers of 17.68 grams; Be that 20% ethanol carries out crystallization to the bilobalide J elutriant with volumetric concentration, obtain the bilobalide J monomers of 4.01 grams.
Claims (9)
1. the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer from Ginkgo Leaf, its step is as follows:
1) get Ginkgo Leaf, extract with Different concentrations of alcohol from high to low, united extraction liquid reclaims ethanol, the extracting solution after obtaining concentrating; Wherein, described usefulness from high to low Different concentrations of alcohol extract and be meant: be that the ethanol of 60-80% extracts Ginkgo Leaf with volumetric concentration earlier; Be that the ethanol of 30-55% extracts Ginkgo Leaf with volumetric concentration then; Be that the ethanol of 10-25% extracts Ginkgo Leaf with volumetric concentration again;
2) add ethyl acetate extraction in the extracting solution after concentrating, be concentrated into medicinal extract after the recovery organic phase;
3) with step 2) the back selective polarity atresia adsorption resin column of going up of gained medicinal extract dilution, use ethanol elution, the gained elutriant obtains ginkgolide compound with alcohol crystal after reclaiming ethanol again;
4) with silicagel column in the ginkgolide compound crystallization, with the mixed solution wash-out of normal hexane and ethyl acetate, the Fractional Collections elutriant obtains bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J successively respectively;
5) recycling step 4) in solvent in the elutriant collected, obtain bilobalide, Ginkgolide A, Ginkgolide B, ginkalide C and bilobalide J monomer respectively with alcohol crystal again.
2. according to claim 1 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 1), the temperature of described extraction is 50-70 ℃.
3. according to claim 1 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 1), the weight that Ginkgo Leaf and alcoholic acid proportioning are pressed Ginkgo Leaf when extracting for the first time: alcoholic acid volume=1: 8-10; The weight that Ginkgo Leaf and alcoholic acid proportioning are pressed Ginkgo Leaf when extracting for the second time: alcoholic acid volume=1: 6-8; The weight that Ginkgo Leaf and alcoholic acid proportioning are pressed Ginkgo Leaf when extracting for the third time: alcoholic acid volume=1: 5-7.
4. according to claim 1 and 2 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: step 2) in, the volume of the ethyl acetate of described adding with concentrate after the volume ratio of extracting solution be 1: 1, the number of times of extraction is 3 times.
5. according to claim 1 and 2 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 3), it is ADS-15 that described selective polarity does not have the macroporous adsorbent resin model, or ADS-17, or ADS-F8.
6. according to claim 1 and 2 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 3), described wash-out is 50-70% with the alcoholic acid volumetric concentration.
7. according to claim 1 and 2 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 3), described crystallization is 50-80% with the alcoholic acid volumetric concentration.
8. according to claim 1 and 2 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 4), in described normal hexane and the ethyl acetate mixed solution, the volume ratio of normal hexane and ethyl acetate is 9: 1-2: 8.
9. according to claim 1 and 2 from Ginkgo Leaf the method for extraction separation Ginkgolide A, B, C, J and bilobalide monomer, it is characterized in that: in the step 4), with the online detection and location of light scattering detector, Fractional Collections elutriant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100502421A CN101134758B (en) | 2007-10-15 | 2007-10-15 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100502421A CN101134758B (en) | 2007-10-15 | 2007-10-15 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101134758A CN101134758A (en) | 2008-03-05 |
| CN101134758B true CN101134758B (en) | 2010-04-14 |
Family
ID=39159106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007100502421A Expired - Fee Related CN101134758B (en) | 2007-10-15 | 2007-10-15 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101134758B (en) |
Families Citing this family (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559085B (en) * | 2008-04-16 | 2011-09-07 | 上海信谊百路达药业有限公司 | Extracting method for improving content of bilobalide in folium ginkgo extract |
| CN101392000B (en) * | 2008-09-25 | 2010-12-22 | 成都普思生物科技有限公司 | High efficiency separation purification method of ginkgolide A, B, C, J and bilobalide monomer |
| CN101974014B (en) * | 2010-09-27 | 2012-08-22 | 徐州技源天然保健品有限公司 | Manufacturing technology for extracting ginkalide A and C from root and bark of maidenhair tree |
| CN102464666B (en) * | 2010-11-09 | 2015-04-08 | 上海医药工业研究院 | Preparation method for ginkgolide C |
| CN102464665B (en) * | 2010-11-09 | 2015-04-08 | 上海医药工业研究院 | Method for preparing ginkgolide A |
| CN102552340A (en) * | 2010-12-15 | 2012-07-11 | 中国医药集团总公司四川抗菌素工业研究所 | Preparation method of ginkgolide monomer and total ginkgo flavone-glycoide |
| CN102070647B (en) * | 2010-12-28 | 2012-11-07 | 浙江大学 | Method for separating ginkgolide B from ginkgolide mixture |
| CN103159779A (en) * | 2011-12-15 | 2013-06-19 | 张加明 | Industrialization production technology for extracting bilobalide from Ginkgo testa |
| CN102659808B (en) | 2012-04-23 | 2014-10-29 | 成都百裕科技制药有限公司 | Extraction separation method of ginkgolides |
| CN102887909B (en) * | 2012-11-07 | 2014-12-03 | 黑龙江天宏药业股份有限公司 | Method for extracting and separating ginkgolide B from ginkgo leaves |
| CN102911184B (en) * | 2012-11-14 | 2015-03-18 | 成都百裕科技制药有限公司 | Separation and purification preparation method for bilobalide |
| CN103044442B (en) * | 2013-01-03 | 2015-08-19 | 苏州泽达兴邦医药科技有限公司 | A kind of method of separation and purification GA, GB and bilobalide from Folium Ginkgo extract |
| CN103525632B (en) * | 2013-09-17 | 2015-06-03 | 李前进 | Health-care wine and preparation method |
| CN103524526B (en) * | 2013-10-15 | 2016-05-25 | 上海信谊百路达药业有限公司 | A kind of isolation and purification method of Bilobalide |
| CN104784168B (en) * | 2014-01-20 | 2017-11-17 | 成都百裕制药股份有限公司 | Ginkgolides prepares the purposes in contraceptive |
| CN104435017A (en) * | 2014-11-11 | 2015-03-25 | 常州大学 | Extraction method of flavonol in ginkgo leaves |
| CN105801600B (en) * | 2016-04-14 | 2018-03-23 | 江苏康缘药业股份有限公司 | A kind of Bilobalide, ginkalide A, the preparation method of ginkolide B and ginkalide C |
| CN107129505B (en) * | 2017-06-01 | 2019-03-29 | 陕西理工大学 | The industrial production process of lactone element monomers in a kind of ginkgo leaf purification |
| CN108329328B (en) * | 2018-05-09 | 2020-09-11 | 桂林医学院 | Method for extracting bilobalide |
| CN113801133B (en) * | 2021-10-28 | 2022-08-19 | 江苏得乐康生物科技有限公司 | Preparation method of ginkgolide and monomer contained in ginkgolide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1379029A (en) * | 2002-04-27 | 2002-11-13 | 贵州省生化工程中心 | Process for extracting ginkgolectone AB |
| CN1651436A (en) * | 2004-12-07 | 2005-08-10 | 王敬勉 | Extraction method of ginkgolactone B and ginkgo lactone in ginkgo leaf |
| CN1680392A (en) * | 2005-01-07 | 2005-10-12 | 上海同田生化技术有限公司 | Preparation of high-purity ginkgolide |
| CN1977868A (en) * | 2005-12-05 | 2007-06-13 | 浙江海正药业股份有限公司 | Ginkgo biloba leaf total terpene lactone extract, and its preparing method, medicinal composition and use |
-
2007
- 2007-10-15 CN CN2007100502421A patent/CN101134758B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1379029A (en) * | 2002-04-27 | 2002-11-13 | 贵州省生化工程中心 | Process for extracting ginkgolectone AB |
| CN1651436A (en) * | 2004-12-07 | 2005-08-10 | 王敬勉 | Extraction method of ginkgolactone B and ginkgo lactone in ginkgo leaf |
| CN1680392A (en) * | 2005-01-07 | 2005-10-12 | 上海同田生化技术有限公司 | Preparation of high-purity ginkgolide |
| CN1977868A (en) * | 2005-12-05 | 2007-06-13 | 浙江海正药业股份有限公司 | Ginkgo biloba leaf total terpene lactone extract, and its preparing method, medicinal composition and use |
Non-Patent Citations (2)
| Title |
|---|
| 杜安全 等.银杏叶提取物中银杏内酯A、B、C和白果内酯的提取、分离和结构鉴定.江苏药学与临床研究9 3.2001,9(3),1-3. * |
| 杜安全，等.银杏叶提取物中银杏内酯A、B、C和白果内酯的提取、分离和结构鉴定.江苏药学与临床研究9 3.2001,9(3),1-3. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101134758A (en) | 2008-03-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101134758B (en) | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf | |
| US11267775B2 (en) | Method for preparing cannabidiol by separation and purification using high-speed countercurrent chromatography | |
| CN101597296B (en) | Novel method for efficiently extracting and producing artemisinin by ionic liquid | |
| CN106543248B (en) | The method that high speed adverse current chromatogram isolates and purifies flavonoid glycoside compound in lotus nut | |
| CN106967137B (en) | Method for separating high-purity oleuropein by liquid chromatography through macroporous resin combined preparation | |
| CN101412725B (en) | Method for extracting and separating bilobalide B from ginkgo leaf | |
| CN111960930A (en) | Method for separating and purifying cannabidiol from industrial cannabis sativa leaves | |
| CN101781351B (en) | Method for extracting ginsenoside Rb1 from American ginseng and powder-injection thereof | |
| CN101747338A (en) | Method for preparing ginkgolide compound | |
| CN101982471B (en) | Technological process for extracting aucubin from fruits of eucommia ulmoides oliver | |
| CN105294628A (en) | Method for preparing flavonoid component by separating wild chrysanthemum flower | |
| CN102423329A (en) | Decolorization method of panax notoginsenoside extract | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN101468997B (en) | Method for extracting and separating bilobalide from ginkgo leaf | |
| CN101693689A (en) | New method for extracting and separating high-purity huperzine A from thousand-layer column | |
| CN102115467A (en) | Method for preparing catechin monomers | |
| CN101643484B (en) | High-purity syringin, preparation method and application | |
| CN102875619A (en) | Method for extracting kaempferitrin from prunus cerasifera leaves | |
| CN101412724B (en) | Method for extracting bilobalide compound from ginkgo leaf | |
| CN101468998B (en) | Method for extracting and separating bilobalide A from ginkgo leaf | |
| CN101412722B (en) | Method for extracting and separating bilobalide C from ginkgo leaf | |
| CN101153048A (en) | Tea polyphenol monomer and separation process thereof | |
| CN103610708A (en) | Preparation technology of low-acidity and high-purity terpene lactone extract in gingko root and bark | |
| CN103739648A (en) | Preparation method for mussaendoside U | |
| CN102190665B (en) | Method for separating and purifying artemisinin by activated charcoal column chromatography employing nonaqueous system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100414 Termination date: 20161015 |