CN101412724B - Method for extracting bilobalide compound from ginkgo leaf - Google Patents

Method for extracting bilobalide compound from ginkgo leaf Download PDF

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Publication number
CN101412724B
CN101412724B CN2007100502417A CN200710050241A CN101412724B CN 101412724 B CN101412724 B CN 101412724B CN 2007100502417 A CN2007100502417 A CN 2007100502417A CN 200710050241 A CN200710050241 A CN 200710050241A CN 101412724 B CN101412724 B CN 101412724B
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ginkgo leaf
extracting
ethanol
alcoholic acid
extract
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CN101412724A (en
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孙莉莉
罗增桂
唐江明
李振志
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GUILIN ZHENDA BIOLOGY SCIENCE TECHNOLOGY Co Ltd
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GUILIN ZHENDA BIOLOGY SCIENCE TECHNOLOGY Co Ltd
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Abstract

The invention discloses a method for extracting and separating ginkgolides compounds from folium ginkgo, which comprises the following steps: 1) taking the folium ginkgo, carrying out extraction by ethanol with different concentrations from high to low, combining extracting solutions, and reclaiming the ethanol to obtain concentrated extracting solution; 2) adding ethyl acetate into the concentrated extracting solution for extraction, reclaiming organic phase and concentrating the extracting solution into extract; and 3) diluting the extract, putting the extract to preferential polar imperforate adsorption resin, washing the preferential polar imperforate adsorption resin by ethanol, reclaiming the ethanol in eluate, and crystallizing by the ethanol to obtain the ginkgolides compounds. The ginkgolides compounds comprise ginkgolides A, B, C, J and ginkgolide. The method adopts the ethanol with different concentrations from high to low to extract the folium ginkgo, improves the extraction yield for the ginkgolides compounds by more than 10 percent, and has the advantages of simple preparation process, low cost and easy industrial production; and the purity of the ginkgolides compound product reaches more than 60 percent.

Description

From Ginkgo Leaf, extract the method for ginkgolide compound
The present invention relates to from plant, extract the method for effective ingredient, be specifically related to from Ginkgo Leaf, extract the method for ginkgolide compound.
(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%.Ginkgolide compound is the consistent strong active platelet factor antagonist of generally acknowledging of domestic and foreign literature, has obtained the support approval of document and lot of experiments in the clinical treatment that can be used for ishemic stroke and cerebral infarction.Based on this, research, the development and application of ginkgolide compound in the Ginkgo Leaf become the new point of current new drug development.The production technology of present domestic ginkgolide compound mainly adopts the technology of macroporous resin, as application number is 20051004266.1, name is called the Chinese invention patent of " bilobalide extracts and purifying process ", disclosing a kind of bilobalide extracts and purifying process, its step is as follows: take by weighing the ginkgo cured leaf, pulverize, add 2-10 doubly to the ethanol or the methanol extraction of its weight by medicinal material weight, extracting solution reclaims the degreasing solvent removal of impurities of alcohol back, extraction, removal of impurities again, get raw product, use ethyl alcohol recrystallization again, filter, drying obtains the bilobalide highly finished product.This technology cost is low, pollute less, safe, gained bilobalide purity can reach more than 92%; But the extraction yield of this technology bilobalide is lower, causes the yield of final finished also lower.
(3) summary of the invention:
The present invention will disclose a kind of high method of extracting ginkgolide compound from Ginkgo Leaf of income rate height, product purity of extracting.
Ginkgolide compound of the present invention comprises Ginkgolide A, B, C, J and bilobalide.
The present invention extracts the method for ginkgolide compound 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 reclaims ethanol, again with obtaining ginkgolide compound behind the alcohol crystal;
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, promptly obtains ginkgolide compound.
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%, has also adopted special selective polarity not have macroporous adsorbent resin among the present invention and has carried out removal of impurities; Compared with prior art, method technology provided by the invention is simple, production cost is low, and gained ginkgolide compound product purity can reach more than 60%, 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% alcoholic acid crystallization again with volumetric concentration, obtain 70 gram ginkgolide compound crystal.
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.
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.

Claims (8)

1. extract the method for ginkgolide compound 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; Described usefulness Different concentrations of alcohol is from high to low extracted and is 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) ADS-15 is gone up in gained medicinal extract dilution back, or ADS-17, or the ADS-F8 adsorption resin column, uses ethanol elution, and the gained elutriant reclaims ethanol, again with obtaining ginkgolide compound behind the alcohol crystal.
2. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1, it is characterized in that: described ginkgolide compound comprises Ginkgolide A, B, C, J and bilobalide.
3. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1 and 2, it is characterized in that: in the step 1), the temperature of described extraction is 50-70 ℃.
4. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1 and 2, it is characterized in that: in the step 1), the time of described extraction is 1-3 hour.
5. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1 and 2 is characterized in that: in the step 1), and 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.
6. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1 and 2 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.
7. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1 and 2, it is characterized in that: in the step 3), described wash-out is 50-70% with the alcoholic acid volumetric concentration.
8. the method for extracting ginkgolide compound from Ginkgo Leaf according to claim 1 and 2, it is characterized in that: in the step 3), described crystallization is 50-80% with the alcoholic acid volumetric concentration.
CN2007100502417A 2007-10-15 2007-10-15 Method for extracting bilobalide compound from ginkgo leaf Expired - Fee Related CN101412724B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102464665B (en) * 2010-11-09 2015-04-08 上海医药工业研究院 Method for preparing ginkgolide A
CN104922109B (en) * 2015-05-25 2017-07-21 黑龙江珍宝岛药业股份有限公司 A kind of high purity ginkgolide composition and its preparation method and application
CN108703981B (en) * 2018-07-09 2021-04-13 湖北工程学院 Method for extracting ginkgetin from ginkgo leaves

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