CN102351825B - Method for extracting and separating ginkgetin - Google Patents
Method for extracting and separating ginkgetin Download PDFInfo
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- CN102351825B CN102351825B CN2011102247359A CN201110224735A CN102351825B CN 102351825 B CN102351825 B CN 102351825B CN 2011102247359 A CN2011102247359 A CN 2011102247359A CN 201110224735 A CN201110224735 A CN 201110224735A CN 102351825 B CN102351825 B CN 102351825B
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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 and separating ginkgetin, namely a method of integrating solvent digestion, extraction, solvent re-crystallization and supercritical CO2 quick desolventizing crystallization. The method is used for deep processing of residue produced after a crude extract is prepared from ginkgo leaves so as to prepare the high-purity ginkgetin. Absolute ethyl alcohol and ethyl acetate are used for extracting; petroleum ether is used as a re-crystallization solvent; and the supercritical CO2 quick desolventizing crystallization is performed under the conditions that the pressure is less than or equal to 20MPa and the temperature is less than or equal to 50 DEG C. The highest content of the ginkgetin can reach over 98 percent. The separation and purification method is simple, convenient, low in cost and easy for industrial production and application.
Description
One, technical field
The present invention relates to a kind of Effective Component of Chinese Medicine extraction and separation method, exactly is a kind of extraction and separation method of ginkegetin.
Two, background technology
Ginkgo (Gimkgo biloba) has another name called maidenhair tree, is Ginkgoaceae, the Ginkgo plant.Ginkgo is distributed more widely in China.Mainly be distributed in the ground such as Jiangsu, Shandong, Guangxi, Yunnan, Guizhou, Sichuan, its owning amount accounts for more than 70% of world's total amount, and in recent years along with the development and use of gingko resource, China various places in a planned way enlarge the plantation of ginkgo.Since 1960's, because ginkgo agent is to control cardiovascular and cerebrovascular diseases, senile dementia with to the discovery of the effect of anti-platelet activating factor, strengthened the dynamics to aspect researchs such as ginkgo chemical composition, pharmacologically active and clinical applications both at home and abroad, and the extraction process of ginkgo effective constituent has been done a large amount of exploratory developments.
Ginkgo Leaf contains flavonoid compound, flavonoid glycoside, and its glucoside unit is respectively trifolitin, Quercetin, Isorhamnetol, bisflavones, and Folium Ginkgo terpene lactones A, B, C, pycnogenols, shikimic acid, β-sitosterol etc.
Flavonoid substances is a kind of physiologically active substance, and vitaminoid activity is arranged, and removes the ability of free radical, is good oxygen scavenqer and lipid antioxidant.Have and reduce blood pressure, prevent arteriosclerosis and anti-aging effects.
Wherein, the ginkegetin compounds has the extraordinary effect such as anticoagulation, anti-inflammatory and inhibition cAMP phosphodiesterase activity.
Consider that ginkegetin has above-mentioned exclusive effect, is necessary to extract separation.And it is domestic less to ginkegetin compounds extraction Separation Research.Mainly extract with the ether equal solvent, again with ethyl acetate be silicagel column separation on the elutriant (for example, Zhong Yuqing, Xu Li Son. " Acta Pharmaceutica Sinica ", 1995,30 (9): 694-697), mostly be greatly the pre-treating technology of analyte detection process raw material.Less to the report of the extraction Separation Research of ginkegetin class active substance both at home and abroad.
Three, summary of the invention
Content of the present invention is intended to for exploitation protective foods, new Chinese medicine provide high-quality bulk drug-ginkegetin, technical problem to be solved be ginkegetin extraction with separate.
Technical scheme of the present invention is to adopt water to extract the residue of traditional product Folium Ginkgo extract (GBE) as starting raw material as solvent take Ginkgo Leaf, it passes through first the dehydrated alcohol lixiviate, adopt the middle low polar solvent extractions such as ethyl acetate after dry, pass through again the low polar solvent crystallizations such as sherwood oil, carry out supercritical CO after concentrating
2Fast precipitation crystallization can obtain " green " high purity silver ginkgetin product.
Concrete technical scheme is:
The Ginkgo Leaf residue is dissolved in the dehydrated alcohol, is dissolved into behind the concentrate drying in the warm water, use again ethyl acetate extraction 2 times, adopt sherwood oil crystallization 2-3 time behind the extraction liquid precipitation, adopt again supercritical CO after concentrating
2Precipitation crystallization time 20-30min, Tc 35-50 ℃, pressure 8-20MPa can make purity up to the high sterling of the ginkegetin more than 98% fast.
Concrete operation step is
(1) residue of at first selecting warm water (40-60 ℃) to extract behind the Ginkgo Leaf is raw material, selects anhydrous alcohol solution, the temperature of 5-8 times of volume to be controlled at 50-70 ℃, extracts 2-3 time at least;
(2) with after extracting solution merging, the precipitation drying, adopt the warm water (35-45 ℃) of 3 times of volumes to dissolve, adopt again ethyl acetate solvent extraction 2 times;
(3) concentrated after the extraction liquids merging, vacuum concentration are dried to powder, adopt sherwood oil to carry out recrystallization 2-3 time again, purity reaches more than 90%;
(4) above-mentioned crystal crude product is carried out supercritical CO
2Fast precipitation crystallization is controlled at pressure 8～20MPa, and temperature is at 35～50 ℃, and the time is at 20～30min;
(5) shut down the rear anti-solvent crystallization product of collecting, can make purity 98% above ginkegetin.
This law technique is simple, need not complicated, consuming time, the power consumption techniques such as column chromatography, lyophilize be dry.Its yield is also high than traditional technology simultaneously, and ginkegetin purity surpasses 98%, and yield 〉=30% (in ginkegetin in the Ginkgo Leaf) is fit to batch production.At present, the residue utilization ratio that the apricot leaf prepares behind the GBE is low, and low price carries out this Project Product exploitation and both improved the production efficiency of separation and purification, reduce again the Ginkgo Leaf residue environmental pollution, turn waste into wealth.
Four, embodiment
Embodiment 1:
1. take by weighing the residue dry product behind the 10kg warm water extraction Ginkgo Leaf, be dissolved in the dehydrated alcohol by the solid-to-liquid ratio of 1: 6 (W/V), 55 ℃ of extraction temperature extract 2;
2. the merging of dehydrated alcohol extraction liquid, vacuum desolvation are obtained pressed powder, powder is adopted 35 ℃ of warm water dissolvings of 3 times of volumes, adopt again ethyl acetate solvent extraction 2 times;
3. concentrated after extraction liquids merges, vacuum concentration is dried to powder, adopts sherwood oil to carry out recrystallization 3 times again, and purity reaches more than 90%;
4. above-mentioned crystal crude product is carried out supercritical CO
2Fast precipitation crystallization is controlled at pressure 10MPa, and temperature is at 40 ℃, and the time is at 20min;
5. after the off-test, sampling detects, and can obtain the high purity silver ginkgetin 3.5g of purity 98.5%.
Embodiment 2:
1. take by weighing the residue dry product behind the 10kg warm water extraction Ginkgo Leaf, be dissolved in the dehydrated alcohol by the solid-to-liquid ratio of 1: 7 (W/V), 65 ℃ of extraction temperature extract 3;
2. the merging of dehydrated alcohol extraction liquid, vacuum desolvation are obtained pressed powder, powder is adopted 45 ℃ of warm water dissolvings of 3 times of volumes, adopt again ethyl acetate solvent extraction 2 times;
3. concentrated after extraction liquids merges, vacuum concentration is dried to powder, adopts sherwood oil to carry out recrystallization 2 times again, and purity reaches more than 90%;
4. above-mentioned crystal crude product is carried out supercritical CO
2Fast precipitation crystallization is controlled at pressure 15MPa, and temperature is at 45 ℃, and the time is at 30min;
5. after the off-test, sampling detects, and can obtain the high purity silver ginkgetin 4.2g of purity 98.7%.
Claims (1)
1. the extraction and separation method of a ginkegetin, concrete operation step is:
(1) at first selecting the 40-60 ℃ of residue behind the warm water extraction Ginkgo Leaf is raw material, selects anhydrous alcohol solution, the temperature of 5-8 times of volume to be controlled at 50-70 ℃, extracts 2-3 time at least;
(2) with after extracting solution merging, the precipitation drying, adopt 35-45 ℃ of warm water of 3 times of volumes to dissolve, adopt again ethyl acetate solvent extraction 2 times;
(3) concentrated after the extraction liquids merging, vacuum concentration are dried to powder, adopt sherwood oil to carry out recrystallization 2-3 time again, purity reaches more than 90%;
(4) above-mentioned crystal crude product is carried out supercritical CO
2Fast precipitation crystallization is controlled at pressure 8～20MPa, and temperature is at 35～50 ℃, and the time is at 20～30min;
(5) shut down the rear anti-solvent crystallization product of collecting, make purity 98% above ginkegetin.
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| CN2011102247359A CN102351825B (en) | 2011-08-08 | 2011-08-08 | Method for extracting and separating ginkgetin |
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| CN2011102247359A CN102351825B (en) | 2011-08-08 | 2011-08-08 | Method for extracting and separating ginkgetin |
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| CN102351825A CN102351825A (en) | 2012-02-15 |
| CN102351825B true CN102351825B (en) | 2013-01-30 |
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Families Citing this family (3)
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| CN104387356B (en) * | 2013-11-15 | 2016-05-04 | 广西莱吉生物工程有限公司 | In ginkgo leaf, extract the method for flavones |
| CN105456309A (en) * | 2015-12-17 | 2016-04-06 | 东北林业大学 | Process for purifying ginkgetin in gingko extract through anti-solvent recrystallization method |
| CN110585251A (en) * | 2019-10-21 | 2019-12-20 | 西安工程大学 | Method for extracting ginkgetin by using n-butanol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049301A (en) * | 2007-05-14 | 2007-10-10 | 湖北中医学院 | Pharmaceutical preparation of biflavone compound for anti gout |
| CN101991567A (en) * | 2009-08-24 | 2011-03-30 | 赵全成 | Application of three biflavone monomer components extracted from ginkgo leaves in preparing medicament of alpha-glucosidase inhibitor |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049301A (en) * | 2007-05-14 | 2007-10-10 | 湖北中医学院 | Pharmaceutical preparation of biflavone compound for anti gout |
| CN101991567A (en) * | 2009-08-24 | 2011-03-30 | 赵全成 | Application of three biflavone monomer components extracted from ginkgo leaves in preparing medicament of alpha-glucosidase inhibitor |
Non-Patent Citations (4)
| Title |
|---|
| .银杏叶主要活性成分及含量测定方法研究.《中国中医药科技》.2000,第7卷(第4期),第232页. * |
| 姜倩倩 * |
| 季大洪 * |
| 王兴华 * |
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Owner name: JIANGSU BESCON PHARMACEUTICAL CO., LTD. Free format text: FORMER NAME: XUZHOU KANGTAI BIOLOGICAL PRODUCTIONS CO., LTD. |
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Address after: 221300 Jiangsu Province, Pizhou City Industrial Park Patentee after: Jiangsu Bescon Pharmaceutical Co., Ltd. Address before: 221300 Jiangsu Province, Pizhou City Industrial Park Patentee before: Xuzhou Kangtai Biological Product Co.,Ltd. |