CN102351825A - Method for extracting and separating ginkgetin - Google Patents
Method for extracting and separating ginkgetin Download PDFInfo
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- CN102351825A CN102351825A CN2011102247359A CN201110224735A CN102351825A CN 102351825 A CN102351825 A CN 102351825A CN 2011102247359 A CN2011102247359 A CN 2011102247359A CN 201110224735 A CN201110224735 A CN 201110224735A CN 102351825 A CN102351825 A CN 102351825A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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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 Chinese medicine extracts active ingredients 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 distributes wider in China.Mainly be distributed in 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 dynamics both at home and abroad, and the extraction process of ginkgo effective constituent has been done a large amount of exploratory developments aspect researchs such as ginkgo chemical ingredients, pharmacologically active and clinical applications.
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-Gu Zaichun etc.
Flavonoid substances is a kind of physiologically active substance, and vitaminoid activity is arranged, and removes the ability of radical, is good oxygen scavenqer and lipid antioxidant.Have and bring high blood pressure down, prevent arteriosclerosis and anti-aging effects.
Wherein, the ginkegetin compounds has extraordinary effect such as anticoagulation, anti-inflammatory and inhibition cAMP phosphodiesterase activity.
Consider that ginkegetin has above-mentioned exclusive effect, is necessary to carry out extraction separation.And it is domestic less to the research of ginkegetin compounds extraction separation.Mainly extract with the ether equal solvent, use again ETHYLE ACETATE as silicagel column on the elutriant separate (for example, Zhong Yuqing, Xu Li Son. " Acta Pharmaceutica Sinica ", 1995,30 (9): 694-697), be the pre-treating technology of analyte detection process raw material mostly.Less both at home and abroad to the report of the extraction separation research of ginkegetin class active substance.
Three, summary of the invention
Content of the present invention is intended to for exploitation protective foods, new Chinese medicine provide high-quality raw materials medicine-ginkegetin, technical problem to be solved be ginkegetin extraction with separate.
Technical scheme of the present invention is that to adopt water with Ginkgo Leaf be starting raw material as the residue that solvent extracts traditional product Folium Ginkgo extract (GBE); It is earlier through the absolute ethyl alcohol lixiviate; Middle low polar solvent extractions such as ETHYLE ACETATE are adopted in dry back; Pass through low polar solvent crystallizations such as sherwood oil again, carry out supercritical CO after concentrating
2Precipitation crystallization fast can obtain " green " high-purity ginkegetin product.
Concrete technical scheme is:
The Ginkgo Leaf residue is dissolved in the absolute ethyl alcohol, is dissolved into behind the concentrate drying in the warm water, use ethyl acetate extraction again 2 times, adopt sherwood oil crystallization 2-3 time behind the extraction liquid precipitation, adopt supercritical CO again after concentrating
2Precipitation crystallization time 20-30min, Tc 35-50 ℃ fast, pressure 8-20MPa can make purity up to the high-purity article of the ginkegetin more than 98%.
The concrete operations step is
(1) residue of at first selecting warm water (40-60 ℃) to extract behind the Ginkgo Leaf is a 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 ethyl acetate solvent extraction 2 times again;
(3) extraction liquids merging back is concentrated, vacuum concentration is dried to powder, adopts sherwood oil to carry out recrystallization 2-3 time again, and purity reaches more than 90%;
(4) above-mentioned crystal crude product is carried out supercritical CO
2Precipitation crystallization fast is controlled at pressure 8～20MPa, and temperature is at 35～50 ℃, and the time is at 20～30min;
(5) shut down the back and collect anti-solvent crystallization product, can make purity 98% above ginkegetin.
This law technology is simple, need not complicated, consuming time, power consumption technologies 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 produce in batches.At present, the residue utilization ratio that the apricot leaf prepares behind the GBE is low, and low price carries out the production efficiency that the product development of this project had both improved 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 absolute ethyl 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 precipitation are obtained pressed powder, adopt 35 ℃ of warm water of 3 times of volumes to dissolve in powder, adopt ethyl acetate solvent extraction 2 times again;
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
2Precipitation crystallization fast 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 high-purity ginkegetin 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 absolute ethyl 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 precipitation are obtained pressed powder, adopt 45 ℃ of warm water of 3 times of volumes to dissolve in powder, adopt ethyl acetate solvent extraction 2 times again;
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
2Precipitation crystallization fast 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 high-purity ginkegetin 4.2g of purity 98.7%.
Claims (4)
1. the extraction and separation method of a ginkegetin, the concrete operations step is:
(1) residue of at first selecting warm water (40-60 ℃) to extract behind the Ginkgo Leaf is a 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 ethyl acetate solvent extraction 2 times again;
(3) extraction liquids merging back is concentrated, vacuum concentration is dried to powder, adopts sherwood oil to carry out recrystallization 2-3 time again, and purity reaches more than 90%;
(4) above-mentioned crystal crude product is carried out supercritical CO
2Precipitation crystallization fast is controlled at pressure 8～20MPa, and temperature is at 35～50 ℃, and the time is at 20～30min;
(5) shut down the back and collect anti-solvent crystallization product, can make purity 98% above ginkegetin.
2. the extraction and separation method of a kind of ginkegetin according to claim 1; It is characterized in that: 50-70 ℃ of dehydrated alcohol extraction 2-6 time of described employing, ethyl acetate extraction 2-4 time; The extraction liquid precipitation obtains pressed powder, uses sherwood oil crystallization 2-6 time then, is placed on supercritical CO at last
2In fast precipitation crystallization.
3. the extraction and separation method of a kind of ginkegetin according to claim 1, it is characterized in that: the recrystallization organic solvent is selected from sherwood oil.
4. the extraction and separation method of a kind of ginkegetin according to claim 1 is characterized in that: supercritical CO
2Precipitation crystallization fast; Processing parameter is controlled at pressure 5～25MPa, and temperature is at 30～55 ℃, and the time is at 15～35min.
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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 true CN102351825A (en) | 2012-02-15 |
| CN102351825B CN102351825B (en) | 2013-01-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387356A (en) * | 2013-11-15 | 2015-03-04 | 广西莱吉生物工程有限公司 | Method for extracting flavone from folium ginkgo |
| 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 |
-
2011
- 2011-08-08 CN CN2011102247359A patent/CN102351825B/en active Active
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 (1)
| Title |
|---|
| 季大洪; 姜倩倩; 王兴华;: "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》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387356A (en) * | 2013-11-15 | 2015-03-04 | 广西莱吉生物工程有限公司 | Method for extracting flavone from folium ginkgo |
| 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 |
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| CN102351825B (en) | 2013-01-30 |
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