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A kind of extraction separation method of ginkgo diterpene lactone

A technology for the separation of ginkgo diterpene lactones, which is applied in the direction of organic chemistry, can solve the problems of high ginkgolic acid content, low yield and low purity of ginkgo diterpene lactones, and achieve low ginkgolic acid content, high purity, and production low cost effect

Active Publication Date: 2019-02-22
JIANGSU KANION PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the extraction method of "CN 1195665 A" ginkgolide and the preparation containing ginkgolide have a low yield and purity of ginkgo diterpene lactone, and the content of ginkgolic acid is relatively high

Method used

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  • A kind of extraction separation method of ginkgo diterpene lactone
  • A kind of extraction separation method of ginkgo diterpene lactone
  • A kind of extraction separation method of ginkgo diterpene lactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Get Ginkgo biloba (the dried leaf of Ginkgo biloba L. of Ginkgoaceae plant Ginkgo biloba L., purchased in Pizhou, Jiangsu) medical material 50kg, add 14 times the amount of decoction and extract 3 times, each time for 1 hour, combine the extracts, concentrate, filter to obtain Concentrate. Add 10% active carbon by weight of ginkgo biloba to the concentrated solution, stir and adsorb for 24 hours, let stand overnight, discard the supernatant, and collect the adsorbent. Add 20L methanol to the adsorbent, heat to boil for 1 hour, let cool, take the supernatant, add 20L methanol to the extracted adsorbent and repeat the extraction twice, combine the above three extracts, concentrate under reduced pressure to obtain concentrated Liquid (relative density 1.35) was refrigerated for 3 days. Centrifuge the refrigerated concentrated solution, collect the precipitate, add water to the precipitate and wash 3 times, discard the water, add 5 times the amount of methanol to the preci...

Embodiment 2

[0037] Get Ginkgo biloba (the dry leaf of Ginkgo biloba L. of Ginkgoaceae plant Ginkgo biloba L., purchased in Pizhou, Jiangsu) medical material 50kg, add 8 times the amount of 10% ethanol and heat and reflux to extract 2 times, each time for 1.5 hours, combine the extracts, concentrate, filter , to obtain a concentrated solution. Add 15% polyamide by weight of ginkgo biloba to the concentrated solution, stir and adsorb for 36 hours, let stand overnight, discard the supernatant, and collect the adsorbent. Add 30L 95% ethanol to the adsorbent, heat to boiling for 1.5 hours, let cool, take the supernatant, add 30L ethanol to the extracted adsorbent and repeat the extraction 3 times, combine the above 4 extracts, concentrate under reduced pressure, The concentrated solution (d=1.40) was refrigerated for 5 days. Centrifuge the refrigerated concentrate, collect the precipitate, add water to the precipitate and wash 3 times, discard the water, add 2 times the amount of ethanol to t...

Embodiment 3

[0040] Get Ginkgo biloba (the dry leaf of Ginkgo biloba L. of Ginkgoaceae plant Ginkgo biloba L., purchased in Pizhou, Jiangsu) medical material 50kg, add 5 times the amount of 20% ethanol and heat and reflux to extract 4 times, each time for 3 hours, combine the extracts, concentrate, filter , to obtain a concentrated solution. Add 20% silica gel by weight of ginkgo biloba to the concentrated solution, stir and adsorb for 48 hours, let stand overnight, discard the supernatant, and collect the adsorbent. Add 20L 40% acetone to the adsorbent, heat it to boiling for 1.5 hours, let it cool, take the supernatant, add 20L 40% acetone to the extracted adsorbent and repeat the extraction twice, combine the above three extracts, and depressurize Concentrate to obtain a concentrated solution (d=1.38) and refrigerate for 3 days. Take the refrigerated concentrated solution and centrifuge to collect the precipitate, add water to the precipitate and wash 3 times, discard the water, add 5 ...

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Abstract

A method for extraction and separation of ginkgo biloba diterpene lactones is disclosed. The method includes a step of subjecting ginkgo leaves to extraction with a solvent, and concentrating an extract liquid to obtain a concentrate; a step of adding an adsorbent into the concentrate, stirring the mixture, performing adsorption, allowing a liquid containing the adsorbent to stand, removing liquidsupernatant, and collecting the adsorbent; a step of adding a solvent into the adsorbent, heating the mixture, performing extraction, concentrating an extract liquid and refrigerating a concentrate;a step of centrifuging the refrigerated concentrate, collecting precipitates, adding water into the precipitates to wash the precipitates, then adding a proper organic solvent into the obtained precipitates to perform extraction, and performing filtration and recovering the solvent until a product is dry so that a crude product of total precipitates; and a step of adding water into the crude product to wash the crude product, removing an aqueous solution, then adding an organic solvent, and performing recrystallization to obtain a refined product of the ginkgo biloba diterpene lactones. The method has stable process conditions, and can obtain the ginkgo biloba diterpene lactones having relatively fixed components. The content of ginkgolic acid in the obtained ginkgo biloba diterpene lactones is less than 2 ppm, and no bilobalide is detected.

Description

technical field [0001] The invention relates to the field of plant extraction, in particular to a method for extracting and separating ginkgo diterpene lactones. Background technique [0002] Ginkgo biloba is one of the oldest plants on earth and has unique pharmacological effects and clinical application value. Since the 1960s, foreign studies on the chemical composition, pharmacological activity and clinical application of ginkgo have shown that the part with the greatest medicinal value of ginkgo is the leaf. The most important active ingredients in Ginkgo biloba and its preparations are Ginkgo diterpene lactones and flavonoids. [0003] Ginkgo diterpene lactones are unique and rare natural compounds in Ginkgo biloba, which have not been found in other plants so far. Modern pharmacological studies have shown that ginkgo diterpene lactones have strong specific inhibitory activity on receptors, are specific platelet activating factor (PAF) antagonists, and can inhibit pla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 萧伟周恩丽康小东王永香殷洪梅胡晗绯吴云王振中章晨峰
Owner JIANGSU KANION PHARMA CO LTD
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