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Method for separation and purification of shikimic acid from ginkgo biloba leaves

A technology of deciduous leaves and ginkgo biloba, applied in the field of separation and purification of shikimic acid, can solve the problems of large dosage and limited star anise resources, achieve high yield, simple and feasible extraction method, and relieve demand pressure

Active Publication Date: 2017-01-11
贵州北极兴药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Star anise belongs to the same origin of medicine and food. It can be used for family consumption and in traditional Chinese medicine formulas. It is used in a large amount among the people. At present, almost all shikimic acid in the world is extracted from star anise. Although the extraction The method is very mature, but the resources of star anise are limited, which cannot meet the current demand of the whole world for shikimic acid. Therefore, there are studies on the extraction of shikimic acid from the star anise leaf and the waste residue after the essential oil extraction of the star anise leaf
But so far there is no relevant report on the isolation and purification of shikimic acid from Ginkgo biloba leaves

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for separating and purifying shikimic acid from ginkgo leaves, comprising the following steps:

[0020] (1) Dry and crush the fallen leaves of Ginkgo biloba, then reflux extract with 70% ethanol for 3 times, each time for 1 hour, combine the extracts, concentrate under reduced pressure to an extract; the mass volume of fallen leaves of Ginkgo biloba and 70% ethanol during each extraction process The ratio is 0.25g / mL;

[0021] (2) Ultrasonic dissolve the extract obtained in step (1) in deionized water, and then sequentially extract with petroleum ether, ethyl acetate and n-butanol, each solution is extracted 3 times, and the extracted aqueous solution is combined and rotated Evaporate to dryness by rotary evaporation in an evaporator to obtain an aqueous phase extract;

[0022] (3) Dissolve the aqueous phase extract obtained in step (2) in methanol, and then mix it with 100-200 mesh silica gel, stir evenly, dry at 40°C and cool to room temperature; the extract...

Embodiment 2

[0026] A method for separating and purifying shikimic acid from ginkgo leaves, comprising the following steps:

[0027] (1) Ginkgo fallen leaves are dried and crushed, and then refluxed with 70% ethanol for 2 times, each time for 1.5h, the extracts are combined, concentrated under reduced pressure to an extract; the mass of ginkgo fallen leaves and 70% ethanol in each extraction process The volume ratio is 0.3g / mL;

[0028] (2) Ultrasonic dissolve the extract obtained in step (1) in deionized water, and then sequentially extract with petroleum ether, ethyl acetate and n-butanol, each solution is extracted 3 times, and the extracted aqueous solution is combined and rotated Combined after rotary evaporation in the evaporator to obtain the aqueous phase extract;

[0029] (3) Dissolve the aqueous phase extract obtained in step (2) in methanol, and then mix it with 100-200 mesh silica gel, stir evenly, dry at 40°C and cool to room temperature; the extract obtained in step (1) The...

Embodiment 3

[0033] A method for separating and purifying shikimic acid from ginkgo leaves, comprising the following steps:

[0034] (1) Dry and crush the fallen leaves of Ginkgo biloba, then reflux extract with 70% ethanol for 3 times, each time for 2 hours, combine the extracts, concentrate under reduced pressure to an extract; the mass volume of fallen leaves of Ginkgo biloba and 70% ethanol during each extraction process The ratio is 0.35g / mL;

[0035] (2) Ultrasonic dissolve the extract obtained in step (1) in deionized water, and then sequentially extract with petroleum ether, ethyl acetate and n-butanol, each solution is extracted 3 times, and the extracted aqueous solution is combined and rotated Evaporate to dryness by rotary evaporation in an evaporator to obtain an aqueous phase extract;

[0036] (3) Dissolve the aqueous phase extract obtained in step (2) in methanol, and then mix it with 100-200 mesh silica gel, stir evenly, dry at 40°C and cool to room temperature; the extrac...

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Abstract

The invention discloses a method for separation and purification of shikimic acid from ginkgo biloba leaves, which comprises the following steps: 1, drying and smashing the ginkgo biloba leaves and refluxing and extracting through ethyl alcohol with the mass percentage being 70%, and then concentrating the mixture into a concrete shape; 2, using ultrasound to dissolve the concentrate obtained in step one in deionized water and then using petroleum ether, ethyl acetate and n-butyl alcohol to extract sequentially, and obtaining aqueous phase concrete after the aqueous phase is fully concentrated; 3, dissolving the aqueous phase concrete obtained from step two into methyl alcohol, blending with 100-200 parts of target silica gel and then drying the mixture; 4, packing the dry substance obtained in step three, eluting the substance through the mixture of ethyl acetate and methyl alcohol, gathering elution fluid, concentrating the elution fluid until the fluid is fully dry, and obtaining rough shikimic acid; 5, producing shikimic acid crystal through the recrystallization of the methyl alcohol. The method for separation and purification of shikimic acid from ginkgo biloba leaves uses ginkgo biloba leaves as the raw materials, and realizes the cyclic utilization of waste resources, having the advantages of simple extraction process and low cost; meanwhile, the shikimic acid has high production rate and purity.

Description

technical field [0001] The invention relates to the technical field of shikimic acid separation and purification, in particular to a method for separating and purifying shikimic acid from ginkgo leaves. Background technique [0002] Shikimic acid, the chemical name is 3,4,5-trihydroxy-1-cyclohexyl-1-carboxylic acid, the melting point is 185-187°C, easily soluble in water, insoluble in chloroform, benzene and petroleum Ether has anti-inflammatory, analgesic, antithrombotic, cerebral ischemia, and antitumor effects. Currently, Tamiflu, the only effective treatment drug for H5N1 avian influenza virus confirmed by the World Health Organization, is synthesized from shikimic acid. The preliminary study of the Pharmacology Laboratory of Beijing University of Traditional Chinese Medicine found for the first time that shikimic acid has obvious antithrombotic effect, can inhibit Arterial and venous thrombosis and cerebral thrombosis. [0003] In 1960, Simonart and Wiaux reported the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/47C07C51/48C07C62/32
CPCC07C51/42C07C51/47C07C51/48C07C62/32
Inventor 王晓玲常颜唐晓莹陈炼红
Owner 贵州北极兴药业有限公司
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