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A method for extracting and separating shikimic acid from star anise

A technology of shikimic acid and star anise, which is applied in the extraction field of biotechnology, can solve the problems of large damage loss of active ingredients and large differences in content indicators, and achieve the effect of narrow particle distribution and good uniformity

Active Publication Date: 2018-06-05
GUANGXI WANSHAN SPICE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing traditional extraction method used for extraction and separation of shikimic acid uses petroleum ether as an organic solvent for extraction. Due to technical conditions, the active ingredients are greatly damaged and lost, and the content indicators vary greatly.

Method used

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  • A method for extracting and separating shikimic acid from star anise

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Experimental program
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Embodiment 1

[0022] A method for extracting and separating shikimic acid from star anise, specifically comprising the following steps:

[0023] 1) Pre-treatment: crush the star anise, extract it with pure water, concentrate it to obtain the extract, add the same weight of pure water, put it into a high-speed dispersing emulsifier for processing, the speed is 2500r / min, and the time is 10min to obtain a high-speed dispersing emulsion;

[0024] 2) Column chromatography: pass the high-speed dispersion emulsion obtained in step 1) through a 330 weakly basic epoxy-based anion resin column, so that shikimic acid is exchanged and adsorbed, and then eluted with 5% sodium hydroxide solution to obtain the washed Dehydration;

[0025] 3) Desalting: desalting the eluent obtained in step 2) through a 732 strongly acidic styrene-based cationic resin column to remove sodium salt;

[0026] 4) Crystallization: Concentrate the desalted eluate, add it to acetone, precipitate and crystallize shikimic acid, a...

Embodiment 2

[0028] A method for extracting and separating shikimic acid from star anise, specifically comprising the following steps:

[0029] 1) Pre-treatment: Grind the star anise, extract it with alcohol, concentrate it to obtain the extract, add the same weight of pure water, put it into a high-speed dispersing emulsifier for processing, the speed is 2000r / min, and the time is 8min to obtain a high-speed dispersing emulsion;

[0030] 2) Column chromatography: pass the high-speed dispersion emulsion obtained in step 1) through a D-941 macroporous weak base anion resin column, so that shikimic acid is exchanged and adsorbed, and then eluted with 8% sodium hydroxide solution to obtain the washed Dehydration;

[0031] 3) Desalting: desalting the eluent obtained in step 2) through a D001 macroporous strongly acidic styrene-based cationic resin column to remove sodium salt;

[0032] 4) Crystallization: Concentrate the desalted eluate, add it to acetone, precipitate and crystallize shikimic...

Embodiment 3

[0034] A method for extracting and separating shikimic acid from star anise, specifically comprising the following steps:

[0035] 1) Pretreatment: Degrease the extract obtained from star anise industrial residues with petroleum ether, add the same weight of pure water, put it into a high-speed dispersing emulsifier for processing, the speed is 3000r / min, and the time is 5min to obtain a high-speed dispersing emulsion ;

[0036] 2) Column chromatography: pass the high-speed dispersion emulsion obtained in step 1) through a D318 macroporous weak base anion resin column, so that shikimic acid is exchanged and adsorbed, and then eluted with 1% sodium hydroxide solution to obtain an eluent ;

[0037] 3) Desalting: the eluent obtained in step 2) is superacid 1 # Cationic resin column desalting to remove sodium salt;

[0038] 4) Crystallization: Concentrate the desalted eluate, add it to acetone, precipitate and crystallize shikimic acid, and then use acetone to recrystallize.

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Abstract

The invention discloses a method for extracting and separating shikimic acid from fructus anisi stellati. The method particularly comprises the following steps of 1 pretreatment, wherein an extract obtained by extracting the fructus anisi stellati is added to pure water with the weight equal to that of the extract, the materials are put into a high-speed dispersing and emulsifying machine to be treated, and a high-speed dispersed and emulsified mixture is obtained; 2 column chromatography, wherein the high-speed dispersed and emulsified mixture obtained in the first step passes through an anion resin column to enable the shikimic acid to be exchanged and adsorbed, elution is conducted with a sodium hydroxide solution, and eluent is obtained; 3 desalination, wherein the eluent obtained in the second step passes through a cationic resin column for desalination, and sodium salt is removed; 4 crystallization, wherein the desalinated eluent is concentrated and then added into acetone to enable the shikimic acid to be precipitated and crystallized, and then recrystallization is conducted with acetone.

Description

technical field [0001] The invention relates to an extraction method in the field of biotechnology, in particular to a method for extracting and separating shikimic acid from star anise. Background technique [0002] The molecular formula of shikimic acid is C 7 h 10 o 5 , the relative molecular weight is 174.15, the scientific name is 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid, it is white fine powder, slightly gas, bitter taste, soluble in water, insoluble in chloroform, benzene And petroleum ether, the melting point is 185°C, and the optical rotation is -180°. There are three hydroxyl groups, one carboxyl group, and one double bond in the molecular structure of shikimic acid, and it has chiral isomers. It can form esters or salts. Shikimic acid is an intermediate in the synthesis of biological and metabolic compounds, and it is also a raw material for the synthesis of many alkaloids, aromatic amino acids and indole derivatives, and chiral drugs (such as antivir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/42C07C62/32
CPCC07C51/42C07C62/32
Inventor 杨少凡陈思羽马创伟雷长林胡林刚赖积南
Owner GUANGXI WANSHAN SPICE