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Process of extracting and separating shikimic acid from aniseed

A technology of shikimic acid and star anise, applied in chemical instruments and methods, medical preparations containing active ingredients, pharmaceutical formulas, etc., can solve the problems of large differences in content indicators, large damage loss of active ingredients, and high cost, and is easy to promote , Reduce production costs and reduce energy consumption

Inactive Publication Date: 2007-03-21
GUANGXI WANSHAN SPICE +1
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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 is extraction with organic solvents such as petroleum ether. Due to technical conditions, the active ingredient is damaged and lost, the content index varies greatly, and the cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 50 kg of star anise medicinal material (the content of medicinal material is 11.5%), crush it into coarse powder, put it into an extraction tank; add 5 times, 3 times, and 2 times of water respectively (based on the quality of star anise), boil it and extract it three times , put the extract on a 330 weakly basic epoxy-based anion-exchange resin column, fully wash with deionized water until the color is clear, elute with 3% sodium hydroxide, and pass through a 732 strong-acidic styrene-based cation-exchange resin column for desalting to remove sodium Salt, adsorption and elution flow rate is 1 / 2 the resin volume per hour. Concentrate the eluent under reduced pressure at 80°C to a thick paste, add acetone to precipitate the crude shikimic acid, and recrystallize the crude shikimic acid with acetone solvent to obtain 5.0 kg of 98.5% finished shikimic acid.

Embodiment 2

[0037] Take 50 kg of star anise medicinal material (medicinal material content 9.5%), grind it into coarse powder, put it into an extraction tank; add 5 times, 4 times, and 3 times of water respectively, boil it and keep it warm for extraction three times, and adjust the pH of the extract to 9 , on the D-941 macroporous weak base anion exchange resin column, fully washed with deionized water until the color is clear, eluted with 8% sodium hydroxide, and desalted through D001 macroporous strongly acidic styrene-based cation exchange resin column to remove sodium salt , the adsorption and elution flow rate is 1 / 2 of the resin volume per hour. Concentrate the eluent at 70°C under reduced pressure to a thick paste, add acetone to precipitate the crude shikimic acid, and recrystallize the crude shikimic acid with acetone solvent to obtain 4.1 kg of 99% finished shikimic acid.

Embodiment 3

[0039] Take 50 kg of star anise medicinal material (medicinal material content 10.7%), crush it into coarse powder, put it into an extraction tank; add 4 times, 3 times, and 2 times of water respectively, boil it and keep it warm for extraction three times, and adjust the pH of the extract to 7 , on a D318 macroporous weak base anion exchange resin column, fully washed with deionized water until the color is clear, and eluted with 1% sodium hydroxide, superacid 1 # Cationic column desalting to remove sodium salt, the adsorption and elution flow rate is 1 / 2 of the resin volume per hour. Concentrate the eluate at 90°C under reduced pressure to a thick paste, add acetone to precipitate the crude shikimic acid, and recrystallize the crude shikimic acid with acetone solvent to obtain 4.8 kg of 98.8% finished shikimic acid.

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PUM

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Abstract

The present invention is process of extracting and separating shikimic acid from aniseed. The process includes the steps of water extraction to obtain extracted solution, exchanging and adsorbing shikimic acid from the extracted solution with anionic resin column, eluting with 1-8 % sodium hydroxide solution to obtain eluted solution, desalting the eluted solution in cationic resin column, concentrating the desalted solution and crystallizing in acetone to obtain shikimic acid crystal. Compared with traditional technology, the present invention has the advantages of low power consumption, low production cost and less environmental pollution.

Description

technical field [0001] The invention relates to a chemical extraction method, in particular to a method for extracting and separating shikimic acid from star anise by an ion exchange method. 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 acid, 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 anti...

Claims

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Application Information

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IPC IPC(8): C07C62/04C07C51/64A61K36/57A61K131/00
Inventor 韦万章刘新伟
Owner GUANGXI WANSHAN SPICE
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