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Method for separating refined dihydroartemisinic acid from artemisinin production waste through ion-exchange resin method

A technology of ion exchange resin and dihydroartemisinic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of resource waste, achieve high recovery rate, reduce concentration time and energy consumption, and facilitate operation Effect

Inactive Publication Date: 2014-12-24
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production process of artemisinin, dihydroartemisinic acid is also extracted from the plant at the same time, but in the further separation and purification of artemisinin, dihydroartemisinic acid is left in the production waste, and there is no re-use, resulting in a large waste of resources

Method used

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  • Method for separating refined dihydroartemisinic acid from artemisinin production waste through ion-exchange resin method
  • Method for separating refined dihydroartemisinic acid from artemisinin production waste through ion-exchange resin method

Examples

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Effect test

Embodiment 1

[0020] Take 100g of completely dried artemisinin production waste, add 450mL of 0.3% (W / V) sodium hydroxide solution, crush the artemisinin production waste, adjust the pH value to 8.0, soak at 50°C for 30min, and centrifuge at 2500rpm at room temperature 15min, take the supernatant. Open the lower end plug of the chromatography column and load it on the column at a speed of 1.5BV / h (the initial processing capacity of 717 anion exchange resin is 100mL). After loading the column, close the lower end plug of the chromatography column and statically adsorb to saturation. After the adsorption is complete, open the plunger at the lower end of the chromatographic column and rinse with 500 mL of deionized water at a rate of 6 BV / h. Take 10% (W / V) ammonium chloride solution and 60% (V / V) edible alcohol mixed in a 1:1 volume ratio, add the mixed solution to the chromatographic column, and elute at a speed of 3BV / h, collect the eluted A total of 350mL was removed. At 40°C, concentrate...

Embodiment 2

[0024] Take 725g of completely dried artemisinin production waste, add 2200mL of 0.3% (W / V) sodium hydroxide solution, crush the artemisinin production waste, adjust the pH value to 9.0, soak at 60°C for 20min, and centrifuge at 3000rpm at room temperature 15min, take the supernatant. Open the lower end piston of the chromatography column and load it on the column at a speed of 1BV / h (the initial processing capacity of 717 anion exchange resin is 500mL). After the adsorption is completed, open the plunger at the lower end of the chromatographic column, and rinse with 3000 mL of deionized water at a rate of 4 BV / h. Get the mixed solution of 6% (W / V) ammonium chloride solution and 85% (V / V) edible alcohol mixed by 1:1 volume ratio, add the chromatographic column, carry out elution with the speed of 2BV / h, collect and wash A total of 1500mL was removed. At 35°C, the eluate was concentrated in vacuo to 1 / 3 volume, then extracted twice with 500mL of dichloromethane, the extracts ...

Embodiment 3

[0026] Take 1.2kg of completely dry artemisinin production waste, add 4.8L of 0.3% (W / V) sodium hydroxide solution, crush the artemisinin production waste, adjust the pH value to 8.5, soak at 55°C for 26min, and Centrifuge at 2800rpm for 15min, and take the supernatant. Open the lower plug of the chromatography column, and load the column at a rate of 1.2BV / h (the initial processing capacity of 717 anion exchange resin is 1000mL). After loading the column, close the lower plug of the chromatography column, and statically adsorb to saturation. After the adsorption is completed, open the lower end piston of the chromatography column and wash with 5.5L deionized water at a washing speed of 5BV / h. Take 8% (W / V) ammonium chloride solution and 70% (V / V) edible alcohol mixed in a 1:1 volume ratio, add the mixed solution to the chromatography column, and elute at a speed of 2.5BV / h, collect A total of 3.3L of eluate. At 38°C, the eluate was concentrated in vacuo to 1 / 3 volume, then ...

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Abstract

The invention discloses a method for separating refined dihydroartemisinic acid from artemisinin production waste through an ion-exchange resin method. The method for separating the refined dihydroartemisinic acid from the artemisinin production waste through the ion-exchange resin method comprises enabling the dried artemisinin production waste to be served as raw materials, dissolving through a sodium hydroxide solution, centrifuging to remove precipitate, obtaining supernatant liquor, gradually adding preprocessed and balanced processed anion exchange resin, flushing through deionized water, performing desorption, collecting eluent, perform vacuum concentration, performing extraction through organic solvent and finally obtaining high-purity dihydroartemisinic acid products through crystallization. According to the method for separating the refined dihydroartemisinic acid from the artemisinin production waste through the ion-exchange resin method, the artemisinin production waste is served as the raw materials firstly and the dihydroartemisinic acid is separated and purified through the ion-exchange resin method; the concentration time and energy consumption are reduced due to the vacuum concentration and organic solvent extraction combined technology, the product yield is increased, production costs are reduced, the product purity which is high is more than 99%; the recovery rate which is high in larger than 80%; the operation is convenient, the production is large, and industrial scale production is easy to achieve.

Description

technical field [0001] The invention relates to a method for preparing dihydroartemisinic acid, in particular to a method for separating and refining dihydroartemisinic acid from artemisinic acid production waste by using an ion exchange resin method. Background technique [0002] Artemisia annua is an important economic crop of national treasure level in my country. Its main active ingredient artemisinin is the first natural medicine developed in my country that is internationally recognized and has independent intellectual property rights. traditional Chinese medicine. Chinese scientist Tu Youyou won my country's first Lax Award in 2011 for her outstanding contribution to the discovery of artemisinin. Since the World Health Organization identified artemisinin as the safest and most effective antimalarial drug at present, and as the first drug to treat malaria, the market demand for artemisinin has grown rapidly. At present, drugs based on artemisinin are sold in 31 countr...

Claims

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Application Information

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IPC IPC(8): C07C57/26C07C51/42C07C51/47
CPCC07C51/43C07C51/47C07C51/48C07C57/26
Inventor 刘硕谦田冬铭廖欢曹娟扬威吴敦超周兰
Owner HUNAN AGRICULTURAL UNIV
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