Method for recovering artemisinin from artemisinin recrystallization waste

A technology of artemisinin and recrystallization, applied in organic chemistry methods, organic chemistry, etc., can solve the problems of low recovery rate and low purity, achieve simple steps, stable process, and improve the effect of impurity removal

Active Publication Date: 2019-04-19
GUANGXI XIANCAOTANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for recovering artemisinin from artemisinin recrystallization waste in view of the low recovery rate and low purity of artemisinin recrystallization waste

Method used

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  • Method for recovering artemisinin from artemisinin recrystallization waste
  • Method for recovering artemisinin from artemisinin recrystallization waste
  • Method for recovering artemisinin from artemisinin recrystallization waste

Examples

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Embodiment 1

[0035] A method for recovering artemisinin from artemisinin recrystallization waste, comprising the following steps:

[0036]a. Primary crystallization: According to the weight ratio, take 30 parts of artemisinin recrystallization waste, heat it in a water bath to 50 ° C to dissolve, add 13 parts of a mixed solution of petroleum ether and ethyl acetate, keep the temperature and stir for 20 minutes, and continue to maintain Stand still at temperature until the solution is separated into layers. At this time, it can be seen that crystals are precipitated in the lower layer solution, and then the upper layer solution is separated for subsequent use. Then the lower layer solution is filtered while it is hot, and the filtered crystals are washed repeatedly with a mixed solution of petroleum ether and ethyl acetate for 2 times, get one crystal;

[0037] Wherein, the volume ratio of the mixed solution of petroleum ether and ethyl acetate is 80:2.

[0038] The cleaning method is as f...

Embodiment 2

[0048] A method for recovering artemisinin from artemisinin recrystallization waste, comprising the following steps:

[0049] a. Primary crystallization: According to the weight ratio, take 60 parts of artemisinin recrystallization waste, heat it in a water bath to 95 ° C to dissolve, add 41 parts of a mixed solution of petroleum ether and ethyl acetate, keep the temperature and stir for 40 minutes, and continue to maintain Stand still at temperature until the solution is separated into layers. At this time, it can be seen that crystals are separated out in the lower layer solution, and then the upper layer solution is separated for subsequent use. Then the lower layer solution is filtered while it is hot, and the filtered crystal is repeatedly washed with a mixed solution of sherwood oil and ethyl acetate for 5 times, get one crystal;

[0050] Wherein, the volume ratio of the mixed solution of petroleum ether and ethyl acetate is 98:33.

[0051] The cleaning method is as fol...

Embodiment 3

[0061] A method for recovering artemisinin from artemisinin recrystallization waste, comprising the following steps:

[0062] a. Primary crystallization: According to the weight ratio, take 37 parts of artemisinin recrystallization waste, heat it in a water bath to 65°C to dissolve, add 18 parts of a mixed solution of petroleum ether and ethyl acetate, keep the temperature and stir for 25 minutes, and continue to keep Stand still at the temperature until the solution is separated into layers. At this time, it can be seen that crystals are separated out in the lower layer solution, and then the upper layer solution is separated for subsequent use. Then the lower layer solution is filtered while hot, and the filtered crystals are washed repeatedly with a mixed solution of sherwood oil and ethyl acetate for 3 times, get one crystal;

[0063] Wherein, the volume ratio of the mixed solution of petroleum ether and ethyl acetate is 95:5.

[0064] The cleaning method is as follows: a...

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Abstract

The invention provides a method for recovering artemisinin from artemisinin recrystallization waste, and concretely relates to the technical field of artemisia carvifolia production. The method crystallizes recrystallization waste twice by using a mixed solution of petroleum ether and ethyl acetate. After the first crystallization, the recrystallization waste is cleaned by using an appropriate mixed solution of petroleum ether and ethyl acetate to improve the purity of an artemisinin first crystal. During the second crystallization, chlorobutanol is added as a crystallization aid, and refrigeration crystallization is combined to increase the amount of artemisinin crystallization precipitation, fully recover the artemisinin in the waste and increase the purity of crude products. Meanwhile,after the crude products obtained by the twice crystallization are dissolved, a mixture of microcrystalline cellulose and activated carbon is added to improve the impurity removal effect and the purity of a fine product. The method of the invention is stable in process, controllable in parameters and simple in steps, can effectively save pharmaceutical costs and improve the utilization rate of theraw materials, can increase the yield of artemisinin by more than 0.5%, and is suitable for large-scale production and popularization.

Description

【Technical field】 [0001] The invention relates to the technical field of artemisinin production, in particular to a method for recovering artemisinin from artemisinin recrystallization waste. 【Background technique】 [0002] Artemisinin is a sesquiterpene lactone drug with peroxy groups extracted from the stems and leaves of the plant Artemisia annua. It can be used for symptom control of vivax malaria and falciparum malaria, as well as for the treatment of chloroquine-resistant strains. It can be used to treat dangerous types of falciparum malaria, such as cerebral type and icteric type, and can also be used to treat systemic lupus erythematosus and discoid lupus erythematosus. [0003] At present, the method of extracting artemisinin from Artemisia annua is mature and has achieved large-scale mass production. The process steps are generally solvent extraction, column elution, and recrystallization. Most of the artemisinin in artemisia, after a large amount of waste liquid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/18C07D493/20
CPCC07B2200/13C07D493/18C07D493/20
Inventor 周源凯黄宗延覃华兴盘玉淑马爱群
Owner GUANGXI XIANCAOTANG PHARMA
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