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Extraction and separation method for artemisinin

A separation method, the technology of artemisinin, applied in the direction of organic chemistry, etc., can solve the problems that cannot meet the requirements of artemisinin extraction and separation, the solution of artemisinin is difficult to release, tailing and elution are not complete, etc., to achieve Reduced equipment requirements, shortened extraction time, and the effect of shortened extraction time

Inactive Publication Date: 2014-03-26
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There have been many reports on the extraction and separation of artemisinin from Artemisia annua. Since Artemisia annua is easily soluble in non-polar organic solvents such as petroleum ether, the existing artemisinin production processes generally use non-polar organic solvents such as petroleum ether. Polar organic solvents are used for extraction, but non-polar solvents have poor penetration to hydrophilic substances such as cellulose and pectin, and artemisinin is wrapped in plant cell tissues with cellulose and pectin as the main components Therefore, there is a large mass transfer resistance in the extraction process with non-polar solvents such as petroleum ether. It is difficult for the solvent to pass through the plant cell tissue to dissolve artemisinin, and it is also difficult to release the solution dissolved in artemisinin. Extraction Long time and low efficiency
[0004] In order to overcome the influence of mass transfer resistance, new extraction processes such as countercurrent extraction and ultrasonic extraction have been developed, but the equipment required for these processes is very demanding and expensive; on the other hand, silica gel column chromatography is used in the separation process of artemisinin. There are also problems of tailing and incomplete elution during elution. Therefore, the existing technology cannot meet the requirements of artemisinin extraction and separation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Treatment of raw medicinal materials: dry and pulverize raw medicinal materials Artemisia annua.

[0017] (2) Extraction of artemisinin: use solvent gasoline as a solvent to reflux extract the material twice, the volume-to-mass ratio of the solvent to the material during extraction is 3:1, and the extraction time is 4.5 hours. The two extracts are combined and concentrated for later use. , During the extraction process, the extraction tank is intermittently vacuumed and broken.

[0018] (3) Separation of artemisinin: The concentrated artemisinin extract was subjected to silica gel column chromatography, and then eluted with a mixture of n-hexane and ether. The elution process was assisted by ultrasonic waves. The eluent was concentrated, After decolorization, drying and crystallization, the artemisinin product with improved purity is obtained, and the mass fraction of artemisinin in the product is 98.3%.

Embodiment 2

[0020] (1) Treatment of raw medicinal materials: dry and pulverize raw medicinal materials Artemisia annua.

[0021] (2) Extraction of artemisinin: use petroleum ether as a solvent to reflux the material twice, the volume-to-mass ratio of the solvent to the material during extraction is 13:1, and the extraction time is 1.5 hours. The two extracts are combined and concentrated for later use. , During the extraction process, the extraction tank is intermittently vacuumed and broken.

[0022] (3) Separation of artemisinin: The concentrated artemisinin extract was subjected to silica gel column chromatography, and then eluted with a mixture of n-hexane and ether. The elution process was assisted by ultrasonic waves. The eluent was concentrated, After decolorization, drying and crystallization, the artemisinin product with improved purity is obtained, and the mass fraction of artemisinin in the product is 98.9%.

Embodiment 3

[0024] (1) Treatment of raw medicinal materials: dry and pulverize raw medicinal materials Artemisia annua.

[0025] (2) Extraction of artemisinin: The mixture of petroleum ether and solvent gasoline was used as the solvent to reflux the material for two extractions. The volume-to-mass ratio of the solvent to the material during extraction was 7:1, and the extraction time was 8.5 hours. The two extractions were combined The liquid is concentrated and set aside for use. During the extraction process, the extraction tank is intermittently vacuumed and broken.

[0026] (3) Separation of artemisinin: The concentrated artemisinin extract was subjected to silica gel column chromatography, and then eluted with a mixture of n-hexane and ether. The elution process was assisted by ultrasonic waves. The eluent was concentrated, After decolorization, drying and crystallization, the artemisinin product with improved purity is obtained, and the mass fraction of artemisinin in the product is...

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Abstract

The invention discloses an extraction and separation method for artemisinin. The extraction and separation method comprises the following steps: (1) grinding abrotani herba serving as a raw medicinal material after the artemisinin is dried; (2) performing backflow extraction on the material by petroleum ether or solvent gasoline or a mixture of the petroleum ether and the solvent gasoline, which serves as a solvent, twice for 1-10 hours according to that the volume-mass ratio of the solvent to the material is (2:1)-(15:1), intermittently vacuumizing an extraction pot and breaking vacuum in an extraction process, and combining and concentrating extracting solutions of the two times for later use; (3) performing silica gel column chromatography on the concentrated artemisinin extracting solution, then eluting the artemisinin extracting solution through a normal hexane and diethyl ether mixture, and concentrating, decoloring, drying and crystallizing an eluant to obtain the artemisinin. According to the extraction separation method for the artemisinin, vacuum pulse type extraction and ultrasonic auxiliary elution are organically combined, so that low cost and high efficiency for extracting the artemisinin from the abrotani herba are achieved, and the application prospect is wide.

Description

technical field [0001] The invention relates to a method for extracting and separating artemisinin, in particular to a method for extracting and separating artemisinin from Chinese medicinal material Artemisia annua. Background technique [0002] Artemisinin is a new sesquiterpene lactone antimalarial drug with peroxy groups extracted from the traditional Chinese medicine Artemisia annua. It is also the first internationally recognized natural drug discovered in China. Various derivatives have been synthesized on the basis of it , such as dihydroartemisinin, artemether, artesunate, etc. Artemisinin drugs have low toxicity and strong anti-masochistic properties, and have been approved by the WTO as the first choice for the treatment of cerebral malaria and falciparum malaria worldwide. [0003] There have been many reports on the extraction and separation of artemisinin from Artemisia annua. Since Artemisia annua is easily soluble in non-polar organic solvents such as petrol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20
CPCC07D493/20
Inventor 李志平
Owner JISHOU UNIVERSITY
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