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Artemisinin and preparation method thereof

A technology of artemisinin and Artemisia annua, applied in the direction of organic chemistry, can solve the problems of not meeting the requirements of artemisinin production, difficult release of artemisinin solution, low yield of silica gel column chromatography, etc., and achieve market application The effect of broad prospects, improved extraction rate, and 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] Artemisinin is a colorless needle-like crystal with a bitter taste, and is easily soluble in acetone, ethyl acetate, chloroform, benzene, petroleum ether and other weakly polar organic solvents, so artemisinin is generally extracted from Artemisia annua. These organic solvents are used as extractants, but the main components of Artemisia annua are highly polar and hydrophilic substances such as cellulose and pectin, and these solvents have poor penetration to strong polar and hydrophilic substances. Artemisinin is wrapped by plant cell tissue with cellulose and pectin as the main components, so these solvents have great mass transfer resistance during the extraction process, and it is difficult for the solvent to pass through the plant cell tissue to dissolve artemisinin. The solution of artemisinin is also difficult to release, the extraction time is long and the efficiency is low, and the residual rate of artemisinin is often high
[0004] On the other hand, due to the low content of artemisinin in Artemisia annua, a large amount of impurities are brought along during the extraction process, so purification is required. At this stage, the purification process mainly uses silica gel column chromatography, but silica gel column chromatography has The shortcomings of low yield and high cost, therefore, the existing technology can not meet the requirements of artemisinin production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Treatment of the raw medicinal material: the raw medicinal material Artemisia annua was dried and crushed to 25 meshes.

[0017] (2) Extraction of artemisinin: The material was refluxed twice with ethyl acetate as the solvent, the volume-to-mass ratio of the solvent to the material was 3:1, and the extraction time was 4.5 hours. The two extracts were combined and concentrated. For standby, the unit of volume in the volume-to-mass ratio is milliliters, and the unit of mass is grams. During the extraction process, the extraction tank is vacuumed and broken intermittently, and vacuum pulses are used to enhance mass transfer.

[0018] (3) Purification of artemisinin: Adsorb the concentrated artemisinin extract with medium-polarity macroporous adsorption resin, then elute with 91% ethanol, and the eluate is concentrated, crystallized and 60% ethanol After recrystallization and drying, the artemisinin product is obtained, and the mass fraction of artemisinin in the produc...

Embodiment 2

[0021] (1) Treatment of the raw medicinal material: the raw medicinal material Artemisia annua was dried and crushed to 40 mesh.

[0022] (2) Extraction of artemisinin: The material was refluxed twice with ethyl acetate as the solvent, the volume-to-mass ratio of the solvent to the material was 6:1, the extraction time was 3 hours, the two extracts were combined and concentrated, For standby, the unit of volume in the volume-to-mass ratio is milliliters, and the unit of mass is grams. During the extraction process, the extraction tank is vacuumed and broken intermittently, and vacuum pulses are used to enhance mass transfer.

[0023] (3) Purification of artemisinin: Adsorb the concentrated artemisinin extract with a medium-polarity macroporous adsorption resin, then elute with 95% ethanol, and the eluate is concentrated, crystallized and mixed with 75% ethanol After recrystallization and drying, the artemisinin product is obtained, and the mass fraction of artemisinin in the p...

Embodiment 3

[0026] (1) Treatment of the raw medicinal material: the raw medicinal material Artemisia annua was dried and crushed to 70 mesh.

[0027] (2) Extraction of artemisinin: The material was refluxed twice with ethyl acetate as the solvent, the volume-to-mass ratio of the solvent to the material was 10:1, and the extraction time was 1.5 hours. The two extracts were combined and concentrated. For standby, the unit of volume in the volume-to-mass ratio is milliliters, and the unit of mass is grams. During the extraction process, the extraction tank is vacuumed and broken intermittently, and vacuum pulses are used to enhance mass transfer.

[0028] (3) Purification of artemisinin: Adsorb the concentrated artemisinin extract with medium-polarity macroporous adsorption resin, then elute with 99% ethanol, and the eluate is concentrated, crystallized and 88% ethanol After recrystallization and drying, the artemisinin product is obtained, and the mass fraction of artemisinin in the product...

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Abstract

The invention discloses a preparation method for artemisinin. The method comprises the following steps: (1) drying and smashing artemisia apiacea as a medical raw material into powder of 20-80 meshes; (2) performing reflux extraction twice on the material, combing extracting solutions generated from the two reflux extractions and concentrating for standby, wherein ethyl acetate is used as a solvent, and intermittent vacuumizing and vacuum breaking are performed on an extracting tank during extracting process; (3) adsorbing a concentrated artemisinin extracting solution by using macroporous resin with moderate polarity, eluting the concentrated artemisinin extracting solution by using 90-99.7% of alcohol, concentrating and crystallizing an eluate, recrystallizing with 50-90% of alcohol, and drying to obtain an artemisinin product. According to the invention, through the combination between pulsating vacuum extraction and adsorption of macroporous resin, the production with low cost and high efficiency for preparing the artemisinin from the artemisia apiacea is realized and the market application prospect is wide.

Description

technical field [0001] The invention relates to a preparation method of artemisinin, in particular to a method for extracting and purifying 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, on the basis of which a variety of derivatives have been synthesized, such as dihydroartemisinin, artemether, artemisia annua Artemisinin drugs have very important medicinal value due to their low toxicity and strong anti-masochistic properties. [0003] Artemisinin is a colorless needle-like crystal with a bitter taste, and is easily soluble in acetone, ethyl acetate, chloroform, benzene, petroleum ether and other weakly polar organic solvents, so artemisinin is generally extracted from Artemisia annua. These organic solvents are used as extractants, but the main components of Artemisia annua are highly ...

Claims

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Application Information

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IPC IPC(8): C07D493/20
CPCC07D493/20
Inventor 田宏现
Owner JISHOU UNIVERSITY
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