Simple and new technology for extracting and purifying arteannuin and artemisinic acid from southernwood through single process

A technology of artemisinin and artemisinic acid, applied in the direction of organic chemistry, can solve the problems of flammable and explosive solvents, low extraction recovery rate, complicated process flow, etc., achieve good content and purity, high extraction recovery rate, save The effect of the solvent

Inactive Publication Date: 2013-05-08
ZHANG JIA GANG VINSCE BIO PHARM
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  • Summary
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is reported in the literature that the extraction recovery rate is extremely low, within 10%, and the technological process is very complicated, requiring repeated column chromatography
[0006] The above-mentioned preparation method of artemisinin and its biological and c

Method used

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  • Simple and new technology for extracting and purifying arteannuin and artemisinic acid from southernwood through single process

Examples

Experimental program
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Example Embodiment

[0021] Example 1

[0022] Weigh 500 kg of dried Artemisia annua leaves and put them in a 5-ton extraction tank, add 2.5 tons of industrial ethanol, stir at room temperature (about 25°C) and extract for 4 hours, twice for each batch, and use it for the third time. Filter and combine the extracts, concentrate under reduced pressure to 1 / 4 volume, add 1 ton of petroleum ether to disperse, transfer to the extraction tank, then adjust the pH value to 8 with sodium bicarbonate solution, and add water until the water phase is 1 / 4 of the volume of the organic phase. / 2, 1 ton of petroleum ether extracted twice. Combine the organic phases, concentrate to 1 / 20 volume, dry filter, cool and crystallize, filter to obtain crude artemisinin, wash the crude product with methanol to obtain coarse crystals of artemisinin; use 100% to 20% petroleum ether / ethyl acetate Or eluted with petroleum ether / acetone to obtain crude crystals of artemisinin column chromatography, combined the two kinds of ...

Example Embodiment

[0023] Example 2

[0024] The alkaline aqueous phase obtained above was adjusted to about 6-7 with acetic acid, then extracted twice with 500L of petroleum ether, the organic phase was combined and concentrated to 400L, dried and crystallized to obtain crude artemisinic acid, and then extracted with ethyl acetate Recrystallization obtained 13.5 kg of pure artemisinic acid. HPLC detection content is greater than 99.0%, related substances, simple impurities are less than 0.5%, and total impurities are less than 1%.

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Abstract

The invention relates to a technology for extracting, separating and purifying arteannuin and artemisinic acid from southernwood through a single process. The technology comprises the following steps of: extracting for 4 hours at room temperature twice by adopting a solvent, wherein the volume-mass ratio of the solvent to a material is 4-6; extracting at room temperature for 4 hours twice, wherein extracting solution is repeatedly used when being extracted for the third time; concentrating an obtained extracting solution into liquid extract, then dispersing through organic solvents, such as petroleum ether, and processing and extracting through a sodium bicarbonate solution; concentrating and crystallizing organic phases to obtain a part of crude arteannuin products, and carrying out gradient elution on a crystallizing mother solution through a mixed solvent; concentrating to obtain other arteannuin, and merging to obtain qualified pure arteannuin products through ethanol recrystallization; regulating the pH value of a water phase part obtained from the last step through acid water to 6-7; and extracting through the solvents, such as the petroleum ether, and concentrating, drying, crystallizing and recrystallizing to obtain pure artemisinic acid products. The process disclosed by the invention has the advantages of simple and high-efficiency process flow, high recovery rate, high product content and purity and high operation feasibility, and is suitable for mass production.

Description

technical field [0001] The invention relates to a single-process preparation method for artemisinin and artemisinin, in particular to a simple new process for simultaneously obtaining high-purity artemisinin and artemisinic acid through simple solvent extraction, separation and purification using artemisia annua as a raw material. Background technique [0002] Artemisia annua, also known as Artemisia annua, Artemisia annua, and Artemisia annua, contains many active ingredients as a traditional Chinese medicine, including artemisinin, artemisinic acid, artemisinin, artemisinin, artemisinin, dehydrogenation Artemisinin, coumarin, flavonoids, stigmasterol and Artemisia annua volatile oil and so on. In traditional Chinese medicine, the aerial part of Artemisia annua is used to treat malaria, fever caused by tuberculosis, jaundice, heat-heat fever, and afternoon fever due to yin deficiency (World Health Organization Monograph: Quality Management Practice for Planting and Harvesti...

Claims

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Application Information

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IPC IPC(8): C07D493/20
Inventor 彭学东张梅赵金召闫勇义
Owner ZHANG JIA GANG VINSCE BIO PHARM
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