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Method used for extracting dihydroartemisinic acid from artemisia apiacea wax oil

A technology of dihydroartemisinic acid and wax oil, applied in organic chemical methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of incomplete crystallization, difficult refining, difficult crystallization, etc., and achieve low production cost , Saving raw material resources, reducing the effect of usage

Pending Publication Date: 2019-08-09
湖南威嘉生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the problems of difficult crystallization, low yield and difficult refining caused by incomplete crystallization in the prior art, and to provide a kind of artemisinin wax oil that can be effectively obtained from the by-product artemisinin production process. Separation, extraction, concentration and purification of high-quality dihydroartemisinic acid, which improves the conversion efficiency of artemisinin from Artemisia annua, saves the raw material resources of Artemisia annua, and reduces the environmental pollution caused by wastes in the production process of artemisinin. Method for extracting dihydroartemisinic acid in plain wax oil

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] This embodiment includes the following steps:

[0029] (1) Extraction and filtration: add 100kg of artemisia wax oil, 2000L of 70% methanol water and 10kg of caustic soda into a stirring tank for stirring, extract at room temperature for 4 hours, let stand until the solution is separated, take the supernatant and filter to obtain wax Oil extract, the extract was centrifugally filtered to obtain a clarified wax oil extract; the operation was repeated 4 times, and 5 batches of extract 9600L were collected;

[0030] (2) Chromatographic column: Pass the wax oil extract obtained in step (1) through a 500kg DX-7 resin column (produced by Xi'an Lanxiao Resin Factory), collect the effluent after loading the column, and obtain 10100L of chromatographic column collected liquid;

[0031] (3) Extraction and removal of impurities from the concentrated liquid: Concentrate the liquid collected from the chromatographic column obtained in step (2) to 1500L, add 3000L petroleum ether or ...

Embodiment 2

[0038] This embodiment includes the following steps:

[0039] (1) Extraction and filtration: add 100kg of artemisia wax oil, 1800L of 70% methanol water and 10kg of caustic soda into a stirring tank for stirring, extract at room temperature for 4 hours, let stand until the solution is separated, take the supernatant and filter to obtain wax Oil extract, the extract was centrifugally filtered to obtain a clarified wax oil extract; the operation was repeated 4 times, and 5 batches of extract 9500L were collected;

[0040] (2) Chromatographic column: Pass the wax oil extract obtained in step (1) through a 500kg DX-7 resin column (produced by Xi'an Lanxiao Resin Factory), collect the effluent after loading the column, and obtain 9900L of chromatographic column collected liquid;

[0041] (3) Extraction and removal of impurities from the concentrated liquid: Concentrate the liquid collected from the chromatographic column obtained in step (2) to 1500L, add 3000L petroleum ether or i...

Embodiment 3

[0048] This embodiment includes the following steps:

[0049] (1) Extraction and filtration: add 100kg Artemisia annua wax oil, 2000L 70% methanol water and 10kg caustic soda into a stirring tank for stirring, extract at room temperature for 12 hours, let stand until the solution is separated, take the supernatant and filter to obtain wax Oil extract, the extract was centrifugally filtered to obtain a clarified wax oil extract; the operation was repeated 4 times, and a total of 5 batches of extract were collected, totaling 9700L;

[0050] (2) Chromatographic column: Pass the wax oil extract obtained in step (1) through a 500kg DX-7 resin column (produced by Xi'an Lanxiao Resin Factory), collect the effluent after loading the column, and obtain 10100L of chromatographic column collected liquid;

[0051] (3) Extraction and removal of impurities from the concentrated liquid: Concentrate the liquid collected from the chromatographic column obtained in step (2) to 1500L, add 3000L ...

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Abstract

The invention discloses a method used for extracting dihydroartemisinic acid from artemisia apiacea wax oil. The method comprises following steps: 1, extracting filtering; 2, chromatography column processing; 3, extracting and impurity removing; 4, condensation and acid adjusting; 5, extraction and condensation; 6, crystallization pumping filtration; and 7, crude product refining. According to themethod, dihydroartemisinic acid is extracted and separated from artemisinin production by-product artemisia apiacea wax oil, chromatography is adopted to remove terpenes which possess structures similar to that of dihydroartemisinic acid and are not removed through saponification, and then condensation, extraction, and purification are carried out to produce the high quality dihydroartemisinic acid with a purity of 99% or higher. The method is capable of changing waste into valuables, increasing conversion efficiency of artemisinin from artemisia apiacea, saving artemisia annua raw material resource, reducing organic solving using amount, reducing pollution of artemisinin production process on the environment, and promoting artemisia annua resource comprehensive development and utilization.

Description

technical field [0001] The invention relates to a method for extracting dihydroartemisinic acid, in particular to a method for extracting dihydroartemisinic acid from artemisinin wax oil. Background technique [0002] Artemisinin (Arteannuin) is a compound containing peroxo-sesquiterpene lactones extracted from Artemisia annua, a traditional Chinese medicine. It is an antimalarial drug with high efficiency and low toxicity. Although artemisinin is very effective against multidrug-resistant malaria parasites, the planting period of Artemisia annua is long, the extraction process is complicated, the output is limited, and the supply is insufficient. Most malaria patients cannot afford the market price. In addition to artemisinin, Artemisia annua contains other sesquiterpenes, such as artemisinin G, artemisinin, artemisinin B, artemisinin, artemisinin, artemisinin , epi-deoxyartemisinin, artenimol, methyl artemisinate, artemisinic acid, 6,7-dehydroartemisinic acid, dihydroarte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/43C07C51/47C07C51/48C07C57/26
CPCC07B2200/13C07C51/42C07C51/43C07C51/47C07C51/48C07C2602/10C07C57/26
Inventor 刘小波易静云
Owner 湖南威嘉生物科技有限公司
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