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Method for separating and purifying high-purity artemisinic acid

A technology for separation and purification of artemisinic acid, applied in the field of separation and purification of high-purity artemisinic acid, which can solve the problems of large amount of organic solvent usage, complicated operation, and low separation efficiency, and achieve easy control of production conditions, simple process steps, and high purity high effect

Active Publication Date: 2016-03-23
CHONGQING QIANTAI BIOLOGICAL MEDICINE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN102702220A Extract artemisinic acid from artemisinin mother liquor, adopt five steps of saponification, acidification, extraction, dry column chromatography, and refining to separate and purify high-content artemisinic acid, which requires organic solvent for recrystallization, Complicated operation and long crystallization time
And these methods have all adopted column chromatography to deal with at last, the column chromatography separation of large batches, the use amount of organic solvent is large, brings serious environmental pollution and potential safety hazard, and has improved production cost, is unfavorable for industrialized production
CN103467274A discloses a method for extracting artemisinic acid from Artemisia annua, including using CO 2 Supercritical extraction, the extract is decolorized with activated carbon, after concentration, recrystallized from anhydrous methanol, the cost is high, and it is not suitable for industrial production
CN103570739A and CN103524527A also disclose methods for separating and extracting artemisinin from artemisinin waste liquid or artemisinin essential oil, both of which involve the use of organic solvents for recrystallization, the use of organic solvents is large, the environment is not friendly, and the production cost is high
[0010] In summary, the existing methods for extracting and purifying artemisinic acid have problems such as low separation efficiency, complex operation, high cost, and unsuitability for industrial production.

Method used

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  • Method for separating and purifying high-purity artemisinic acid
  • Method for separating and purifying high-purity artemisinic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0045] 6 L of fermentation broth was suction filtered to obtain 1 kg of wet mycelia. The mycelium was dried at 50° C. for 12 hours to obtain 430 g of dry mycelium. Add 1.6 L of butyl acetate to the dried mycelium, and stir for 5 hours. Suction filtration to collect the butyl acetate layer. 1.6 L of a pH 8 aqueous solution of sodium bicarbonate was added. After stirring for 30 minutes, the layers were separated, and the butyl acetate layer was collected. The butyl acetate layer was concentrated at 70°C until the concentration of artemisinic acid was 150g / L, and the volume was about 400ml. Add 400ml of water to the butyl acetate layer, heat the feed solution to 75°C, add 30% sodium hydroxide solution dropwise with stirring, and adjust the pH to 11.5. After cooling to room temperature, the layers were separated and the aqueous layer was collected. The aqueous layer was heated to 70°C. Add 10% sulfuric acid under stirring to adjust the pH to 5.5. Slowly lower the temperatur...

Embodiment 2

[0047] 34L of the fermentation broth was suction filtered to obtain 3.6kg of wet mycelium. The mycelium was dried at 50° C. for 12 hours to obtain 2.1 kg of dry mycelium. Add 8.4 L of methyl isobutyl ketone to the dry mycelium, and stir for 5 hours. Suction filtration to collect the methyl isobutyl ketone layer. 8.4 L of a pH 9 aqueous solution of sodium carbonate was added. After stirring for 30 minutes, the layers were separated, and the methyl isobutyl ketone layer was collected. The methyl isobutyl ketone layer was concentrated at 70°C until the concentration of artemisinic acid was about 150g / L, and the volume was about 2.3L. Add 2.3 L of water to the methyl isobutyl ketone layer, heat the feed solution to 75°C, add 20% potassium hydroxide solution dropwise with stirring, and adjust the pH to 13. After cooling to room temperature, the layers were separated and the aqueous layer was collected. The aqueous layer was heated to 70°C. 10% hydrochloric acid was added unde...

Embodiment 3

[0049] 36L of the fermentation broth was suction-filtered to obtain 3.6kg of mycelia. The mycelium was dried overnight at 50° C. to obtain dry mycelium. Add 8.4 L of methyl isobutyl ketone to the dry mycelium, and stir for 5 hours. Suction filtration to collect the methyl isobutyl ketone layer. 8.4 L of a pH 8 aqueous solution of sodium bicarbonate was added. After stirring for 30 minutes, the layers were separated, and the methyl isobutyl ketone layer was collected. The methyl isobutyl ketone layer was concentrated at 75°C until the concentration of artemisinic acid was about 150g / L, and the volume was about 2L. Add 2L of pure water to the methyl isobutyl ketone layer, heat the feed solution to 75°C, add 30% sodium hydroxide solution dropwise with stirring, and adjust the pH to 11.5. After cooling to room temperature, the layers were separated and the aqueous layer was collected. The aqueous layer was heated to 70°C. Add 10% sulfuric acid under stirring to adjust the pH...

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Abstract

The present invention relates to a method for separating high-purity artemisinic acid from a yeast cell fermentation liquid and purifying, particularly separating the artemisinic acid from the fermentation liquid and purifying by using an extraction-crystallization method. The method needs no column chromatography, the process is simple, the production conditions are easy to control and the method is suitable for large-scale industrial production. The method provided by the present invention crystallizes by adjusting the pH by taking water as a solvent, and is low in cost and environmental-friendly. Moreover, the artemisinic acid obtained by the method is high in purity.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, and further relates to a method for separating and purifying high-purity artemisinic acid from brewer's cells. Background technique [0002] In the 1970s, Chinese scientists first isolated artemisinin from the traditional Chinese medicine Artemisia annua (Artemisia annua L.), which is a sesquiterpene lactone compound containing an oxygen bridge. It was discovered in China. The first natural medicine to be recognized internationally. Artemisinin not only has a significant therapeutic effect on malaria that is resistant to a variety of malaria drugs that are resistant to antimalarial drugs such as chloroquine, mefloquine, and antipyrimethamine, but also has a good therapeutic effect on hepatitis, Inhibition of tumor cell growth, killing schistosomiasis and other effects. [0003] At present, artemisinin is mainly obtained in the following ways: [0004] 1. It is isolated from the leaves and fl...

Claims

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Application Information

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IPC IPC(8): C07C57/26C07C51/42
Inventor 唐恒郭明杨久林徐星灿袁建栋
Owner CHONGQING QIANTAI BIOLOGICAL MEDICINE
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