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Method for simultaneously extracting arteannuic acid and dihydroarteannuic acid from liquid waste after separation of artemisinin

A technology of dihydroartemisinic acid and artemisinic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of unfavorable industrial production, low separation efficiency, complicated operation, etc., and achieve strong implementability, High extraction efficiency and improved separation efficiency

Active Publication Date: 2014-01-22
GUANGZHOU HONSEA SUNSHINE BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, the existing methods for extracting and separating artemisinic acid and dihydroartemisinic acid from Artemisia annua plants have many problems such as low separation efficiency, small processing capacity, complicated operation, and high cost, which are not conducive to the realization of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Send 100 kg of Artemisia annua waste liquid with 3.10% and 4.02% content of artemisinic acid and dihydroartemisinic acid respectively to a molecular still, and control the reaction conditions as follows: temperature 120~160°C, pressure 30~100 Pa , For example, the temperature is 150°C, the pressure is 50 Pa, and the heavy phase and the light phase are obtained after continuous distillation; the heavy phase is sent to the molecular still again, and the reaction conditions are controlled as follows: the temperature is 150~200°C, the pressure is 1~10 Pa, for example The temperature was 180°C, the pressure was 1 Pa, and secondary distillation was carried out to obtain 19.7 kg of an oily product with a content of artemisinic acid of 14.56% and a content of dihydroartemisinic acid of 19.31%. The yield of artemisinic acid was 92.53%. The yield of artemisinic acid was 94.63%.

[0027] (2) Add petroleum ether (60~90°C) to the oily product obtained in step (1), extract twice ...

Embodiment 2

[0032](1) Send 100 kg of Artemisia annua waste liquid with 3.10% and 4.02% content of artemisinic acid and dihydroartemisinic acid respectively to a molecular still, control the temperature at 140°C, and the pressure at 45 Pa. After continuous distillation, the heavy phase and Light phase; send the heavy phase to the molecular still again, control the temperature at 185°C and the pressure at 5 Pa, and carry out secondary distillation to obtain an oily product with a content of artemisinic acid of 13.44% and a content of dihydroartemisinic acid of 17.98%. 20.82kg, the yield of artemisinic acid was 90.26%, and the yield of dihydroartemisinic acid was 93.12%.

[0033] (2) Add petroleum ether (60~90°C) to the oily product obtained in step (1), extract twice at 50°C, the amount of petroleum ether added is 60, 60L respectively, separate and combine the petroleum ether layer, and discard the insoluble matter .

[0034] (3) Add 2% sodium hydroxide solution (or potassium hydroxide sol...

Embodiment 3

[0038] (1) Send 100kg of Artemisia annua waste liquid with 3.10% and 4.02% content of artemisinic acid and dihydroartemisinic acid to molecular still, control the temperature at 155°C and pressure at 55 Pa, and obtain the heavy phase and The light phase; send the heavy phase to the molecular still again, control the temperature at 175°C, and the pressure at 1 Pa, and carry out secondary distillation to obtain an oily product with a content of artemisinic acid of 13.95% and a content of dihydroartemisinic acid of 18.47%. 20.29kg, the yield of artemisinic acid was 91.30%, and the yield of dihydroartemisinic acid was 93.22%.

[0039] (2) Add petroleum ether (60~90°C) to the oily product obtained in step (1), extract twice at 50°C, the amount of petroleum ether added is 60, 60L respectively, separate and combine the petroleum ether layer, and discard the insoluble matter .

[0040] (3) Add 5% potassium bicarbonate solution to the petroleum ether solution obtained in step (2) to e...

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Abstract

The invention discloses a method for simultaneously extracting arteannuic acid and dihydroarteannuic acid from liquid waste after separation of artemisinin. The method disclosed by the invention comprises the following steps: firstly, initially enriching arteannuic acid and dihydroarteannuic acid in artemisia apiacea liquid water by adopting a molecular distillation technology; then, further separating a molecular distillation product by adopting a solvent extraction method and an acid-alkali method to obtain an oily crude product; and finally, carrying out clathration on the oily crude product through urea to remove part of saturated and monounsaturated fatty acid, and repeatedly crystallizing to obtain mixed crystals of arteannuic acid and dihydroarteannuic acid with the total content which is not lower than 95%. Compared with the prior art, the method disclosed by the invention has the characteristics of high extraction efficiency, environment-friendliness, relatively low cost, strong implementability and applicability to industrial production.

Description

technical field [0001] The invention relates to a method for simultaneously extracting artemisinic acid and dihydroartemisinic acid from waste liquid after separation of artemisinin. technical background [0002] Artemisinin is a new type of sesquiterpene lactone antimalarial drug containing a peroxide bridge discovered by Chinese scientists in 1973 from the leaves and buds of the traditional Chinese medicine Artemisia annua, which is the plant Artemisia annua. Features. At present, it has been used as the drug of choice for the treatment of malaria, and its curative effect has been widely recognized all over the world. The content of artemisinin in Artemisia annua plants is low, much lower than that of its biosynthetic precursors, artemisinic acid and dihydroartemisinic acid. If certain technical means can be used to extract and separate artemisinic acid and dihydroartemisinic acid from the waste liquid after separation of artemisinin, and use them as raw materials for se...

Claims

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Application Information

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IPC IPC(8): C07D493/20C07C57/26C07C51/42
CPCC07C51/42C07C2602/28C07D493/20C07C57/26
Inventor 吕雪斌雷海军易宇阳罗安东
Owner GUANGZHOU HONSEA SUNSHINE BIOTECH CO LTD
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