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Method for selectively extracting and separating artemisinin/artemisitene by using hydrophilic ionic liquid

An ionic liquid, artemisinin technology, applied in organic chemistry and other directions, can solve the problems of long time and complicated operation, and achieve the effect of simple operation and reduced dosage

Active Publication Date: 2021-11-02
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN107746407 A discloses a method for reducing artemisinin in artemisinin, first prepare the petroleum ether extract of Artemisia annua, and make it flow through a silica gel column, After that, the silica gel column is eluted with a mixture of petroleum ether and ethyl acetate, and finally the eluate is crystallized and recrystallized to achieve the purpose of separating artemisinin and artemisinin, which can reduce the content of artemisinin to 0.93-1.96%. , but the process is complex and time-consuming, so it is necessary to develop new methods to obtain high-quality artemisinin

Method used

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  • Method for selectively extracting and separating artemisinin/artemisitene by using hydrophilic ionic liquid
  • Method for selectively extracting and separating artemisinin/artemisitene by using hydrophilic ionic liquid
  • Method for selectively extracting and separating artemisinin/artemisitene by using hydrophilic ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Mix an equal volume of 5% allyltrimethylammonium chloride aqueous solution (mole fraction) with a cyclohexane solution containing artemisinin / artemisinin (artemisinin content 4.9%), shake at 50°C for 5h , Stand at 50°C for 4h, and separate the layers to obtain a two-phase solution.

[0024] 2) Take 0.5 mL each of the extract phase (ionic liquid phase) and the raffinate phase (organic solvent phase) with a syringe, dilute to 5 mL with methanol, and determine artemisinin and artemisinin in the two phases by high performance liquid chromatography. concentration, the calculated separation selectivity is 6.45.

Embodiment 2

[0026] 1) Mix equal volumes of 5% triethylamine hydrochloride aqueous solution (mole fraction) and cyclohexane solution containing artemisinin / artemisinin (artemisinin content 4.9%), shake at 50°C for 5h, and 50°C After standing for 4h, the layers were separated to obtain a two-phase solution.

[0027] 2) Take 0.5 mL each of the extract phase (ionic liquid phase) and the raffinate phase (organic solvent phase) with a syringe, dilute to 5 mL with methanol, and determine artemisinin and artemisinin in the two phases by high performance liquid chromatography. concentration, the calculated separation selectivity was 5.97.

Embodiment 3

[0029] 1) Mix equal volumes of 5% allyltrimethylammonium chloride aqueous solution (mole fraction) with cyclohexane solution containing artemisinin / artemisinin (artemisinin content 5%), shake at 50°C for 0.5 h, stand at 50°C for 4h, and separate the layers to obtain a two-phase solution.

[0030] 2) Take 0.5 mL each of the extract phase (ionic liquid phase) and the raffinate phase (organic solvent phase) with a syringe, dilute to 5 mL with methanol, and determine artemisinin and artemisinin in the two phases by high performance liquid chromatography. concentration, the calculated separation selectivity was 4.67.

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Abstract

The invention relates to a method for selectively extracting and separating artemisinin / artemisitene by using a hydrophilic ionic liquid, which comprises the following steps: mixing an aqueous solution of an ionic liquid and an organic solvent solution of artemisinin / artemisitene, oscillating at constant temperature, standing, respectively taking an ionic liquid phase and an organic solvent phase, fixing the volume by using methanol, and detecting the concentration of artemisinin and artemisinene in the raffinate phase (organic solvent phase) and the extract phase (ionic liquid phase) to obtain separation selectivity. The ionic liquid aqueous solution can highly selectively extract artemisitene from the artemisinin crude product, and then the raffinate phase is directly cooled and crystallized to obtain the artemisinin product. The method is suitable for removing low-content artemisitene, is simple to operate, is green, and can realize high-selectivity separation of artemisinin / artemisitene.

Description

technical field [0001] The invention relates to the field of purification and separation of natural products, in particular to a method for selectively extracting and separating artemisinin / artemisinin with a hydrophilic ionic liquid. Background technique [0002] Artemisinin is the most effective antimalarial drug recognized by the World Health Organization. It also has pharmacological activities such as antiparasitic, antifungal, anti-inflammatory, anticancer, and treatment of lupus erythematosus. It is mainly derived from Artemisia annua. This natural plant contains hundreds of components, including artemisinin, artemether, dihydroartemisinin, deoxyartemisinin and other substances that are very similar in structure to artemisinin. [0003] The industry mainly adopts column chromatography-recrystallization purification to obtain artemisinin products, but studies have shown that it is difficult to effectively remove artemisinin with existing technologies. The structures of...

Claims

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Application Information

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IPC IPC(8): C07D493/20
CPCC07D493/20Y02P20/54
Inventor 王慧曹莹莹祝艺伟陈柄彤张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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