Method for purifying cheliensisin A

A technology of carnation and fragrant leaves, which is applied in the field of supercritical CO2 extraction and high-speed countercurrent chromatography to purify Jinghong gonacarin, which can solve the problems of low extraction efficiency and yield, environmental pollution, etc., and achieve a large amount of preparation , short extraction time and high efficiency

Inactive Publication Date: 2012-01-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this traditional process has relatively low extraction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take Jinghonggena fragrant leaf medicinal material, crush 60 mesh, take 500g of raw material and add supercritical CO 2 In the extraction kettle, turn on the equipment and adjust the parameters: the extraction temperature is 50°C, the extraction pressure is 25MPa, the temperature of the separation kettle I is 55°C, and the pressure is 10MPa, the temperature of the separation kettle II is 45°C, and the pressure is 5MPa. After reaching the above parameters, extract at a flow rate of 20L / h for 4h, and analyze the extract. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 3:3:5:4. The following phase is the stationary phase, and the upper phase is the mobile phase. Turn on the high-speed countercurrent chromatograph, and inject the dissolved extract of ethyl acetate into the Chromatograph, adjust rotating speed 900r / min, flow velocity 2ml / min, separate to obtain jinghongfen, collect jinghong, and dry it under reduced pressure to obtain jinghong, ...

Embodiment 2

[0017] Take Jinghong Gona fragrant leaf medicinal material, crush 60 mesh, take 500g raw material and add CO 2 In the extraction kettle, turn on the equipment and adjust the parameters: the extraction temperature is 50°C, the extraction pressure is 20MPa, the temperature of the separation kettle I is 50°C, and the pressure is 8MPa, the temperature of the separation kettle II is 45°C, and the pressure is 6MPa. After reaching the above parameters, extract at a flow rate of 30L / h for 2h and collect the extract. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 3:5:4:4. The following phase is the stationary phase, and the upper phase is the mobile phase. Turn on the high-speed countercurrent chromatograph, and inject the dissolved extract of ethyl acetate into the Chromatograph, adjust rotating speed 850r / min, flow velocity 2ml / min, separate jinghongcona, collect jinghongzheng fraction, dry under reduced pressure to get jinghongcona 671mg, high performa...

Embodiment 3

[0019] Take Jinghong Gona fragrant leaf medicinal material, crush 80 mesh, take 1kg of raw material and add CO 2 In the extraction kettle, turn on the equipment and adjust the parameters: the extraction temperature is 55°C, the extraction pressure is 22MPa, the temperature of the separation kettle I is 50°C, and the pressure is 8MPa, the temperature of the separation kettle II is 45°C, and the pressure is 6MPa. After reaching the above parameters, extract at a flow rate of 30L / h for 2h and collect the extract. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 3:4:5:4. The following phase is the stationary phase, and the upper phase is the mobile phase. Turn on the high-speed countercurrent chromatograph, and inject the ethyl acetate-dissolved extract into the chromatogram. Apparatus, adjust the rotating speed 850r / min, flow rate 2ml / min, separate jinghongcona, collect jinghongcona fraction, dry under reduced pressure to get jinghongcona 1.31g, high ...

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PUM

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Abstract

The invention provides a method for purifying cheliensisin A. The method is characterized by comprising the following steps: taking leaves of goniothalamus cheliensis as raw materials, grinding the leaves to 60-80 meshes, adding the ground leaves to an extraction kettle, extracting the leaves by adopting supercritical CO2, collecting the extracts, adopting a high-speed counter-current chromatography for separation and drying stream under reduced pressure by taking n-hexane-ethyl acetate-methanol-water as a solvent system, thus obtaining cheliensisin A. The method has the advantages of high efficiency, environment friendliness and the like.

Description

technical field [0001] The present invention relates to a kind of method of purifying Jinghong cornagarin, in particular to a method of using supercritical CO 2 Methods of extraction and high-speed countercurrent chromatography purification of Jinghong genarin. Background technique [0002] Jinghong Cheliensisin A, chemical name 6(7,8-epoxy-styryl)-5-acetoxy-5,6-dihydro-2-pyrone, molecular weight 274, White crystal, melting point 152-153°C. [0003] Jinghong Gonagenin A is extracted from the leaves of Jinghong Gonagarin, an anemone plant, and has a strong anti-tumor effect. Both the literature "Jinghong Gnagarin Induces Human Promyelocytic Leukemia Cell Apoptosis and Its Signal Transduction Pathway" and the patent "Jinghong Gnagarin A and Its Preparation and Application" have reported Significant anti-tumor effects of nalcohol. [0004] The existing method for purifying Jinghong Gonagenin is as follows: Jinghong Gonaxiang leaves or stems are extracted by cold immersion i...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCY02P20/54Y02P20/582
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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