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Preparation method of cleomiscosin A

A technology of stinky brucellin and raw materials, which is applied in the field of preparation of stinky blain A, and can solve problems such as pollution, large amount of solvent used, and low yield

Inactive Publication Date: 2013-11-27
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Through literature search, stinkin A is prepared by conventional solvent extraction and silica gel column separation. This kind of method has low yield, large amount of solvent and serious pollution defect

Method used

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  • Preparation method of cleomiscosin A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take the stinky vegetable raw material and grind it into 40 mesh after drying, take 2kg, put it in a supercritical CO2 extraction tank for extraction, feed CO2 at a flow rate of 2ml / min / g raw material, and use methanol solution as an entrainer at a flow rate of 0.3ml / min / g Raw materials, at an extraction temperature of 45°C, a pressure of 20Mpa, and an extraction time of 2 hours, add 100g of neutral alumina resin to the obtained extract and pack it into a column, elute impurities with 400ml of petroleum ether, and then elute with 400ml of ethyl acetate, collect and wash with 150ml Reagent is recovered by dehydration to obtain extract. Take n-hexane, ethyl acetate, methanol, and water as the solvent system, mix according to the ratio of 1:3:2:2, take the upper phase and inject it into a high-speed countercurrent chromatography tube as the stationary phase, and remove the lower phase as the mobile phase at a flow rate of 3ml / min. The speed of the main engine is 850rpm, th...

Embodiment 2

[0018] Take the stinky vegetable raw material and grind it into 60 mesh after drying, take 2kg, put it in a supercritical CO2 extraction tank for extraction, feed CO2 at a flow rate of 3ml / min / g raw material, methanol solution as entrainer, and the flow rate is 0.2ml / min / g Raw materials, at an extraction temperature of 40°C, a pressure of 18Mpa, and an extraction time of 2 hours, add 80g of neutral alumina resin to the obtained extract and pack it into a column, elute impurities with 400ml of petroleum ether, and then elute with 400ml of ethyl acetate, collect and wash with 300ml Reagent is recovered by dehydration to obtain extract. Take n-hexane, ethyl acetate, methanol, and water as the solvent system, mix according to the ratio of 2:3:4:2, take the upper phase and inject it into a high-speed countercurrent chromatography tube as the stationary phase, and remove the lower phase as the mobile phase at a flow rate of 3ml / min. The speed of the main engine is 800rpm, the mobile...

Embodiment 3

[0020] Take the stinky vegetable raw material and grind it into 80 meshes after drying, take 2kg, put it in a supercritical CO2 extraction tank for extraction, feed CO2 at a flow rate of 3ml / min / g raw material, and use methanol solution as an entrainer at a flow rate of 0.2ml / min / g Raw materials, at an extraction temperature of 60°C, a pressure of 20Mpa, and an extraction time of 3 hours, add 100g of neutral alumina resin to the obtained extract and pack it into a column, elute impurities with 500ml of petroleum ether, and then elute with 400ml of ethyl acetate, collect and wash with 300ml Reagent is recovered by dehydration to obtain extract. Take n-hexane, ethyl acetate, methanol, and water as the solvent system, mix according to the ratio of 4:8:7:5, take the upper phase and inject it into a high-speed countercurrent chromatography tube as the stationary phase, and remove the lower phase as the mobile phase at a flow rate of 2ml / min. The speed of the main engine is 850rpm, ...

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Abstract

The invention discloses a preparation method of cleomiscosin A. The method comprises the following steps: A. taking a Cleome vircosa L. raw material, drying, pulverizing into 20-80 meshes, extracting at 30-60 DEG C under the pressure of 15-30 Mpa in a supercritical CO2 extraction tank for 1-4 hours, and resolving to obtain an extract, wherein the CO2 flow rate is 1-4ml / min / g raw material, methanol is used as an entrainer, and the flow rate of the methanol is 0.3-0.5ml / min / g raw material; and B. adding an aluminum oxide resin into the extract, drying, filling into a column, sequentially eluting with petroleum ether and ethyl acetate, collecting the ethyl acetate eluate, concentrating reduced pressure, separating the obtained extractum by high-speed counter-current chromatography, collecting the fraction according to the chromatogram, concentrating reduced pressure, and drying. The invention is convenient to operate and low in pollution, and is suitable for producing high-purity cleomiscosin A.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a preparation method of stinky sagittalin A. Background technique [0002] Smelly savannin A is a coumarin substance, molecular formula C20H18O8, molecular weight 386.36, molecular structural formula: [0003] [0004] Smelly sagittalin A has cytotoxic activity and stem protection activity. Cleome vircosa L. is a Cleome vircosa L. of the cauliflower family. The whole herb is used as medicine. It is bitter, pungent, warm, toxic, and has the effects of dispelling blood stasis, reducing swelling, removing putrefaction and promoting muscle growth. [0005] According to the literature search, stinkinin A is prepared by conventional solvent extraction and silica gel column separation. This method has the technical defects of low yield, large amount of solvent, and serious pollution. Contents of the invention [0006] The purpose of the present invention is...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCY02P20/54
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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