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Method for separating and preparing components of eclipta monomer

A technology of Eclipta chinensis and monomer, which is applied in the field of separation and preparation of Eclipta sativa monomer components, can solve the problems of small preparation amount, cumbersome method, and low specificity, and achieve easy control, simple process, and high utilization rate of raw materials Effect

Inactive Publication Date: 2012-01-25
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the existing separation methods for the monomer components of Eclipta chinensis are the combination of silica gel column and gel column. The method is cumbersome, has poor reproducibility, small preparation amount, and low specificity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Grind the Eclipta medicinal material and use 5 times the amount (V / W) of 55% ethanol solution to ultrasonically extract 3 times, each time for 1 hour, concentrate under reduced pressure until no alcohol is obtained to obtain a concentrated solution, extract with n-butanol, recover n-butanol, and extract The product was chromatographed on a silica gel column, eluted with chloroform-methanol solution, the volume ratio of chloroform-methanol was 15:7, the collected fraction was concentrated and dried to obtain a crude extract; : 5: 6: 2 configuration, placed in a separatory funnel to fully shake and then stand still, layered, the upper phase is the stationary phase, the lower phase is the mobile phase, the injection valve is in the injection state, the stationary phase is 10ml / Fill the chromatographic separation column of the countercurrent chromatograph at a flow rate of 1 min, turn on the speed controller, and rotate the helical column clockwise. The extract was dissolv...

Embodiment 2

[0024] Grind the medicinal material of Eclipta officinalis and use 8 times the amount (V / W) of 80% ethanol solution to reflux and extract twice, each time for 2 hours, concentrate under reduced pressure until no alcohol is obtained to obtain a concentrated solution, extract with n-butanol, recover n-butanol, and extract The product was chromatographed on a silica gel column, eluted with chloroform-methanol solution, and the volume ratio of chloroform-methanol was 18:7, and the collected fraction was concentrated and dried to obtain a crude extract; hexane, chloroform, methanol, and water were mixed in a volume ratio of 5 : 6: 5: 4 configuration, placed in a separatory funnel and fully oscillated, let it stand still, layered, the upper phase is the stationary phase, the lower phase is the mobile phase, and the injection valve is in the injection state, the stationary phase is 10ml / Fill the chromatographic separation column of the countercurrent chromatograph at a flow rate of 1...

Embodiment 3

[0027] Grind the Eclipta medicinal material and use 6 times the amount (V / W) of 70% ethanol solution to microwave extract once, extract for 0.5h, concentrate under reduced pressure until there is no alcohol to obtain a concentrated solution, extract with n-butanol, recover n-butanol, extract The product was chromatographed on a silica gel column, eluted with chloroform-methanol solution, and the volume ratio of chloroform-methanol was 20:7, and the collected fraction was concentrated and dried to obtain a crude extract; hexane, chloroform, methanol, and water were mixed in a volume ratio of 3 : 8: 7: 2 configuration, placed in a separatory funnel to fully shake and then stand still, layered, the upper phase is the stationary phase, the lower phase is the mobile phase, the injection valve is in the injection state, the stationary phase is 10ml / Fill the chromatographic separation column of the countercurrent chromatograph at a flow rate of 1 min, turn on the speed controller, an...

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Abstract

The invention relates to a method for separating and preparing components of an eclipta monomer, which comprises the following steps: extracting an eclipta medicinal material by using 55-80% ethanol solution, concentrating an extracted solution, extracting a concentrated solution by using an organic solvent, carrying out column chromatography on an extract by adopting silica gel, eluting the extract by using trichloromethane-methanol, collecting a cut fraction crude extract, and separating the crude extract by applying high-speed counter current chromatography, so as to obtain an eclalbasaponins I monomer, an eclalbasapnoins II monomer and an eclalbasaponins III monomer. The method has the advantages that the operation is simple, the sample loss is less, the preparation amount is large, and the product purity is higher than 98%.

Description

technical field [0001] The invention relates to a method for separating and preparing the monomeric components of Eclipta chinensis, in particular to a method for separating and preparing the monomeric components of Eclipta chinensis from crude extracts of Eclipta spp. Background technique [0002] The traditional Chinese medicine Eclipta chinensis is the whole herb of the Compositae plant, which has the effects of cooling blood, stopping bleeding, nourishing the kidney, and benefiting yin. It is mainly used to treat hematemesis, hemoptysis, epistaxis, hematuria, blood in the stool, bloody dysentery, bleeding from knife wounds, and premature graying of beard and hair. , diphtheria, stranguria, leukorrhea and genital itching embolism. Whole grass contains 1.32% saponin, about 0.08% nicotine, tannin, vitamin A, enterin, various thiophene compounds such as α-tertiary thienylmethanol and its acetate, 2-(butadiynyl)-5 -(vinylethynyl)thiophene, 2-(but-diynyl)-5-(4-chloro-3-hydrox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV