Method for purifying sennoside A

A purification method, the technology of sennoside, which is applied in the field of purification of sennoside A, can solve the problems such as the rare separation and research of sennoside A, achieve the simultaneous completion of separation, purification and preparation, facilitate separation and preparation, and save organic The effect of the solvent

Inactive Publication Date: 2011-11-16
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the prior art, there are many studies on the extraction of total sennosides, but few studies on the separation of sennoside A
At present, there is no relevant research report on the application of high-speed countercurrent chromatography technology to the separation of sennoside A

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 1kg of senna leaves, add 5L of petroleum ether to reflux and degrease for 30min, filter out the degreased matter and dry it, add 10L of ethanol for percolation extraction for 2h, keep the extraction temperature at 50°C, concentrate the extract to extract, and use an appropriate amount of 1 % sodium bicarbonate solution was dissolved, the insoluble matter was filtered out, and an equal amount of dichloromethane was added to extract twice, the raffinate was adjusted to neutrality by adding dilute hydrochloric acid, allowed to stand for precipitation, and the precipitate was filtered out and dried to obtain crude sennoside;

[0019] Measure ethyl acetate-methanol-water according to the ratio of 20:3:20, mix well and take the upper phase as the stationary phase, and the lower phase as the mobile phase, dissolve the crude sennoside in the upper phase to make a sample solution, and use 10ml Pump the stationary phase into the chromatographic column at a flow rate of / min. ...

Embodiment 2

[0021] Take 1kg of senna leaf medicinal material, add 7L petroleum ether to reflux and degrease 3 times, 20min each time, filter out the degreased matter and dry, add 20L ethanol for percolation extraction for 2h, keep the extraction temperature at 80°C, and concentrate the extract to extract Dissolve with an appropriate amount of 5% sodium bicarbonate solution, filter out the insoluble matter, add an equal amount of dichloromethane to extract 5 times, add dilute hydrochloric acid to the raffinate to neutral, let it stand for precipitation, filter out the precipitate and dry to obtain sennoside Crude;

[0022] Measure ethyl acetate-methanol-water according to the ratio of 20:1:20, mix well and take the upper phase as the stationary phase, and the lower phase as the mobile phase, dissolve the crude sennoside in the upper phase to make a sample solution, and use 10ml Pump the stationary phase into the chromatographic column at a flow rate of / min. After the stationary phase is f...

Embodiment 3

[0024] Take 5kg of senna leaves, add 30L of petroleum ether to reflux and degrease for 40min, filter out the degreased matter and dry, add 60L of ethanol for percolation extraction for 2h, keep the extraction temperature at 70°C, concentrate the extract to extract, and use an appropriate amount of 3 % sodium bicarbonate solution was dissolved, the insoluble matter was filtered out, and an equal amount of dichloromethane was added to extract 3 times, the raffinate was adjusted to neutrality by adding dilute hydrochloric acid, allowed to stand for precipitation, and the precipitate was filtered out and dried to obtain crude sennoside;

[0025] Measure ethyl acetate-methanol-water according to the ratio of 20:2:20, mix well and take the upper phase as the stationary phase, and the lower phase as the mobile phase, dissolve the crude sennoside in the upper phase to make a sample solution, and use 10ml Pump the stationary phase into the chromatographic column at a flow rate of / min. ...

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Abstract

The invention provides a method for sennoside A, which comprises the following steps of: taking a medicinal material of folium sennae, adding petroleum ether for refluxing and defatting, adding ethanol into a defatted product for temperature-keeping percolation, concentrating an extracting solution to obtain an extract, dissolving the extract by adding a sodium bicarbonate solution, filtering off insoluble substances, extracting by adding dichloromethane, adding acid into raffinate to regulate the pH to be neutral, filtering out a precipitate, and separating by adopting high speed countercurrent chromatography to obtain the sennoside A. The method has the advantages of short production period and high product purity, and can be directly used for chromatographic standard samples, commerce and the like.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry and relates to a method for purifying sennoside A. Background technique: [0002] Senna leaf is the dry leaflet of Cassia angustifolia Vahl or Cassia acutifolia Delile of the leguminous plant. It is sweet, bitter and cold in nature, and returns to the large intestine meridian; it is used for treating fever Stomach stagnation, constipation, abdominal pain, edema, fullness, etc. According to literature reports, it mainly contains sennosides A, B, C (sennoside A, B, C) and anthracene glycosides such as rhein, aloe-emodin and chrysophanol, among which sennosides A and B are senna leaves Its main active ingredient has a stronger laxative effect and irritation than other anthraquinone-containing laxatives, and is often used clinically for acute constipation. [0003] Sennoside A: Pale yellow crystals [0004] Molecular formula: C 42 h 38 o 20 [0005] Molecular weight: 826.74 [0006] P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/244C07H1/08
Inventor 刘东锋吴艳波杨成东
Owner NANJING ZELANG MEDICAL TECH
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