Separation method of effective components of sharpleaf galangal fruit aqueous extract

A separation method and technology of active ingredients, applied in the separation/purification of carboxylic acid compounds, separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of unreported research on the chemical components of Yizhiren

Active Publication Date: 2015-04-29
HEBEI YILING MEDICINE INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the chemic...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The separation method of the active ingredient in the Yizhiren aqueous extract consists of the following steps:

[0021] A. Extraction: take dry Yizhi kernels, grind them, and use 8 times the amount of water to reflux and extract twice, each time for 1.5 hours, combine the filtrates, and distill under reduced pressure to obtain extracts, dissolve the extracts in distilled water, and use petroleum ether, Extract with ethyl acetate and n-butanol, recover the solvent, and obtain the dry powder of ethyl acetate;

[0022] B. Gel column separation: Dissolve the dry powder obtained in step A with water, filter, put on Sephadex LH-20 gel column, elute with 20-40% ethanol gradient, collect the effluent of each section, 20% ethanol Eluted as F 1 , eluted with 30% ethanol to obtain F 2 , F 3 , F 4 , eluted with 40% ethanol to obtain F 5 , F 6 ;

[0023] C, HPLC purification: the obtained F of step B 2 ~F 6 The components were separated and purified by HPLC, the chromatog...

Embodiment 2

[0025] The separation method of the active ingredient in the Yizhiren aqueous extract consists of the following steps:

[0026] A. Extraction: take the dry Yizhi kernels, crush them and extract them twice with 10 times of water backflow, each time for 1.5 hours, combine the filtrates, and distill under reduced pressure to obtain extracts, dissolve the extracts in distilled water, and use petroleum ether, Extract with ethyl acetate and n-butanol, recover the solvent, and obtain the dry powder of ethyl acetate;

[0027] B. Gel column separation: Dissolve the dry powder obtained in step A with water, filter, put on Sephadex LH-20 gel column, elute with 20-40% ethanol gradient, collect the effluent of each section, 20% ethanol Eluted as F 1 , eluted with 30% ethanol to obtain F 2 , F 3 , F 4 , eluted with 40% ethanol to obtain F 5 , F 6 ;

[0028] C, HPLC purification: the obtained F of step B 2 ~F 6 The components were separated and purified by HPLC, the chromatographic...

Embodiment 3

[0030] The separation method of the active ingredient in the Yizhiren aqueous extract consists of the following steps:

[0031] A. Extraction: take dry Yizhi kernels, crush them and extract them twice with 9 times the amount of water under reflux, each time for 1.5 hours, combine the filtrates, and distill under reduced pressure to obtain extracts, dissolve the extracts in distilled water, and use petroleum ether, Extract with ethyl acetate and n-butanol, recover the solvent, and obtain the dry powder of ethyl acetate;

[0032] B. Gel column separation: Dissolve the dry powder obtained in step A with water, filter, put on Sephadex LH-20 gel column, elute with 20-40% ethanol gradient, collect the effluent of each section, 20% ethanol Eluted as F 1 , eluted with 30% ethanol to obtain F 2 , F 3 , F 4 , eluted with 40% ethanol to obtain F 5 , F 6 ;

[0033] C, HPLC purification: the obtained F of step B 2 ~F 6 The components were separated and purified by HPLC, the chrom...

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PUM

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Abstract

The invention discloses a separation method of effective components of a sharpleaf galangal fruit aqueous extract, belonging to the field of pharmaceutical analysis. The separation method comprises the following steps: (A) fetching dried sharpleaf galangal fruit, grinding, carrying out reflux extraction with water, combining filtrate, carrying out reduced pressure distillation to obtain extractum, dissolving the extractum into distilled water, respectively extracting by virtue of petroleum ether, ethyl acetate and normal butanol, and recycling solvents, so as to obtain ethyl acetate extract dry powder; (B) dissolving the dry powder obtain in the step (A), filtering, and processing by virtue of a sephadex LH20 gel column, so as to obtain six components from F1 to F6; and (C) carrying out HPLC separation and purification on the components from F2 to F6, so as to obtain compounds including protocatechualdehyde, protocatechuic acid, p-coumaric acid, (-)-epicatechin and (+)-catechinic acid. According to the separation method, the effective active components are separated and extracted from the sharpleaf galangal fruit, the structures of the effective components are further defined, the basis is provided for later medication, and required components can be extracted according to different requirements.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to the separation and purification of active ingredients of traditional Chinese medicines. Background technique [0002] Yizhiren is the dry and mature fruit of A.oxyphylla Miq., a plant of the genus Alpinia Roxb. in the Zingiberaceae family. It is one of the four major southern medicines in China and is mainly produced in Hainan and Guangdong. For commonly used Chinese herbal medicines. Yizhiren has the functions of warming the kidney, consolidating essence and shrinking urination, warming the spleen, stopping diarrhea, and absorbing saliva. It is mostly used clinically for enuresis due to kidney deficiency, frequent urination, white turbid spermatorrhea, diarrhea due to spleen cold, cold pain in the abdomen, and excessive saliva. Modern pharmacological studies have shown that the water extract of Yizhiren has neuroprotective and antioxidant effects, and Yizhiren also has the function...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C65/03C07C59/48C07C47/565C07C45/78C07D311/62
CPCC07C45/78C07C51/42C07D311/62C07C47/565C07C65/03C07C59/52
Inventor 王宗权常青鲜贾继明乔莉姜新刚孟作环秦拢马艳玲宋剑裴彩云王贵金蔡燕周梦夏
Owner HEBEI YILING MEDICINE INST
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