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Preparation method of high-purity epicatechin gallate (ECG)

A high-purity technology of epicatechin gallate, which is applied in the field of preparation of high-purity epicatechin gallate, and achieves obvious effects, high yield and good stability

Inactive Publication Date: 2014-01-22
JIANGSU TIANSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the published documents and patents, there is no relevant or similar report of the present invention

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 10 kg of crude tea polyphenols (with an ECG content of 40.4%), add 40 L of purified water, stir and dissolve at room temperature, let stand at room temperature for 24 hours, filter, and discard the residue;

[0025] Add 60L of ethyl acetate to the filtrate to extract twice, combine the ethyl acetate layers, concentrate under reduced pressure at 60°C to a thick paste, add 30L of purified water to dissolve, and obtain a tea polyphenol sample solution;

[0026] Pass the above-mentioned tea polyphenol sample solution through a chromatography column equipped with HPD-600 macroporous adsorption resin, add 100 L of purified water for sufficient desorption and elution, collect the eluent, and obtain epicatechin gallate solution;

[0027] Concentrate the above epicatechin gallate solution under reduced pressure at 55°C to a thick paste, add 18L of purified water to dissolve, let it cool, add about 100mg of high-purity epicatechin gallate with a content of 99.6% to make It w...

Embodiment 2

[0030] Take 10 kg of crude tea polyphenols (with an ECG content of 48.4%), add 100 L of purified water, stir and dissolve at room temperature, let stand at room temperature for 24 hours, filter, and discard the residue;

[0031] Add 100L of ethyl acetate to the filtrate for liquid-liquid extraction twice, combine the ethyl acetate layers, concentrate under reduced pressure at 60°C to a thick paste, add 30L of purified water to dissolve, and obtain a tea polyphenol sample solution;

[0032] Pass the above-mentioned tea polyphenol sample solution through a D101 macroporous adsorption resin chromatography column, add 10% ethanol 100 L to carry out sufficient desorption and elution, collect the eluent, and obtain epicatechin gallate solution;

[0033] Concentrate the above epicatechin gallate solution under reduced pressure at 55°C to a thick paste, add 8 L of acetone to dissolve, let it cool, add about 100 mg of high-purity epicatechin gallate with a content of 99.6% as Seed crys...

Embodiment 3

[0036] Take 10 kg of crude tea polyphenols (with an ECG content of 39.4%), add 20 L of purified water, stir and dissolve at room temperature, let stand at room temperature for 2 hours, filter, and discard the residue;

[0037] Add 20L of ethyl acetate to the filtrate for liquid-liquid extraction twice, combine the ethyl acetate layers, concentrate under reduced pressure at 60°C to a thick paste, add 30L of purified water to dissolve, and obtain a tea polyphenol sample solution;

[0038] Pass the above-mentioned tea polyphenol sample solution through a chromatography column equipped with HPD-600 macroporous adsorption resin, add 100 L of purified water for sufficient desorption and elution, collect the eluent, and obtain epicatechin gallate solution;

[0039]Concentrate the above-mentioned epicatechin gallate solution at 55°C to a thick paste under reduced pressure, add 10 L of ethanol to dissolve, let it cool, add about 100 mg of high-purity epicatechin gallate with a content o...

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Abstract

The invention provides a preparation method of high-purity epicatechin gallate (ECG), belonging to the technical field and domain of organic chemistry. The ECG content is 98.0-99.9%. The preparation method comprises the procedures of abstraction, extraction, chromatographic separation and crystallization. According to the invention, the preparation process has favorable reproducibility; and the obtained epicatechin gallate has the advantages of high content, high yield, no organic solvent residue, low cost, stable and controllable quality and short production cycle, is green, environment-friendly and suitable for industrial production, and conforms to the requirements for clean production.

Description

technical field [0001] The invention discloses a preparation method of high-purity epicatechin gallate (ECG). The invention belongs to the technical field of organic chemistry. Background technique [0002] Tea polyphenols are a polyphenolic component extracted from green tea, which is composed of more than six monomers, among which epicatechin gallate (ECG) and epigallocatechin gallate (EGCG) ) The two main components have the highest content and the strongest pharmacological activity. At present, EGCG has been widely used, and a large amount of ECG is directly discarded and wasted. [0003] Due to the emergence of antibiotic resistance, the huge side effects of anti-tumor drugs and the growth of senile diseases, natural antibacterial, anti-viral, anti-tumor, and anti-aging drugs have gradually attracted widespread attention. And epicatechin gallate (ECG) is one of the natural substances with strong medicinal effect. [0004] Based on domestic and foreign research resul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62
CPCC07D311/62
Inventor 黄全书杨永安魏元刚钟慧易铭金显友袁继文季浩
Owner JIANGSU TIANSHENG PHARMA
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