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Method for purifying monomer of epigallocatechingallate (EGCG)

A technology of epigallocatechin and gallate, applied in the field of epigallocatechin gallate monomer purification, can solve problems such as difficult industrialized production, low yield, difficulty in regeneration of adsorbents, etc., and achieves low cost, The effect of high yield, easy industrial control and mass production

Inactive Publication Date: 2004-01-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods can obtain high-purity epigallocatechin gallate (EGCG) products, they only stay in the laboratory because of their large investment, low yield, difficult regeneration of adsorbent and complicated operation. Not easy to industrialize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Take by weighing 25 grams of tea extracts whose total amount of tea polyphenols is greater than 95%, add 75ml of methanol or other dissolving solvents to dissolve it (no insolubles), add 450ml of dichloromethane or other crystallization solvents to this solution at low temperature, stir Make the catechin precipitate, stand still for 30min, vacuum filter with nitrogen to get the filter cake; use 75ml of methanol or other dissolving solvent to dissolve and filter out the slightly insoluble matter, add 450ml of dichloromethane or other crystallization solvent to make the catechin Precipitate, vacuum suction filtration with nitrogen filling, get filter cake, so repeat 5~6 times, dissolve with distilled water and make the solution that concentration is 15%, pass Sephadex LH-20 column (sample solid weight and adsorbent weight ratio 1:20), elute with 80% ethanol or other elution solvents, collect the EGCG fraction (collect after the green strips are exhausted), the volume is on...

Embodiment 2

[0011] Take by weighing 25 grams of tea extracts whose total amount of tea polyphenols is greater than 90%, add 100ml of acetone or other dissolving solvents to dissolve it (no insolubles), add 700ml of dichloromethane or other crystallization solvents to this solution at low temperature, stir Make the catechin precipitate, let it stand for 30min, vacuum filter with nitrogen to get the filter cake; use 100ml of methanol or other dissolving solvent to dissolve and filter out the slightly insoluble matter, add 700ml of dichloromethane or other crystallization solvent to make the catechin Precipitate, vacuum suction filtration with nitrogen filling, get filter cake, so repeat 5~6 times, dissolve with distilled water and make the solution that concentration is 15%, pass Sephadex LH-20 column (sample solid weight and adsorbent weight ratio 1:20), elute with 80% ethanol or other elution solvents, collect the EGCG fraction (collect after the green strips are exhausted), the volume is ...

example 3

[0013] Take by weighing 50 grams of tea extracts whose total amount of tea polyphenols is greater than 80%, add 200ml of ethyl acetate or other dissolving solvents to dissolve it, remove insoluble matter, add 1600ml of chloroform or other crystallization solvents to this solution at low temperature, Stir to precipitate catechins, let stand for 30 minutes, fill with nitrogen and vacuum filter to obtain a filter cake; repeat this for 8 to 9 times, dissolve with distilled water to make a solution with a concentration of 15%, and pass through a Sephadex LH-20 column (the ratio of sample solid weight to adsorbent weight is 1:20), elute with 80% ethanol or other elution solvents, and collect the EGCG fraction (collect after the green strips are exhausted), the volume is 1 / 10 of the total elution solvent 1. Recover ethanol under reduced pressure and vacuum at 40°C, and freeze-dry to obtain 5.8 g of EGCG, which is an off-white powder with a purity of 98.3% by HPLC analysis.

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Abstract

The method for purifying epigallocatechin gallate monomer includes the following steps: using 1g of tea extract, adding 3-4 ml of dissolution solvent, filtering to obtain red-brown solution, slowly-adding 18-32 ml of crystallization solvent at low temp. of 4-6 deg.C, separating out catechin completely, stirring to make block be precipitated and dispersed, standing still, charging nitrogen, vacuumsuction-filtering, taking out filter residue and adding dissolution solvent and dissolving adding crystallization solvent to make precipitation, charging nitrogen, vacuum suction-filtering, taking out filter kesidue, repeating the above-mentioned operation for above 7 times, dissolving filter residue with distilled water to obtain solution whose concentration is 15%, making said solution pass through gel column, eluting, collecting EGCG fraction.

Description

technical field [0001] The invention relates to a purification method of epigallocatechin gallate (EGCG) monomer. Background technique [0002] Tea polyphenols (Tea polyphenols, referred to as TP) is a natural antioxidant extracted from the traditional beverage green tea, which is composed of flavanols (catechins), anthocyanins, flavonoids and flavonols, A complex composed of more than 30 compounds in four categories, including phenolic acids and phenolic acids. It has a variety of health care and pharmacological effects such as scavenging free radicals, anti-oxidation, anti-mutation, anti-aging, anti-radiation, anti-cancer and anti-cancer, lowering blood fat and cholesterol, anti-atherosclerosis and antibacterial. It has been proved that the biological activity of tea polyphenols is mainly related to the action of epigallocatechin gallate (EGCG). Therefore, the research and development of a new process for the purification of epigallocatechin gal...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 沈生荣于海宁
Owner ZHEJIANG UNIV
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