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Method for purifying epigallo catechin gallate (EGCG)

A technology of epigallocatechin and gallate, which is applied in the field of separation and purification of effective components of natural plants, can solve the problems of time-consuming, non-continuous automatic production, and low utilization rate of adsorbents, and achieve the effect of reducing costs

Active Publication Date: 2011-12-14
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

EGCG is the polyphenol mixture extracted from tea leaves, the main component of tea polyphenols. In tea polyphenols, there are other flavanol compounds that are very similar in chemical structure and properties to EGCG, such as: epicatechin (EC) ; epicatechin gallate (ECG); epigallocatechin gallate (EGC); gallocatechin gallate (GCG); DL-catechin (DL-C), and these flavanols Very easy to oxidize and poly(condense), making it difficult to separate and purify EGCG monomer
[0003] At present, the main technology to obtain high-purity EGCG monomer (higher than 95%) is to prepare chromatographic separation method, such as: CN1319597 (a kind of separation method of catechin compounds in tea polyphenols), CN1603319 (catechin monomer separation and purification method) and CN1465572 (purification method of epigallocatechin gallate monomer) using Sephadex LH-20 column chromatography; CN101381359 (a high-purity epigallocatechin extracted from green tea The method of plain gallate) adopts the chromatography of flashing silica gel column, and CN101723927A (a kind of catechin monomer EGCG industrial production separation and purification method) adopts the chromatography of KR100-5C18 column, although these methods can be used in industry High-purity EGCG is produced, but it is a batch process, that is, a batch purification process, which cannot be produced continuously and automatically, and the utilization rate of the adsorbent is low, the consumption of the eluent is large, the processing amount of the raw material is small, time-consuming, and the production efficiency is low.
There is no report on the separation and purification of EGCG by simulated moving bed chromatography

Method used

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  • Method for purifying epigallo catechin gallate (EGCG)
  • Method for purifying epigallo catechin gallate (EGCG)
  • Method for purifying epigallo catechin gallate (EGCG)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) SMB device

[0036] 8 chromatographic columns, mobile phase D delivery pump flow rate 0-10mL / min, pressure 0-10Mpa; material liquid F pump flow rate 0-30mL / h, pressure 0-8Mpa; mobile phase P delivery pump flow rate 0-10mL / min, Pressure 0-10Mpa, 48 automatic control valves, a set of single-chip automatic control system, 5 liquid storage tanks (mobile phase D, raw material F, mobile phase P, extract E, raffinate R each need a liquid storage tank) , multi-pass, pipelines, connectors, computer; the chromatographic column is 10cm×1cm; the stationary phase uses octadecylsilane bonded silica gel ODS, 20-30μm.

[0037] (2) SMB working conditions

[0038] The first SMB working conditions are as follows:

[0039] SMB operation mode: set the total number of columns of the SMB system to N=4, set the SMB elution zone to 1 chromatographic column, the refining zone to 1 chromatographic column, the adsorption zone to 2 chromatographic columns, and the operating mode is 1-1-2;

...

Embodiment 2

[0055] (1) SMB equipment: same as embodiment 1.

[0056] (2) SMB working conditions

[0057] The first SMB working conditions are as follows:

[0058] SMB operation mode: set the total number of columns of the SMB system to N=5, set the SMB elution zone to 1 chromatographic column, the refining zone to 2 chromatographic columns, the adsorption zone to 2 chromatographic columns, and the operating mode is 1-2-2;

[0059] Mobile phase composition: the mobile phase D of the refining zone and the adsorption zone is a mixed solution of ethanol and water, and the volume percentage of ethanol is C D is 15%; the mobile phase P of the elution band is ethanol;

[0060] Mobile phase flow rate: In the elution zone, eluent P flow rate U p is 3.8cm / min, the flow rate of extract E is U E =U p ; In the polishing zone and the adsorption zone, the eluent D flow rate U D is 2.9cm / min, the flow rate of the sample fluid F is U F 0.25cm / min, raffinate R flow rate U R =U D + U F .

[0061]...

Embodiment 3

[0073] (1) SMB equipment: same as embodiment 1.

[0074] (2) SMB working conditions

[0075] The first SMB working conditions are as follows:

[0076] SMB operation mode: set the total number of columns of the SMB system to N=6, set the SMB elution zone to 1 chromatographic column, the refining zone to 3 chromatographic columns, the adsorption zone to 2 chromatographic columns, and the operating mode is 1-3-2;

[0077] Mobile phase composition: the mobile phase D of the refining zone and the adsorption zone is a mixed solution of ethanol and water, and the volume percentage of ethanol is C D is 15%; the mobile phase P of the elution band is ethanol;

[0078] Mobile phase flow rate: In the elution zone, eluent P flow rate U p is 5.1cm / min, the flow rate of extract E is U E =U p ; In the polishing zone and the adsorption zone, the eluent D flow rate U D is 2.9cm / min, the flow rate of the sample fluid F is U F 0.25cm / min, raffinate R flow rate U R =U D + U F .

[0079]...

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Abstract

The invention discloses a method for separating and purifying epigallo catechin gallate (EGCG) by using a simulated moving bed (SMB) chromatography. The method is characterized in that: a tea leaf extract, which is tea polyphenol, is adopted as a raw material; EGCG is separated and purified by using an SMB chromatography system. According to the method, fundamental zones of the SMB are set as an eluting zone, a refining zone and an absorbing zone. The eluting zone is independent. Octadecylsilane chemically bonded silica ODS is adopted as a stationary phase, a mixed solution of alcohol and water is adopted as a mobile phase, and SMB separation are carried out two times upon a tea polyphenol raw material liquid, wherein one time is for removing impurities which are hard to elute, and the other time is for removing impurities which are easy to elute. The product is processed through a solvent removing process, such that the EGCG product is obtained. With the method, EGCG can be stably, continuously, and automatically purified from tea polyphenol in large scale, and with high efficiency. The recycling rate of the product is above 94%, and the purity of the product is above 96%. According to the invention, the stationary phase and the mobile phase can be repeatedly utilized, such that the cost is reduced. The invention belongs to green and environment-friendly separation engineering.

Description

technical field [0001] The invention relates to a method for separating and purifying effective components of natural plants, in particular to a method for purifying epigallocatechin gallate (EGCG) by using three-band simulated moving bed chromatography. Background technique [0002] Epigallocatechin gallate (abbreviated as EGCG, hereinafter referred to as EGCG) is an active substance with strong antioxidant and free radical scavenging functions. Its extraction and application have attracted widespread attention at home and abroad. EGCG is the polyphenol mixture extracted from tea leaves, the main component of tea polyphenols. In tea polyphenols, there are other flavanol compounds that are very similar in chemical structure and properties to EGCG, such as: epicatechin (EC) ; epicatechin gallate (ECG); epigallocatechin gallate (EGC); gallocatechin gallate (GCG); DL-catechin (DL-C), and these flavanols It is very easy to oxidize and poly(condensate), which makes it difficult...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 王绍艳郑斯文吴秀红丛景香唐晓丹韩冰杨磊
Owner UNIV OF SCI & TECH LIAONING
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