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Process for preparing methylation catechin by tea

A technology of methylated catechins and process methods, which is applied in the field of extracting methylated catechins, can solve the problems of high process operation requirements, large waste residue treatment capacity, catechin oxidation, etc., and achieves overcoming sample adsorption and safety Good performance and low cost

Inactive Publication Date: 2008-05-14
SOUTHWEST UNIVERSITY
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0009] At present, the methods of industrial extraction of catechins are mainly solvent extraction and ion precipitation. Solvent extraction is the most widely used method at present. This method is mature and stable, and the extraction rate is high. However, various organic solvents are used in production. And the amount is large, and some are even toxic solvents (such as chloroform), so it is difficult to be accepted by industries such as food and medicine
The ion precipitation method reduces the use of organic solvents, and the catechins produced have high purity, but the process operation requirements are high, and the pH value must be strictly controlled, otherwise the catechins may be oxidized. At the same time, a large amount of acid and alkali is used in the process. A large amount of waste residue is processed, which is likely to cause environmental pollution

Method used

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  • Process for preparing methylation catechin by tea
  • Process for preparing methylation catechin by tea
  • Process for preparing methylation catechin by tea

Examples

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preparation example Construction

[0036] The preparation steps of the present invention are as follows:

[0037] (1) Sample preparation: pick fresh tea leaves with one bud and two or three leaves, and wither in a withering room with a withering sieve for 5 to 12 hours under ventilated conditions. , dry with a dryer, and pulverize the tea leaves into 60-80 mesh powder with a pulverizer;

[0038] (2) Ethanol extraction: put tea powder and 60-80% ethanol solution in the extraction tank for solid-liquid extraction at the same time, the extraction temperature is 70-90°C, the time is 30-120 minutes, and the ratio of solid to liquid is 1:3- 1:10, use a vacuum filter to carry out suction filtration, and the filter residue is repeatedly extracted 2 to 5 times;

[0039] (3) Purification of the crude extract: after merging all the extracts, carry out vacuum concentration in the concentration tank, the concentrate and petroleum ether solution are mixed in a volume ratio of 1: 1 to 1: 2, and the liquid-liquid extraction i...

Embodiment 1

[0057] Pick fresh tea leaves with one bud and two or three leaves, and wither in a withering room with a withering sieve for 5 hours under ventilated conditions. Pulverize into 60-mesh powder with a pulverizer; add 60% ethanol to the tea powder according to the ratio of material to liquid 1:3, and extract at 70°C for 30 minutes. After the extraction is completed, filter and extract the filter residue twice. Concentrate, mix the concentrated solution and petroleum ether solution at a volume ratio of 1:1, carry out liquid-liquid extraction for 5 minutes, and repeat the operation twice; then mix the obtained raffinate with ethyl acetate at a volume ratio of 1:1, Carry out liquid-liquid extraction for 5 minutes, repeat the operation 2 times, filter and concentrate the obtained extract to obtain a concentrate, and dry the concentrate to obtain dry powder A of methylated catechin crude extract; use the pretreated Put the 20 mesh crude polyamide resin into the chromatographic column,...

Embodiment 2

[0060] Pick fresh tea leaves with one bud and two or three leaves, and wither in a withering room for 8 hours with a withering sieve under ventilated conditions. Pulverize into a 70-mesh powder; add 70% ethanol to the tea powder according to the ratio of material to liquid 1:6, and extract at 80°C for 60 minutes. After the extraction is completed, filter and extract the filter residue repeatedly for 3 times. Concentrate, mix the concentrated solution and petroleum ether solution at a volume ratio of 1:1, carry out liquid-liquid extraction for 15 minutes, and repeat the operation 3 times; then mix the obtained raffinate with ethyl acetate at a volume ratio of 1:1, Carry out liquid-liquid extraction for 15 minutes, repeat the operation 3 times, filter and concentrate the obtained extract to obtain a concentrate, and dry the concentrate to obtain dry powder A of the crude extract of methylated catechin; 30-mesh crude polyamide resin is loaded into a chromatographic column, and th...

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Abstract

The invention relates to a method for preparing methylated catechin from tea, comprising following steps: tea powder is extracted with ethanol and petroleum ether to remove chlorophyll and fat-soluble constituents; methylated catechin crude extraction dry powder A is obtained through extraction with ethyl acetate; methylated catechin crude product is obtained via separation and purification with crude polyamide resin and fine polyamide resin; methylated catechin pure product is obtained via further purification with high speed counter current chromatography. The invention has the advantages that the invention establishes purification craft of methylated catechin firstly at home and obtains high purity methylated catechin; the invention adopts high speed counter current chromatography (HSCCC) preparation craft, which does not need solid support and overcomes defects such as sample adsorption, loss, pollution and tailed peak arisen from solid phase support compared to high speed liquid chromatography (HSLC) preparation craft; high speed counter current chromatography also has the advantages of large quantity preparation, low comprehensive cost and easy industrial popularization.

Description

technical field [0001] The invention relates to a method for preparing active ingredients from natural products, in particular to a process for extracting methylated catechin from tea leaves. Background technique [0002] In the late 1990s, Japanese scientists were the first to successfully isolate and identify two new catechin derivatives with anti-allergic function from Taiwan Dongding Oolong Tea. After separation and purification, the molecular structures were proved to be (-)- Epigallocatechin 3-O(3-O-methyl)gallate (C-1) and (-)-epigallocatechin 3-O(4-O-methyl)gallate (C -2). It is a white powdery substance, easily soluble in water and organic solvents, and its structural formula is as shown in formula (1): [0003] [0004] R 1 R 2 [0005] EGCG H H [0006] EGCG3″Me CH 3 h [0007] EGCG4″Me H CH 3 [0008] EGCG3″Me and EGCG4″Me have very significant effects on anti-allergy, especially anti-hay fever allergy. Hay fever is the mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62A61K31/353A61P37/08A61K36/82
Inventor 龚正礼罗正飞杨坚童华荣谢进平
Owner SOUTHWEST UNIVERSITY
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