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Preparation method of ECG (epigallocatechin gallate) monomer

A monomer and functional monomer technology, applied in the field of preparation of epicatechin gallate monomer, can solve problems such as human health and safety hazards, export trade obstruction, market application restrictions, etc., and achieve good economic benefits and social value , large amount of preparation and short preparation cycle

Active Publication Date: 2016-07-13
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the limit of pesticide residues in catechin products is implemented according to the standards of tea, and the catechins extracted from qualified tea raw materials often become products with serious pesticide residues, which leads to serious obstacles to its export trade and limited application in domestic and foreign markets. limit
In addition, ECG is easily soluble in water, and is generally used as an additive to water-based beverages or functional foods. The residual pesticides in the beverage or food are then dissolved in the beverage or food and directly ingested by consumers, posing a safety hazard to human health.

Method used

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  • Preparation method of ECG (epigallocatechin gallate) monomer
  • Preparation method of ECG (epigallocatechin gallate) monomer
  • Preparation method of ECG (epigallocatechin gallate) monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Preparation of polymers that specifically recognize ECG

[0045] Add 8.80g of ECG and 6.90g of methacrylic acid monomer reactant into 300mL of chloroform, and react for 2 hours at 4°C in the refrigerator, then add 100g of EGDMA and 2.40g of azobisisobutyronitrile, and ultrasonicate for 10 minutes to make EGDMA Dissolve completely with azobisisobutyronitrile to obtain a mixed solution; shake and react at 60°C for 48 hours, filter the obtained polymer, discard the solution, grind the precipitated polymer, and use 500 mL of methanol and glacial acetic acid with a volume ratio of 9:1 The polymer was subjected to Soxhlet extraction with a mixed solvent, and the extraction was repeated 6 times, each time for 12 hours; after the extraction was completed, the polymer was washed with 200 mL of deionized water and methanol for 20 minutes, and repeated 5 times until the solution was neutral. Finally, dry it in vacuum at 60°C to obtain it.

Embodiment 2

[0046] Example 2 Preparation of polymers that specifically recognize ECG

[0047] Add 8.80g of ECG and 10.6g of methylene succinic acid into 300mL of toluene, react for 4 hours at 4°C in the refrigerator, add 80g of EGDMA and 2.60g of azobisisobutyronitrile, and ultrasonicate for 10 minutes to make EGDMA and diisobutyronitrile Completely dissolve azidione to obtain a mixed solution; shake and react at 70°C for 20 hours, filter the obtained polymer, discard the solution, grind the precipitated polymer, and use 500 mL of a mixed solvent of methanol and glacial acetic acid with a volume ratio of 8:1 The polymer was subjected to Soxhlet extraction, and the extraction was repeated 8 times, each time for 8 hours; after the extraction was completed, the polymer was washed with 200 mL of deionized water and methanol for 20 minutes, and repeated 5 times until the solution was neutral. ℃ vacuum drying, that is.

Embodiment 3

[0048] Example 3 Preparation of polymers that specifically recognize ECG

[0049] Add 8.80g of ECG and 11.8g of p-vinylbenzoic acid into 300mL of chloroform, and react for 4 hours at 6°C in the refrigerator, then add 100g of EGDMA and 2.60g of azobisisobutyronitrile, and ultrasonicate for 10 minutes to make MBAA and azo The diisobutyronitrile was completely dissolved to obtain a mixed solution; the reaction was shaken at 70°C for 20 hours, the obtained polymer was filtered, the solution was discarded, the polymer precipitate was ground, and the mixed solvent of methanol and glacial acetic acid with a volume ratio of 500mL of 10:1 was used to The polymer was subjected to Soxhlet extraction, and the extraction was repeated 6 times, each time for 12 hours; after the extraction was completed, the polymer was washed with 200 mL of deionized water and methanol for 20 minutes, repeated 5 times until the solution was neutral, and finally 60 ° C Vacuum drying, that is.

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Abstract

The invention relates to a preparation method of an ECG (epigallocatechin gallate) monomer. The preparation method comprises the following steps of separating the ECG in tea leaves by column chromatography and crystallizing methods, wherein a filler adopted by the column chromatography is a high molecular polymer which is formed by self-assembly, polymerizing and dilution of one of methacrylic acid, acrylic acid, itaconic acid and 4-vinylbenzoic acid and the ECG. The preparation method has the advantages that the specific recognition capability on the ECG is realized, and the extraction rate and purity of the ECG monomer are high.

Description

technical field [0001] The invention relates to the technical field of tea deep processing, in particular to a preparation method of epicatechin gallate monomer. Background technique [0002] Tea polyphenols is a general term for more than 30 kinds of polyhydric phenolic compounds extracted from tea leaves, accounting for about 10% to 35% of the dry weight of tea leaves, including flavanols (catechins), anthocyanins, flavonoids, Flavonols and phenolic acids, etc., among which catechin is the main component of tea polyphenols, accounting for 70% to 80% of the total amount of tea polyphenols. The catechins in tea can be divided into three free forms: catechin (Catechin, C), epicatechin (Epicatechin, EC), epigallocatechin (Epigallocatechin, EGC); Gallic acid: epicatechin gallate (Epicatechin gallate, ECG), epigallocatechin gallate (Epigallocatechin gallate, EGCG), among which the content of EGCG and ECG is more. [0003] A large number of studies have shown that ester-type ca...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F220/06C08F222/02C08F212/14C08J9/00C07D311/62B01J20/26B01J20/30
CPCB01J20/262B01J2220/445B01J2220/4812C07D311/62C08F222/1006C08F222/102C08J9/00C08J2335/02C08F220/06C08F222/02C08F212/14
Inventor 谭君谭丹文洋
Owner HUNAN AGRICULTURAL UNIV
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