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Preparation method of epiglloctechin gallate imprinted polymer monolithic column

A technology for epigallocatechin and gallate, which is applied in the field of preparing epigallocatechin gallate molecularly imprinted polymer monolithic columns by in-situ polymerization, can solve the problems of easy oxidation, difficulty in obtaining high purity, and the like, Achieve the effect of easy operation, avoid column packing procedures, and simplify the experimental process

Inactive Publication Date: 2013-05-01
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the chemical structure and properties of epigallocatechin gallate (EGCG) and other components in catechin are very similar, and it is very easy to oxidize and poly(condense), it is difficult to obtain high-purity epigallocatechin Ethyl gallate (EGCG) monomer

Method used

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  • Preparation method of epiglloctechin gallate imprinted polymer monolithic column
  • Preparation method of epiglloctechin gallate imprinted polymer monolithic column
  • Preparation method of epiglloctechin gallate imprinted polymer monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of epigallocatechin gallate imprinted monolithic column by in situ polymerization:

[0021] a. According to the mass number of the integrated epigallocatechin gallate imprinted column synthesized in a stainless steel column, the template molecule was accurately weighed as epigallocatechin gallate 2.88%, and the functional monomer was acrylamide 5.45% The cross-linking agent is 74.71% ethylene glycol dimethacrylate, the porogen is 5.5% polystyrene dissolved in THF solution (concentration 40mg / ml) and 10.53% isooctane is added, and the initiator is azobis Mix isobutyronitrile 0.93%, ultrasonic for 20 minutes to make it uniform and clear, then transfer to a clean stainless steel column 100×4.6mmI.D., ultrasonic degassing for 15 minutes, seal both ends of the stainless steel column, React in a constant temperature water bath with a temperature of 60°C for 24 hours;

[0022] b. Removal of template molecules: Take out the synthesized stainless steel column and co...

Embodiment 2

[0025] Embodiment 2 (control)

[0026] Separation of Epigallocatechin Gallate and Its Structural Analogues by Blank Monolithic Column

[0027]In order to investigate the retention of epigallocatechin gallate and its structural analogues on non-imprinted columns, a blank column without template epigallocatechin gallate was synthesized as a control. The specific operation steps are as follows:

[0028] Except that the template molecule epigallocatechin gallate was not added, a non-imprinted blank column was synthesized with the same method and experimental conditions as in Example 1. After the polymerization was completed, it was washed with tetrahydrofuran to remove the porogen and residual porogen in the monolithic column. Unreacted reagents;

[0029] The chromatographic evaluation is the same as the investigation of the imprinted column in Example 1, that is, under the same mobile phase conditions, by measuring the retention time t of epigallocatechin gallate and its analog...

Embodiment 3

[0033] Preparation of epigallocatechin gallate imprinted monolithic column by in situ polymerization:

[0034] a. According to the mass number of the integrated epigallocatechin gallate imprinted column synthesized in a stainless steel column, accurately weigh the template molecule as epigallocatechin gallate 5.60%, and the functional monomer as acrylamide 5.1% , The crosslinking agent is ethylene glycol dimethacrylate 72.62%, the porogen is 5.28% of polystyrene dissolved in tetrahydrofuran solution (concentration 40mg / ml), and then 10.5% of isooctane is added, and the initiator is azo Mix 0.90% diisobutyronitrile, put it into a sonicator, sonicate for 20 minutes to make it homogeneous and clear, then transfer it to a clean stainless steel column (100×4.6mm I.D.), degas it for 15 minutes, and put the stainless steel tube Seal both ends of the column, and react in a constant temperature water bath at a temperature of 60°C for 24 hours;

[0035] b. Removal of template molecules...

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Abstract

The invention relates to a preparation method of an epiglloctechin gallate molecularly imprinted polymer monolithic column by an in-situ polymerization method. The method comprises the step of directly injecting a pre-polymerized mixed solution into a stainless steel pipe column to prepare a continuous clavate polymer to obtain a crosslinked high-polymer material which has the fixed size and shape of a hole, has a functional group with confirmed arrangement, and can identify template molecules, i.e. a molecularly imprinted polymer (MIP). The molecularly imprinted polymer (MIP) monolithic column obtained by the method not only has a printing effect, but also has the advantage of good permeability, imprinted factors can reach 3.09, and the method is simple in preparation process, even in an internal structure, good in reproducibility, free from a complex column packing procedure, and capable of being directly used for analysis.

Description

technical field [0001] The invention relates to a method for preparing an epigallocatechin gallate molecularly imprinted polymer integral column by an in-situ polymerization method. Background technique [0002] Molecular imprinting technology refers to the technology of using a specific molecule as a template to prepare materials with special recognition function and high selectivity for the molecule. It is usually described as an "artificial lock" technology for creating a "molecular key" for identification. It dissolves template molecules, monomers, and cross-linking agents in a certain solution to form a pre-polymerization solution, and forms a three-dimensional space with functional groups that completely match the spatial structure of the template molecule and specifically bind to the template molecule after polymerization. hole polymer. At present, there are many preparation methods of MIP, mainly including: (1) bulk polymerization method; (2) suspension polymerizati...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/26B01J20/30C08F222/14C08F220/56C08F2/44C08J9/26
Inventor 刘照胜孙璇黄艳萍阿吉艾克拜尔·艾萨
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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