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Method for preparing punicalagin molecularly imprinted polymer monolithic column by utilizing in-situ polymerization method

A punicalagin molecule, in-situ polymerization technology is applied in the field of in-situ polymerization to prepare a punicalagin molecularly imprinted polymer monolithic column, which can solve the problems of difficult separation and purification, low content of active components, complex system and the like, and avoids column packing. The procedure, the preparation process is simple, and the effect of simplifying the experimental process

Active Publication Date: 2013-01-02
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

However, due to the low content of active ingredients in natural products, it is difficult to enrich; the system is complex, macromolecules and small molecules, living and non-living substances coexist, especially isomers with similar structures, resulting in difficult separation and purification; many natural products The active ingredients are sensitive to heat, easy to hydrolyze, etc. Therefore, obtaining higher purity punicalagin through separation and purification is a major difficulty in its research and development

Method used

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  • Method for preparing punicalagin molecularly imprinted polymer monolithic column by utilizing in-situ polymerization method
  • Method for preparing punicalagin molecularly imprinted polymer monolithic column by utilizing in-situ polymerization method
  • Method for preparing punicalagin molecularly imprinted polymer monolithic column by utilizing in-situ polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation and separation of punicalagin and its structural analogues on a molecularly imprinted monolithic column for punicalagin

[0019] Molecularly imprinted monolithic column with punicalagin as template was synthesized by in situ polymerization, and its retention performance was evaluated by connecting it to high performance liquid chromatography under appropriate chromatographic conditions. Synthetic reaction conditions and processing method are as follows:

[0020] Preparation of punicalagin molecularly imprinted monolithic column by in situ polymerization:

[0021] a. According to the mass number of punicalagin-imprinted monolithic column synthesized in a stainless steel column, accurately weigh the template molecule as punicalagin 3.00%, the functional monomer as acrylamide 2.37%, and the cross-linking agent as ethyl dimethacrylate Glycol ester 33.03%, porogen is polystyrene dissolved in tetrahydrofuran solution 56.50% (wherein the concentration of polystyre...

Embodiment 2

[0025] Embodiment 2 (contrast)

[0026] Separation of punicalagin and its structural analogues on a blank monolithic column

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

[0028] Except that the template molecule punicalagin was not added, a non-imprinted blank column was synthesized with the same method and experimental conditions as in Example 1. After polymerization is complete, rinse with THF to remove residual porogen and unreacted reagents from the monolith.

[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 punicalagin and its analogues R and retention time t of acetone 0 , to calculate the retention factor k'.

[0030] The results sho...

Embodiment 3

[0033] Preparation of punicalagin molecularly imprinted monolithic column by in situ polymerization:

[0034] a. According to the mass number of punicalagin-imprinted monolithic column synthesized in a stainless steel column, accurately weigh the template molecule as punicalagin 3.19%, the functional monomer as acrylamide 2.51%, and the cross-linking agent as ethyl dimethacrylate Glycol ester 29.03%, porogen is 59.87% polystyrene dissolved in tetrahydrofuran solution (wherein the concentration of polystyrene dissolved in tetrahydrofuran solution is 40mg / ml), then add isooctane 4.96%, initiator is azo Diisobutyronitrile 0.44% mixed, placed in a sonicator, sonicated for 20 minutes to make it uniform and clarified, then transferred to a clean stainless steel column (100×4.6mm I.D.), degassed by sonication for 15 minutes, and 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 32 hours;

[0035] b. Rem...

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Abstract

The invention relates to a method for preparing a punicalagin molecularly imprinted polymer monolithic column by utilizing a in-situ polymerization method, and the method is characterized in that pre-polymerized mixed solution is directly injected inside a stainless steel pipe column to prepare continuous bar-shaped polymer, and a cross-linked polymer material with fixed size and fixed shape of holes and regularly-arranged functional groups and identifying template molecules, i.e. molecularly imprinted polymer is obtained. The molecularly imprinted polymer monolithic column prepared through the method has advantages of good imprinting effect and good permeability, and the imprinted factor reaches 13.1; and meanwhile, the method is simple in preparation process, the internal structure of the molecularly imprinted polymer monolithic column is uniform, recurrence is good, the complicated column loading procedures can be avoided, and the molecularly imprinted polymer monolithic column can be directly used for analysis.

Description

technical field [0001] The invention relates to a method for preparing punicalagin molecularly imprinted polymer monolithic columns by in-situ polymerization. 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 polymerization method; (3) dispersi...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30C08F222/14C08F220/56C08F2/44C08J9/26
Inventor 刘照胜班璐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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