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Preparation method of chlorogenic acid uniformly-imprinted microspheres

A chlorogenic acid, uniform technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of high price of perfluoropolymer dispersants, difficulty in obtaining microsphere particles with uniform particle size, poor selection and recognition ability Advanced problems, to achieve the effect of high practical value, high product recovery rate and strong selectivity

Inactive Publication Date: 2015-03-11
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, although there are many studies on the preparation of molecularly imprinted polymers with polyphenolic compounds such as chlorogenic acid as templates, it is difficult to obtain microspheres with uniform particle size and excellent performance, and have the basic conditions for industrial application.
Molecularly imprinted microspheres with controllable particle size and regular shape can be prepared by dispersion polymerization, but the perfluoropolymer dispersant used is expensive and economical; although multi-step swelling method can be prepared in polar solvent Imprinted microspheres, but the operation process is cumbersome
[0004] In the past, we studied the preparation of caffeic acid-imprinted polymers by in-situ polymerization in empty chromatographic columns, and discussed their chromatographic identification and solid-phase extraction performance. Precipitation polymerization, but without success

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Dissolve chlorogenic acid and functional monomer MAA in acetonitrile-toluene-DMSO mixed solution at a molar ratio of 1:4, shake at room temperature for 5 hours, and then add cross-linking agent (DVB) 5 times the amount of the monomer and 0.475mmol initiator (AIBN), then transfer the mixture into a glass ampule bottle, pass nitrogen gas for 10 min, seal the ampule bottle, rotate and polymerize at 60°C for 24 hours, settle with methanol for 3 times and then with tetrahydrofuran for 2 times After filtering, vacuum drying to constant weight is obtained.

[0013] The invention uses chlorogenic acid as a template molecule, and adopts a precipitation polymerization method to prepare uniform imprinted microspheres with a diameter of about 2.5um, and the polymer yield is 35.93%.

Embodiment 2

[0015] (1) Dissolve chlorogenic acid and functional monomer MAA in acetonitrile-toluene-DMSO mixed solution at a molar ratio of 1:4.6, shake at room temperature for 6.3 hours, and then add cross-linking agent 8 times the amount of the monomer (DVB) and 0.475mmol initiator (AIBN), then transfer the mixture into a glass ampoule, pass nitrogen gas for 13 min, seal the ampoule well, rotate the polymerization at 60°C for 24 hours, settle with methanol for 2 times, and then use tetrahydrofuran After settling for 3 times, filter and vacuum dry to constant weight.

[0016] The present invention uses chlorogenic acid as a template molecule to prepare uniform imprinted microspheres with a diameter of about 2.5um by precipitation polymerization, and the polymer yield is 37.86%.

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PUM

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Abstract

The invention discloses a preparation method of chlorogenic acid uniformly-imprinted microspheres, which comprises the following steps: dissolving chlorogenic acid and functional monomer MMA (methacrylic acid) in a mole ratio of 1:3-1:5 in an acetonitrile-toluene-DMSO (dimethyl sulfoxide) mixed solution, oscillating at room temperature for 3-7 hours, adding a crosslinking agent DVB (divinylbenzene) and a right amount of initiator AIBN (2,2'-azobisisobutyronitrile), transferring the mixture into a glass ampoul, introducing nitrogen for 5-15 minutes, sealing the ampoul, carrying out rotary polymerization at 60 DEG C for 24 hours, precipitating with methanol, precipitating with tetrahydrofuran, and filtering. The uniformly-imprinted microspheres with the diameter of about 2.5 mu m are prepared by using chlorogenic acid as the template molecule by a precipitation polymerization process. The polymer yield is 35-40%; and the molecularly imprinted polymer has uniform particle size and proper size, can be conveniently used as a liquid chromatography separation material and for preparation, separation and purification, and has the advantages of favorable separation efficiency, high extraction yield and wide application prospects.

Description

technical field [0001] The invention relates to a preparation method of chlorogenic acid uniform imprinted microspheres. Background technique [0002] The development of new high-selectivity separation materials is an important step to achieve high-efficiency separation. Molecularly imprinted polymer is a high molecular polymer that completely matches the target molecule in terms of space and binding sites after polymerizing target molecules, functional monomers, and cross-linking agents in a solution and removing the target molecules. This imprinted polymer can specifically recognize target molecules when extracting complex samples, so it is a separation medium with important application prospects. [0003] At present, although there are many studies on the preparation of molecularly imprinted polymers with polyphenolic compounds such as chlorogenic acid as templates, it is difficult to obtain microspheres with uniform particle size and excellent performance, which have th...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F212/36C08J9/26B01J20/285B01J20/30
Inventor 李辉王素素张月李志平
Owner JISHOU UNIVERSITY
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