Novel bifunctional group mixed mode organic polymer monolithic column, and preparation method and application thereof

A mixed-mode, monolithic column technology, applied in the direction of separation methods, chemical instruments and methods, and other chemical processes, can solve the problems of limited application range, insufficient selection of substances to be separated, and single mode, so as to expand the application range, Excellent reverse chromatography retention performance, good permeability effect

Pending Publication Date: 2020-11-03
河南省农产品质量安全检测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional styrene-based organic polymer monolithic columns for electrochromatography mainly include styrene-divinylbenzene, chloromethylstyrene-divinylbenzene, etc., all of which are reversed-phase chromatographic columns. The modes of these types of monolithic columns mainly focus on In single chromatographic modes such as reversed-phase, hydrophilic, anion / cation exchange, etc., the mode is relatively single, and the selection diversity of the substances to be separated is insufficient, which limits its application range

Method used

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  • Novel bifunctional group mixed mode organic polymer monolithic column, and preparation method and application thereof
  • Novel bifunctional group mixed mode organic polymer monolithic column, and preparation method and application thereof
  • Novel bifunctional group mixed mode organic polymer monolithic column, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Capillary pretreatment: First, take a certain length of empty quartz capillary column with an inner diameter of 50 μm, use 1.0M NaOH solution to wash the capillary for 20 minutes, and use deionized water to wash it to neutral; thirdly, use 0.4M HCl solution for alkaline The pretreated capillary was rinsed for 20 min, then rinsed with deionized water until neutral; finally, rinsed with methanol solution for 10 min, and then rinsed with N 2 Blow dry; use the above process to pretreat the four quartz capillary empty columns respectively, and set aside.

Embodiment 2

[0031] Vinylation of the inner wall of the capillary: use 50% volume concentration of methacryloxypropyltriethoxysilane as the solute and methanol as the solvent to carry out the pretreatment of the four quartz capillary empty columns in Example 1, respectively. treatment, and use a Teflon tube (Teflon tube) to connect the two ends of the quartz capillary to form a ring, place it in a water bath with a preset temperature of 45°C and heat it at a constant temperature for 18 hours to vinylize the inner wall of the quartz capillary; then, wash it with methanol for 20 minutes Remove the unreacted silane reagent, then use N 2 Blow dry; get four vinylized quartz capillary empty columns, spare;

Embodiment 3

[0033] Quartz capillary monolithic column preparation: 3.8% (w / w) of 4-vinylbiphenyl, 2.2% (w / w) of N,N,N-trimethylvinylbenzyl ammonium chloride, 9.0% ( w / w) of ethylene glycol dimethacrylate, 42.5% (w / w) of cyclohexanol, 42.5% (w / w) of dodecanol and 1.5% of 4-vinylbiphenyl, N, Azobisisobutyronitrile of the total mass of N,N-trimethylvinylbenzyl ammonium chloride and ethylene glycol dimethacrylate is placed in an Eppendorf centrifuge tube (eppendorf tube) for ultrasonic mixing, and removed Bubbles; inject the polymer solution obtained above into one of the vinylation-modified quartz capillaries in Example 2, control the injection length at 25.5 cm, and heat at a constant temperature in a water bath with a preset temperature of 65°C for 24 hours; rinse with methanol The above-mentioned quartz capillary removes unreacted monomers and porogens to obtain a monolithic column of bifunctional group mixed-mode organic polymers.

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Abstract

The invention relates to the field of preparation of liquid chromatography capillary monolithic columns, in particular to a novel bifunctional group mixed mode organic polymer monolithic column and apreparation method and application thereof, wherein the polymer monolithic column is formed by copolymerization of a bifunctional group monomer and an inner wall vinylation modified capillary tube ina capillary tube; one functional group monomer is N,N,N-trimethylvinylbenzenemethylammonium chloride with extremely strong hydrophilicity and pi-pi interaction, while the other functional group monomer is 4-vinylbiphenyl with excellent reverse chromatography retention performance; the vinylation modified solution is a solution taking methacryloyloxypropyltriethoxysilane as a solute and methanol asa solvent. The organic polymer electrochromatography monolithic column has the advantages of rich porous structure, good permeability, reverse phase and hydrophilic chromatographic separation performances, and realization of the separation of a plurality of substances in different chromatographic modes, high application values. The invention provides a new idea for the development of the novel mixed mode organic polymer electrochromatography monolithic column.

Description

technical field [0001] The invention specifically relates to the field of liquid chromatography capillary monolithic column preparation, in particular to a novel dual-functional group mixed-mode organic polymer monolithic column, its preparation method and its application. Background technique [0002] Mixed-mode chromatography refers to a chromatographic method in which the stationary phase has multiple functions and provides more than two kinds of interaction forces to make the solute partition, retain and separate in the stationary phase (J.Chromatogr.A 2011, 1218, 8813–8825), It mainly includes hydrophilic / ion exchange mixed mode chromatography, reversed phase / ion exchange mixed mode chromatography and reversed phase / hydrophilic interaction mixed mode chromatography. Due to the organic combination of various forces, mixed-mode chromatography has stronger separation selectivity than single-mode chromatography, and is more suitable for the separation and analysis of comple...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/281B01J20/285G01N23/2251G01N30/02G01N30/60G01N30/64B01D15/34B01D15/32
CPCG01N30/48B01J20/265B01J20/285B01D15/325B01D15/34G01N30/02G01N30/6078G01N23/2251G01N30/64B01J20/292
Inventor 崔超姬伯梁包方管立于璐宋伟史俊华余新华乔礼魏钢崔敏张世兰黄继勇何霞许琦刘远航赵毓群张琪王飞刘宇刘姝言赵雅娴王峰刘绍伟
Owner 河南省农产品质量安全检测中心
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