Quaternary ammonium functionalized anion-exchange organic polymer monolithic column for capillary electrochromatography and its preparation and application

A technology of capillary electrochromatography and functionalization, which is applied in the field of quaternary ammonium functionalized anion-exchange organic polymer capillary electrochromatography monolithic columns, which can solve the problems of strong hydrophobicity, not widely used, difficult peak extraction, etc., and achieve good repeatability , good chromatographic performance and simple preparation method

Active Publication Date: 2019-07-09
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the development of organic polymer capillary monolithic columns is mature, but most of them are reversed-phase chromatographic columns with strong hydrophobicity and poor selectivity for the separation of organic acidic substances, and there are problems of difficult or no peaks
Anion-exchange chromatographic columns effectively solve the above problems, but this type of monolithic column has limited development and is not widely used, and it is difficult to meet the needs of complex component material separation

Method used

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  • Quaternary ammonium functionalized anion-exchange organic polymer monolithic column for capillary electrochromatography and its preparation and application
  • Quaternary ammonium functionalized anion-exchange organic polymer monolithic column for capillary electrochromatography and its preparation and application
  • Quaternary ammonium functionalized anion-exchange organic polymer monolithic column for capillary electrochromatography and its preparation and application

Examples

Experimental program
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Effect test

Embodiment 1

[0020] (1) Cut off a 35cm long quartz capillary (inner diameter 100μm). After pretreatment, prepare a 50% (v / v) methanol solution of methacryloxypropyltrimethoxysilane, suck it into a syringe and inject it into the pretreated capillary, Connect the two ends with Teflon to form a ring, and place it in a 45°C water bath overnight to react to vinylize the inner wall of the capillary; then rinse the capillary with methanol for 30 minutes, and dry it with N 2 Blow dry and set aside.

[0021] (2) Mix 20 mg of N-benzylquinine chloride, 20 mg of methacrylamide, 76 μL of ethylene glycol dimethacrylate, 303 μL of methanol, 143 μL of diethylene glycol, and 2.0 mg of azo Diisobutyronitrile was placed in a 2mL eppendorf tube, and ultrasonically mixed for 10 minutes to remove air bubbles.

[0022] (3) Inject the homogeneous solution obtained in step (2) into the capillary treated with the silylating reagent in step (1), control the injection length to 25.5 cm, seal both ends with silica ge...

Embodiment 2

[0025] (1) Cut off a 35cm long quartz capillary (inner diameter 100μm). After pretreatment, prepare a 50% (v / v) methanol solution of methacryloxypropyltrimethoxysilane, suck it into a syringe and inject it into the pretreated capillary, Connect the two ends with Teflon to form a ring, and place it in a 45°C water bath overnight to react to vinylize the inner wall of the capillary; then rinse the capillary with methanol for 30 minutes, and dry it with N 2 Blow dry and set aside.

[0026] (2) Add 25 mg of N-benzylquinine chloride, 15 mg of methacrylamide, 76 μL of ethylene glycol dimethacrylate, 303 μL of methanol, 143 μL of diethylene glycol, and 2.0 mg of azo Diisobutyronitrile was placed in a 2mL eppendorf tube, and ultrasonically mixed for 10 minutes to remove air bubbles.

[0027] (3) Inject the homogeneous solution obtained in step (2) into the capillary treated with the silylating reagent in step (1), control the injection length to 25.5 cm, seal both ends with silica ge...

Embodiment 3

[0029] (1) Cut off a 35cm long quartz capillary (inner diameter 100μm). After pretreatment, prepare a 50% (v / v) methanol solution of methacryloxypropyltrimethoxysilane, suck it into a syringe and inject it into the pretreated capillary, Connect the two ends with Teflon to form a ring, and place it in a 45°C water bath overnight to react to vinylize the inner wall of the capillary; then rinse the capillary with methanol for 30 minutes, and dry it with N 2 Blow dry and set aside.

[0030] (2) Mix 30 mg of N-benzylquinine chloride, 10 mg of methacrylamide, 76 μL of ethylene glycol dimethacrylate, 303 μL of methanol, 143 μL of diethylene glycol, and 2.0 mg of azo Diisobutyronitrile was placed in a 2mL eppendorf tube, and ultrasonically mixed for 10 minutes to remove air bubbles.

[0031] (3) Inject the homogeneous solution obtained in step (2) into the capillary treated with the silylating reagent in step (1), control the injection length to 25.5 cm, seal both ends with silica ge...

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Abstract

The invention discloses a quaternary amine alkali functional anion exchange organic polymer capillary electrochromatography monolithic column as well as a preparation method and application thereof and belongs to the field of analytical chemistry. A stationary phase of the capillary electrochromatography monolithic column is an integral porous organic framework material generated by carrying out in situ polymerization reaction on functional monomers, namely N-benzyl quinine chloride and methacrylamide, and a crosslinking agent ethylene glycol dimethacrylate in pore forming agents, namely methanol and diethylene glycol. The preparation method disclosed by the invention has the advantages that a quaternary amine alkali functional monomer N-benzyl quinine chloride is adopted for preparing ananion exchange chromatography stationary phase, the method is simple, chromatographic performance is excellent, and reproducibility is good; and the quaternary amine alkali functional anion exchange organic polymer capillary electrochromatography monolithic column can be used for rapid separation and detection of organic acid small molecules, solves the problems that a peak of an acid compound appears difficultly and does not appear and has great application potential in the aspect of separation of a complex component substance.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a quaternary ammonium functionalized anion-exchange organic polymer capillary electrochromatographic monolithic column and its preparation and application. Background technique [0002] Capillary electrochromatographic columns are the core of capillary electrochromatographic research, and there are mainly three column types: packed column, open-tubular column, and monolithic column. Organic polymer capillary monolithic columns have become a hotspot in the research of capillary electrochromatographic columns because of their advantages such as simple preparation method, no need to design plungers, large column capacity, and high column efficiency. At present, the development of organic polymer capillary monolithic columns is mature, but most of them are reversed-phase chromatographic columns, which have strong hydrophobicity and are not very selective for the separat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/285B01D15/22B01D15/38G01N30/02
Inventor 陈子林毛振坤覃小宁
Owner WUHAN UNIV
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