Acrylate polymer capillary vessel electric chromatogram monolithic column modified by macrocyclic polyamines and preparation thereof

A technology of capillary electrochromatography and macrocyclic polyamine, which is applied in the fields of analytical chemistry and polymer chemistry, and can solve the problems of complex substance separation without specific selectivity and limited application scope.

Inactive Publication Date: 2010-01-13
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the vast majority of organic polymer monolithic columns are prepared with acrylates as monomers by free radical polymerization, they have strong hy...

Method used

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  • Acrylate polymer capillary vessel electric chromatogram monolithic column modified by macrocyclic polyamines and preparation thereof
  • Acrylate polymer capillary vessel electric chromatogram monolithic column modified by macrocyclic polyamines and preparation thereof
  • Acrylate polymer capillary vessel electric chromatogram monolithic column modified by macrocyclic polyamines and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] First, 30% (v / v) glycidyl methacrylate, 10% (v / v) ethylene glycol dimethacrylate, 20% (v / v) 1,4-butanediol, 30% (v / v) of n-propanol and 10% (v / v) of secondary water are fully mixed, then add azo Diisobutyronitrile, homogenize the resulting solution with N 2 The oxygen was purged to remove the oxygen and mixed into a homogeneous phase. The homogeneous solution obtained above was injected into a capillary with an inner diameter of 100 μm, and then sealed at both ends and placed in a water bath at 50°C for 20 hours to react. After the reaction is completed, the capillary is taken out and the seal is cut off, and the residual reaction solution is washed away with acetonitrile and methanol to obtain an unmodified polymer monolithic column. Inject a 3% (w / v) methanol solution of macrocyclic polyamines containing 1,4,10,13,16-pentaazatricyclohexacane-9,17-dione into the above-mentioned monolithic In the capillary, then seal the capillary and place it in a constant temperatur...

Embodiment 2

[0016] First, 40% (v / v) glycidyl methacrylate, 15% (v / v) ethylene glycol dimethacrylate, 15% (v / v) 1,4-butanediol, After fully mixing 25% (v / v) of n-propanol and 5% (v / v) of secondary water, add azobis Isobutyronitrile, the resulting solution was homogenized by ultrasonic oscillation and then washed with N 2 The oxygen is purged to remove the oxygen and it is mixed into a homogeneous phase. The homogeneous solution obtained above was injected into a capillary with an inner diameter of 100 μm, and then both ends of the capillary were sealed and placed in a water bath at 60° C. for 16 hours to react. After the reaction is completed, the capillary is taken out and the seal is cut off, and the residual reaction solution is washed away with acetonitrile and methanol to obtain an unmodified polymer monolithic column. Inject a 12% (w / v) methanol solution of macrocyclic polyamines containing 1,4,10,13,16-pentaazatricyclohexacane-9,17-dione into the above-mentioned monolithic In the...

Embodiment 3

[0018] First, 35% (v / v) of glycidyl methacrylate, 12% (v / v) of ethylene glycol dimethacrylate, 18% (v / v) of 1,4-butanediol, 30% (v / v) of n-propanol and 5% (v / v) of secondary water are fully mixed, and then add azobis Isobutyronitrile, the resulting solution was homogenized by ultrasonic oscillation and then washed with N 2 The oxygen is purged to remove the oxygen and it is mixed into a homogeneous phase. The homogeneous solution obtained above was injected into a capillary with an inner diameter of 100 μm, and then both ends of the capillary were sealed and placed in a water bath at 50° C. for 20 hours to react. After the reaction is completed, the capillary is taken out and the seal is cut off, and the residual reaction solution is washed away with acetonitrile and methanol to obtain an unmodified polymer monolithic column. Inject the macrocyclic polyamine methanol solution containing 1,4,10,13,16-pentaazatricyclohecodecane-9,17-dione 3% (w / v) into the above-mentioned inte...

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Abstract

The present invention provides an acrylate polymer capillary electrochromatography column decorated by macrocyclic polyamine and its preparing method, the column of acrylate polymer organic polymer decorated by macrocyclic polyamine is prepared by free radical polymerization and method of column back decoration, the whole surface of the acrylate polymer in the electrochromatography column is linked with a macrocyclic polyamine, the macrocyclic polyamine is 1, 4, 10, 13, 16-quinquevalent nitrogen trinuclear heneicosane-9, 17-diketone. The preparing method of acrylate polymer capillary electrochromatography column decorated by macrocyclic polyamine is simple, having better reproduction quality, the capillary electrochromatography column has a better separating effect to inorganic anions, benzenediol isomer, benzoic acid derivatives and ribonucleotide, having better application in the separating aspect for complicated component material.

Description

technical field [0001] The invention relates to a capillary electrochromatographic monolithic column and a preparation method thereof, in particular to a macrocyclic polyamine-modified acrylate polymer capillary electrochromatographic monolithic column and a preparation method thereof, belonging to the field of polymer chemistry and the field of analytical chemistry. Background technique [0002] Capillary electrochromatography combines the advantages of high performance liquid chromatography and capillary electrophoresis, and is a new type of separation technology developed in the past two decades. Among them, the preparation of the electrochromatographic column is the core part of the technology. In recent years, the electrochromatographic column technology has been developed rapidly, and there have been column-making technologies such as packed column, open-tubular column, and monolithic column. solved problem. Since the vast majority of organic polymer monolithic colum...

Claims

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Application Information

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IPC IPC(8): B01D15/22B01D57/02G01N30/60G01N27/447
Inventor 曾昭睿田耘
Owner WUHAN UNIV
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