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Hydrophilic strong anion exchange action hybrid silica gel capillary chromatographic column

A technology of capillary electrochromatography and strong anions, applied in the field of capillary electrochromatography, can solve problems such as poor compatibility and incompatibility, achieve uniform distribution, increase polarity, and apply to a wide range of separation objects

Inactive Publication Date: 2013-08-28
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention applies the water-soluble initiator to the organic-inorganic hybridization reaction, which solves the problem of poor compatibility or even incompatibility of the components in the conventional hybridization technology; The distribution ratio of each component in the polymerization reaction of the column prepared a new hybrid silica monolithic column

Method used

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  • Hydrophilic strong anion exchange action hybrid silica gel capillary chromatographic column
  • Hydrophilic strong anion exchange action hybrid silica gel capillary chromatographic column
  • Hydrophilic strong anion exchange action hybrid silica gel capillary chromatographic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Mix tetramethoxysilane and vinyltrimethoxysilane in a volume ratio of 3:1 to 5:1, 0.27g polyethylene glycol and 2.5mL of 0.01mol / L acetic acid solution in an ice-water bath Stir and hydrolyze to obtain a sol, take 0.5 mL of the sol solution and one of 30-40 mg of acryloyloxyethyltrimethylammonium chloride, 0.7-1.0 mg of azobisisobutyramidine hydrochloride or ammonium persulfate, and ultrasonically After shaking and mixing, the mixture was injected into the pretreated quartz capillary. Both ends of the capillary were closed, immersed in a 40°C water bath for 12 hours, and then transferred to a 60°C water bath for 12 hours. After the reaction was completed, the capillary column was rinsed with deionized water and methanol mobile phase to remove the residual reagents in the column to obtain a polar Ion exchange hybrid silica gel electrochromatographic column.

Embodiment 2

[0021] In CEC mode, pH 5.0, ion concentration 30 mmol / L, acetonitrile:amine formate (85 / 15, v / v) buffer as mobile phase, applied voltage 10 kV, auxiliary pressure 3.5 MPa, pump flow rate 0.1 Under the condition of mL / min, basic nucleosides and base polar compounds can be effectively separated on the polar ion-exchange hybrid silica gel electrochromatographic column, and the peak shape is symmetrical and there is no tailing phenomenon. Its spectrum is as image 3 shown.

Embodiment 3

[0023] In CEC mode, pH 3.5, ion concentration 100 mmol / L, acetonitrile:amine formate (75 / 25, v / v) buffer as mobile phase, applied voltage 20 kV, auxiliary pressure 10.8 MPa, pump flow rate 0.1 Under the condition of mL / min, the nucleotide polar compounds achieved baseline separation on this polar ion-exchange hybrid silica column. Its spectrum is as Figure 4 shown.

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Abstract

The invention provides a hydrophilic strong anion exchange action hybrid silica gel capillary chromatographic column and a preparation method thereof. Stationary phases are obtained by organosiloxane gel condensation polymerization and ethylene bond copolymerization of organic ion monomer and a silica gel framework; and according to the formula of raw materials, in siloxane, the volume ratio of tetramethoxysilane to vinyl trimethoxy silane is (3:1)-(5:1), quarternary ammonium ion monomer is 60 to 80mg / ml, and the weight percentage of water-soluble initiator is 0.7 to 1.0 percent. Polymerization stationary phases of the hybrid silica gel monolithic column are distributed uniformly, positive charge quaternary ammonium groups are carried on the surfaces of the stationary phases, strong and stable normal phase electroosmotic flow can be generated in a large pH range, and good iron exchange sites can be provided, so the capillary chromatographic column has a hydrophilic-strong anion exchange hybrid separation mode, and can meet the continuous quick separation requirement of neutral, acid and alkaline substances.

Description

technical field [0001] The invention relates to a hydrophilic strong anion exchange hybrid silica gel capillary electrochromatographic column and a preparation method thereof, belonging to the technical field of capillary electrochromatography. Background technique [0002] Capillary electrochromatography (CEC) is a fast and efficient micro-separation technology developed in recent years. It uses electroosmotic flow (EOF) or electroosmotic flow combined with pressure to drive the mobile phase. Efficiency of electrophoresis. At present, electrochromatographic columns are mainly divided into three types: capillary open-tube column, capillary packed column and capillary monolithic column. Among them, the capillary monolithic column has the advantages of simple preparation, uniform internal structure, fast mass transfer rate, low column pressure and no need for sintered plunger, and has become a research hotspot in the field of CEC. As a type of capillary electrochromatographi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J41/20B01D15/04
Inventor 林旭聪王啸郑燕琼谢增鸿
Owner FUZHOU UNIV
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