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Raw material prescription with hydrophile ion interchange and inphase opposition ion interchange separation mode chromatographic column and preparation

A technology of ion exchange and reversed-phase ions, applied in the field of electrochromatography, can solve the problems of brittle columns, high column packing skills, and low sample capacity, and achieve a wide range of separation objects, high space utilization, and fast mass transfer. Effect

Inactive Publication Date: 2008-08-27
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Packed columns have developed rapidly in recent years, but they are difficult to fill and require high column packing skills; and the two ends of the capillary must be sintered with plugs, which makes the column brittle and inconvenient to use. At the same time, the existence of the plug usually causes air bubbles , which may cause interruption of the experiment run
Although the open-tube column has no sealing problem and can obtain higher column efficiency, it is also limited by its small size, low sample capacity, and difficult detection.

Method used

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  • Raw material prescription with hydrophile ion interchange and inphase opposition ion interchange separation mode chromatographic column and preparation
  • Raw material prescription with hydrophile ion interchange and inphase opposition ion interchange separation mode chromatographic column and preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 1. Pretreatment of capillaries

[0023] Rinse the empty capillary column with 0.1mol / L HCl solution for 30 minutes, then rinse it with deionized water for 10 minutes, then rinse it with 0.1mol / L NaOH for 4 hours, then rinse it with methanol for 15 minutes, and dry it with nitrogen gas for use;

[0024] 2. Silanization of the Capillary Wall

[0025] Inject a mixture of methanol and methacryloxypropyltrimethoxysilane with a volume ratio of 1:1 into the capillary treated in step 1, and react at 60°C for 24 hours to bond a layer of alkenyl on the capillary wall. The silanized substance; then rinse with methanol for 15 minutes; dry the capillary with nitrogen at 70°C;

[0026] 3. In-column synthesis

[0027] Glycidyl methacrylate, ethylene glycol dimethacrylate, propyl methacrylate sulfonate, N,N-dimethylformamide and 1,4-butanediol are respectively 29.6% by weight , 10.0%, 0.4%, 12.0%, 48.0%, the amount of added initiator azobisisobutyronitrile (AIBN) is 0.3% of the tota...

Embodiment 2

[0030]Glycidyl methacrylate, ethylene glycol dimethacrylate, methacryloyloxyethyltrimethylammonium chloride, N,N-dimethylformamide and 1,4-butanediol were weighed The ratios are 22.2%, 7.5%, 0.3%, 14.0%, and 56.0%, respectively, and the amount of added initiator azobisisobutyronitrile (AIBN) is 0.3% of the total amount of matrix monomer and ionic monomer. Mix the raw materials according to the above formula, ultrasonically vibrate the resulting mixture for 15 minutes, blow nitrogen gas for 10 minutes to remove dissolved oxygen in the mixture, then inject the mixture into a silanized capillary, and control a certain length to seal both ends of the capillary And immersed in a 60°C water bath, reacted for 36 hours, after the reaction was completed, rinse the capillary column with methanol to remove the residual reagent in the column; then, fill the capillary column with 1mol / L hydrochloric acid solution, and heat it in a 60°C water bath for 4 hours, and finally wash the capillary...

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Abstract

The invention provides a material formulation of a chromatographic column with two separating modes including hydrophilic ion exchange and reversed phase ion exchange and a preparation method thereof. The material contains matrix monomers, ionic monomers, initiator and porgenic agent. According to the material formulation, the matrix monomers and the ionic monomers are polymerized in the presence of the porgenic agent and the initiator in a silanized capillary; after the reaction is finished, the chromatographic column is washed with methanol, and epoxy bonds on the surface of an immobile phase are immobilized by hydrolyzing with acid or base solution to obtain the hydrophilic ion exchange chromatographic column and the reversed phase ion exchange chromatographic column. Plug burning at two ends of the entire column is obviated during preparation and difficulty on filling the column is also avoided. The column has good permeability, simple preparation process and wide range of applicable separated objects, and can satisfy the requirement of high-efficiency and continuous separation of neutral, acidic and basic substances. Two different separation modes can be provided for the same chromatographic column by adjusting proportion of organic modifier in a mobile phase.

Description

technical field [0001] The invention belongs to the technical field of electrochromatography, and more specifically relates to a raw material formula and a preparation method of a chromatographic column having two separation modes of hydrophilic ion exchange and reversed-phase ion exchange. Background technique [0002] Micro-column high-performance liquid chromatography (μ-HPLC), also known as capillary-HPLC, is a chromatographic micro-separation technology developed in recent years. Capillary electrochromatography (CEC) is a micro-separation technology combining capillary liquid chromatography and capillary electrophoresis (CE). Its mobile phase is driven by electroosmotic flow in the tube. sex. Both micro-column high-performance liquid chromatography and capillary electrochromatography have the advantages of low mobile phase and sample consumption, low environmental pollution, high separation efficiency, and easy use with other detection methods, so they play an importan...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01D1/26
CPCB01D15/305B01D15/325B01D15/361B01D15/3847
Inventor 谢增鸿王家斌吕海霞林旭聪
Owner FUZHOU UNIVERSITY
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