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Raw material prescription of polar ion interchange electric chromatographic column and preparation thereof

A technology of ion exchange and electrochromatographic column, which is applied in the field of raw material formulation and preparation of polar ion exchange electrochromatographic column, which can solve problems such as interruption of electroosmotic flow, generation of bubbles at the interface, and test failure, so as to achieve good permeability and avoid irreversibility The effect of tailing and a wide range of pH application

Inactive Publication Date: 2011-05-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because in the reversed-phase mode, a mobile phase with little or no organic modifier must be used to separate polar substances. Since the mobile phase cannot fully wet the surface of the stationary phase, it is easy to generate air bubbles at the interface. Causes interruption of electroosmotic flow, test failure (Allen, D., EI Rassi, Z., J. Chromatogr. A 2004, 1029, 239-247)

Method used

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  • Raw material prescription of polar ion interchange electric chromatographic column and preparation thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Pretreatment of capillaries

[0020] First wash the empty capillary column with 0.1mol / L HCl solution for about 30min, then rinse with deionized water for 15min, then rinse with 0.1mol / L NaOH for 4h, then rinse with deionized water for 15min, then rinse with methanol for 15min, Blow dry with nitrogen gas.

[0021] 2. Add a mixture of methanol and methacryloxypropyltrimethoxysilane with a volume ratio of 1:1 to the capillary treated in step 1, and react at 60° C. for 24 hours. Then rinse with methanol for 15min. Blow dry at 70°C with nitrogen.

[0022] 3. In-column synthesis

[0023] 2-hydroxyethyl methacrylate, ethylene glycol dimethacrylate, methacrylic acid, toluene and lauryl alcohol were respectively 23.9%, 8.0%, 8.0%, 29.9%, 30.1% by weight, added The amount of initiator azobisisobutyronitrile (AIBN) is 0.3% of the amount of polymer monomer. After the mixture is ultrasonically oscillated for 15 minutes, nitrogen gas is blown for 10 minutes to remove dissolve...

Embodiment 2

[0025] 2-hydroxyethyl methacrylate, ethylene glycol dimethacrylate, N, N-allyl dimethylamine, cyclohexanol and dodecanol were respectively 28.0%, 8.1%, 4.0%, 29.8%, 30.1%, the amount of the added initiator azobisisobutyronitrile is 1% of the amount of the polymer monomer, after the mixture is ultrasonically oscillated for 15 minutes, nitrogen is blown for 10 minutes to remove dissolved oxygen, and the reaction solution is injected into In the treated capillary of a certain length, seal both ends of the capillary, and react for 20 hours under a UV lamp at 25°C. After the reaction is completed, wash the column with methanol and then with mobile phase to remove possible residual reagents in the capillary. , to obtain a polar ion-exchange electrochromatographic column.

Embodiment 3

[0027] 2-hydroxyethyl methacrylate, ethylene glycol dimethacrylate, methacrylic acid, toluene and lauryl alcohol were respectively 23.9%, 8.0%, 8.0%, 25.8%, 35.2% by weight, added The amount of initiator azobisisobutyronitrile is 0.3% of the amount of polymer monomers. After the mixture is ultrasonically oscillated for 20 minutes, nitrogen gas is blown for 10 minutes to remove dissolved oxygen, and the reaction solution is injected into a treated capillary of a certain length. In the process, both ends of the capillary were sealed, immersed in a water bath at 60°C, and reacted for 10 hours. After the reaction was completed, the column was first washed with methanol and then with mobile phase to remove possible residual reagents in the capillary, and polar ion exchange electrochromatography was obtained. column.

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Abstract

The invention provides a material formulation of a polar ion exchange electrochromatographic column and preparation method thereof. The material contains neutral compound monomer, ionic compound monomer, cross-linking agent, initiator and porgenic agent. According to the material formulation, the neutral compound monomer, the ionic compound monomer and the cross-linking agent are polymerized in the presence of the initiator and the porgenic agent in a capillary to prepare the polar ion exchange electrochromatographic column. The polar ion exchange electrochromatographic column solves a problem of a reverse phase electrochromatographic column on difficult separation of polar compound and can select different ion exchange modes according to different objects to be separated and satisfy the requirement of continuous and rapid separation of neutral, acidic and alkaline substances. The column has good permeability and is applicable in a buffer salt system with a wider pH value range and high concentration. Plug burning at two ends of the column is obviated during preparation, and difficulty on filling the column is also avoided.

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 polar ion exchange electrochromatographic column. Background technique [0002] Capillary electrochromatography (CEC) is a micro-separation technology combining high performance liquid chromatography (HPLC) and capillary electrophoresis (CE). Its mobile phase is driven by electroosmotic flow in the tube. Efficiency of electrophoresis. There are currently three types of electrochromatographic columns: capillary packed columns, capillary open-tube columns, and capillary monolithic columns. Packed columns have been developed rapidly recently, but the plunger must be prepared, and the stopper usually causes the generation of air bubbles, which may cause the interruption of the experimental run. Although the open-tube column has no sealing problem and can obtain higher column efficiency, it is also li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/288B01D15/36
Inventor 谢增鸿王晓春吕海霞林旭聪
Owner FUZHOU UNIV
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