Polarity ion exchange capillary chromatographic column and preparation method thereof

A capillary chromatographic column and ion exchange technology, which is applied in the field of polar ion exchange capillary chromatographic column and its preparation, can solve the problems of weak retention, etc., and achieve the effect of wide application range of pH and good permeability of the column

Inactive Publication Date: 2009-11-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the monolithic columns studied today are based on the principle of reversed-phase chromatography. Although these monolithic columns have good selectivity for hydrophobic to weakly polar substances, the weaker retention of those highly polar substances is in reversed-phase mode.

Method used

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  • Polarity ion exchange capillary chromatographic column and preparation method thereof
  • Polarity ion exchange capillary chromatographic column and preparation method thereof
  • Polarity ion exchange capillary chromatographic column and preparation method thereof

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preparation example Construction

[0017] The steps of preparation method are:

[0018] 1) Pretreatment of the column: Rinse the empty capillary column with 0.1-1mol / l HCl solution for about 15-30min, then rinse with deionized water for 10-15min, then rinse with 0.1-1mol / l NaOH for 2h-3h, then Rinse with methanol for 15-20 minutes, blow dry with nitrogen and set aside.

[0019] 2) This step is optional: add a 1-2:1 mixture of methanol and methacryloxypropyltrimethoxysilane to the treated capillary in step 1), and react at 40-60°C for 12h-24h. Then rinse with methanol for 10min to 15min. Blow dry with nitrogen at 50-70°C.

[0020] 3) In-column synthesis: mix the raw materials according to the above formula, ultrasonically vibrate the resulting mixture for 10-15 minutes, blow nitrogen to remove the dissolved oxygen in the mixture, then inject the mixture into the treated capillary, seal both ends of the capillary and Immerse in a 60°C water bath and react for 5-20 hours. After the reaction is completed, wash t...

Embodiment 1

[0022] 1. Column pretreatment

[0023] First rinse the capillary empty column with 0.1mol / l HCl solution for about 0.5h, then rinse it with deionized water for 10min, then rinse it with 0.1mol / l NaOH for 2h~3h, then rinse it with methanol for 15min, and dry it with nitrogen gas for later use.

[0024] 2. This step is optional. Add a 1:1 mixture of methanol and methacryloxypropyltrimethoxysilane to the capillary treated in step 1, and react at 60°C for 12h to 24h. Then rinse with methanol for 10min to 15min. Blow dry at 70°C with nitrogen.

[0025] 3. In-column synthesis

[0026] 2-acrylamido-2-methylpropanesulfonic acid, polyethylene glycol diacrylate, water, methanol and diethyl ether were respectively 10.00%: 15.00%: 6.00%: 17.25%: 51.75% by weight, added The amount of initiator azobisisobutyronitrile is 2% of the amount of polymer monomer. After the mixture is ultrasonically oscillated for 20 minutes, blow nitrogen for 10 minutes to remove dissolved oxygen. In a capill...

Embodiment 2

[0028] 3-Propanesulfonic acid methacrylate, pentaerythritol triacrylate, cyclohexanol and ethylene glycol are respectively 10.00% by weight: 10.00%: 60.80%: 19.20%, added initiator azobisisobutyronitrile ( The consumption of AIBN) is 1% of polymer monomer consumption, after the mixture ultrasonic vibration 20min, blow nitrogen 10min to remove dissolved oxygen, inject this reaction solution in the capillary tube of certain length that has been processed by step 2, will Both ends of the capillary were sealed and immersed in a water bath at 60°C for 20 hours of reaction. 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. Normal experiments can be carried out or stored for later use after being balanced for 15 hours under pressure. In the capillary electrochromatography mode, with pH 6.0, ion concentration 5mmol / L, acetonitrile: phosphate (95 / 5, v / v) buffer as mobile phase, a...

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Abstract

The invention provides a polarity ion exchange capillary chromatographic column and a preparation method thereof. The raw material comprises ionic compound monomer, cross linker, initiating agent and pore-foaming agent; the ionic compound monomer and the cross linker are put into a capillary for carrying out polyreaction, and the pore-foaming agent and the initiating agent are added, thus the polarity ion exchange capillary chromatographic column is prepared. The invention utilizes polymerization of polarity ionic compound monomer to provide stationary phase with hydrophilic interaction and adopts novel polarity cross linker to dissolve ionic compound monomer, thus solving the problem that the ionic compound monomer is difficult to be dissolved with the traditional hydrophobic cross linker GDMA monomer. The polarity ion exchange capillary chromatographic column has strong hydrophilic interaction, can provide ion exchange function in different modes and can meet continuous and fast separation requirement of neutral, acid and alkaline substances; the column has good permeability and is applicable to buffer salt system with high concentration; and plug is not needed to be wound at the two ends of the column during preparation, thus avoiding difficulty of filling the column.

Description

technical field [0001] The present invention relates to micro-chromatographic separation technology, more specifically to a polar ion-exchange capillary chromatographic column and a preparation method thereof Background technique [0002] Microchromatographic separations include capillary electrochromatography (CEC) and capillary liquid chromatography (CLC). Compared with traditional high-performance liquid chromatography (HPLC), micro-chromatographic separation has the advantages of less sample and solvent consumption, increased column efficiency in a shorter time, and can be connected to a highly sensitive detector without a splitter. At present, micro-chromatographic columns are divided into three types: capillary packed column, capillary open-tube column and capillary monolithic column. Packed columns are the most commonly used at present, but the preparation is more complicated, and a plunger must be prepared, and the stability of the column is limited to a certain ext...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30
CPCB01D15/361B01D15/305
Inventor 谢增鸿林坚林旭聪林葭
Owner FUZHOU UNIV
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