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Zwitterion electric chromatographic column and preparation method thereof

A zwitterion, electrochromatographic column technology, applied in the field of electrochromatography, can solve the problems of good column permeability and difficult separation of polar substances, and achieve the effect of wide range of separation objects and good permeability

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

AI Technical Summary

Problems solved by technology

Because the zwitterions on the surface of the stationary phase are strongly polar and charged, this electrochromatographic column can solve the problem that non-polar stationary phases are difficult to separate polar substances. Different ion exchange modes are selected according to the separation objects to meet neutral and acidic conditions. Continuous and rapid separation requirements of alkaline compounds, good column permeability, wide pH range and high concentration buffer salt system, no need to burn plugs at both ends of the column during preparation, avoiding the difficulty of filling the column

Method used

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  • Zwitterion electric chromatographic column and preparation method thereof
  • Zwitterion electric chromatographic column and preparation method thereof
  • Zwitterion electric chromatographic column and preparation method thereof

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Embodiment 1

[0022] 1. Column pretreatment

[0023] First wash the empty capillary column with 0.1mol / L HCl solution for about 30min, then rinse with deionized water for 20min, then rinse with 0.1mol / L NaOH for 4h, then rinse with deionized water for 20min, then rinse with methanol for 20min, Blow dry with nitrogen gas.

[0024] 2. Silanization

[0025] Add a mixture of methanol and methacryloxypropyltrimethoxysilane at 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 30min. Blow dry at 70°C with nitrogen.

[0026] 3. In-column synthesis

[0027] Acrylamidopropyl quaternary ammonium propanesulfonic acid internal salt, ethylene glycol dimethacrylate, methacrylate ethylsulfonate, toluene and dodecanol are respectively 12.90%, 16.70%, 0.40%, 34.80%, 35.20%, the amount of the added initiator azobisisobutyronitrile is 0.9% of the amount of the polymer monomer, after the resulting mixture is ultrasonically oscillated at...

Embodiment 2

[0029]Dimethacrylate ethyl quaternary ammonium propane sulfonic acid inner salt, pentaerythritol triacrylate, sodium vinyl sulfonate, cyclohexanol and ethylene glycol are respectively 9.95%, 9.9%, 0.25%, 39.95%, 39.95%, the consumption of added initiator azobisisobutyronitrile (AIBN) is 1.0% of polymer monomer consumption, after the mixture of gained is ultrasonically vibrated at room temperature 15min, nitrogen blowing 10min removes the dissolved oxygen in the mixture, then Inject the mixture into a silanized capillary, seal both ends of the capillary, immerse in a water bath at 60°C, and react for 20 hours. After the reaction is completed, wash the capillary column with methanol mobile phase to remove the residual reagent in the column to obtain zwitterions Electrochromatographic column. In CEC mode, pH 3.0, ion concentration 5mmol / L, acetonitrile: ammonium formate (97 / 3, v / v) buffer solution as mobile phase, applied voltage 20kV, auxiliary pressure 0.3MPa, pump flow rate 0....

Embodiment 3

[0031] Dimethacrylate ethyl quaternary ammonium propane sulfonic acid inner salt, pentaerythritol triacrylate, acryloyloxyethyltrimethylammonium chloride, cyclohexanol and dodecanol were respectively 9.95%, 9.87%, 0.28%, 40.00%, 40.00%, the amount of the added initiator azobisisobutyronitrile is 1.0% of the amount of the polymer monomer, after the resulting mixture is ultrasonically oscillated at room temperature for 15 minutes, blow nitrogen for 10 minutes to remove the dissolved Oxygen, then inject the mixture into the silanized capillary, seal both ends of the capillary, immerse in a water bath at 60°C, and react for 20 hours. After the reaction is completed, wash the capillary column with methanol mobile phase to remove the residual reagent in the column. A zwitterionic electrochromatographic column is obtained. In CEC mode, pH 3.0, ion concentration 20mmol / L, acetonitrile: ammonium formate (80 / 20, v / v) buffer as mobile phase, applied voltage 20kV, auxiliary pressure 0.9MP...

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Abstract

The invention provides a zwitterion electric chromatographic column and a preparation method thereof. The raw material is composed of zwitterion monomer, cross linker, ionic compound monomer, initiating agent and pore-foaming agent; the zwitterion monomer, cross linker and ionic compound monomer are put into a siliconized capillary tube under action of the initiating agent and pore-foaming agent for carrying out polyreaction, so as to obtain the zwitterion electric chromatographic column. The zwitterion electric chromatographic column of the invention can realize that the stationary phase surface on one electric chromatographic column is provided with positive and negative charges simultaneously, can produce strong electroosmotic flow, can solve the problem that non-polar stationary phase is difficult to separate polar substance, has good permeability and is applicable to buffer salt system with wider pH range and high concentration; and plug is not needed to be wound at the two ends of the column during preparation, thus avoiding column filling difficulty. The electric chromatographic monolithic column can select ionic compound monomer with different groups for preparation according to different separation object and can satisfy continuous and fast separation requirement of neutral, acid and alkaline compound, thus the applicable separation object range is wider.

Description

technical field [0001] The invention relates to electrochromatography technology, and more specifically relates to a raw material formula of an amphoteric ion electrochromatographic column and a preparation method thereof. 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. At present, electrochromatographic columns are mainly divided into three types: capillary packed column, capillary open-tube column and capillary monolithic column. Packed columns have been developed rapidly recently, but plugs must be prepared, and plugs usually cause air bubbles, which may cause interruptions in the experimental run; moreover, they are difficult to fill and require high column packing skills. Although the open-tube column has no sealing problem and can o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30
Inventor 谢增鸿王晓春林旭聪
Owner FUZHOU UNIV
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