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
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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 inner salt, ethylene glycol dimethacrylate, ethyl methacrylate, 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 room temper...
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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