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
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[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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