A metal ion-immobilized modified silica gel monolithic column and its preparation method
A silica monolithic column and metal ion technology, applied in the field of analytical chemistry, can solve problems such as loss, and achieve the effects of increased mass transfer rate, large specific surface area, and strong acid and alkali resistance
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Embodiment 1
[0027] 1) Rinse the empty capillary column with 0.1mol / L hydrochloric acid solution for 30 minutes, 1.0 mol / L NaOH solution for 3 hours, deionized water for 15 minutes, and methanol for 15 minutes, and then dry it with nitrogen at 50°C;
[0028] 2) Add a mixture of methanol and methacryloxypropyltrimethoxysilane at a volume ratio of 1:1 to the capillary tube treated in step 1), react at 60°C for 12 hours, then rinse with methanol for 15 minutes, and then Blow dry with nitrogen at 50~70°C;
[0029] 3) The metal ion-containing functional monomer zinc dimethacrylate monomer, cross-linking agent octamethacrylate cage polysilsesquioxane, toluene, dodecanol, N, N-dimethylformamide and initiator azobisisobutyronitrile were mixed, ultrasonically oscillated for 10-15 minutes, nitrogen was purged for 10 minutes, and then injected into the capillary treated in step 2), both ends were sealed and immersed in 60°C React in a water bath for 16 hours. After the reaction is completed, wash th...
Embodiment 3
[0036] The monolithic column B prepared in Example 1 was used, with acetonitrile-phosphate buffer (30.0mmol / L, pH 3.0) at a volume ratio of 70:30 as the mobile phase, the separation voltage was −10 kV, the pump pressure was 500 psi, and the flow rate was 0.1mL / min, capillary electrochromatographic separation of 4 kinds of polar nucleoside bases, the results are shown in figure 2 .
[0037] figure 2 The elution peak 1 is uridine, the elution peak 2 is adenosine, the elution peak 3 is guanine, the elution peak 4 is cytosine, and the elution peak 5 is cytidine. Depend on figure 2 It can be seen that under the hydrophilic effect provided by the monolithic column and the electron coordination effect of the zinc ion-nucleoside base amino group, each polar nucleoside base is effectively separated.
Embodiment 4
[0039] Using the monolithic column B prepared in Example 1, acetonitrile-phosphate buffer (40.0mmol / L, pH 5.0) with a volume ratio of 75:25 was used as the mobile phase, the separation voltage was -10 kV, the pump pressure was 500psi, and the flow rate was 0.1mL / min, 4 kinds of polar enkephalin substances were separated by capillary electrochromatography, the results are shown in image 3 .
[0040] image 3The elution peak 0 is N, N-dimethylformamide, the elution peak 1 is Tyr-Gly-Gly-Phe-Met, the elution peak 2 is Tyr-Gly-Gly-Phe, and the elution peak 3 is Tyr -Gly, elution peak 4 is Tyr-Gly-Gly. Depend on image 3 It can be seen that under the hydrophilic effect provided by the monolithic column and the electron coordination effect of the zinc ion-enkephalin peptide bond, each polar enkephalin is effectively separated.
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