Neutral hydrophilically-interacted hybrid silicagel-based monolithic column
A hybrid silica gel, hydrophilic technology, applied in the field of analytical chemistry, can solve the problems of difficult to prepare neutral silica gel monolithic column, difficult to eliminate silanol groups, etc., to meet the requirements of continuous separation, high mechanical strength and uniform internal structure.
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Embodiment 1
[0024] Organic monomer: hydroxyethyl methacrylate, polycage siloxane crosslinking agent: methyl methacrylate based cage oligomeric silsesquioxane, initiator: azobisisobutyronitrile, mixed Porogen: the mass ratio of toluene-dodecanol is prepared according to the following data respectively:
[0025] Column A: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 35.0%, toluene: 34.0%, initiator 1%.
[0026] Column B: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 26.8%, toluene: 42.2%, initiator 1%.
[0027] Column C: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 19.0%, toluene: 50.0%, initiator 1%.
[0028] Column D: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 10.9%, toluene: 59.1%, initiator 1%.
[0029] Column E: polycage siloxane crosslinker 5.1%, organic monomer: 24.9%, dodecyl alcohol: 19.0%, toluene: 50.0%, initiator 1%.
[0030] Column F: polycage siloxane cro...
Embodiment 2
[0034] Apply the monolithic column C prepared above, use acetonitrile:triethylamine phosphate buffer (5mmol / L, pH6.5)=94:6 as the mobile phase, the separation voltage is minus 20 kV, the auxiliary pressure is 1.1MPa, and the pump flow rate is 0.1 Under the condition of mL / min, the neutral amide compounds can achieve baseline separation on the non-charged hydrophilic interaction hybrid silica gel electrochromatographic column, and the elution peaks are as follows: 1. N, N-dimethylformamide; 2. . N, N-Dimethacrylamide; 3. Acrylamide; 4. Acetamide; 5. Formamide; 6. Thiourea.
[0035]Apply the monolithic column C prepared above, use acetonitrile: triethylamine phosphate buffer (2mmol / L, pH 6.5) = 90:10 as the mobile phase, the separation voltage is minus 15 kV, the auxiliary pressure is 3.5MPa, and the pump flow rate is 0.1 mL Under the condition of 1 / min, basic nucleosides and basic polar compounds are effectively separated on the non-charged hydrophilic interaction hybrid silica...
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