Preparation method of glycosyl-functionalized imidazole ionic liquid stationary phase
An ionic liquid and imidazole-based technology, which is applied in the field of preparation of glycosyl-functionalized imidazole-based ionic liquid stationary phase, can solve the problems of single target analyte and limited stability, and achieve high separation efficiency, resistance to organic solvents, Apply a wide range of effects
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Embodiment 1
[0033] Such as figure 1 Shown, a kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase, operate according to the following steps:
[0034] Step 1: Heat 3 g of silica gel with concentrated hydrochloric acid to reflux for 4 hours, wash with water until neutral, and dry in vacuum at 120°C for 6 hours to obtain surface-activated silica gel;
[0035] Step 2: Weigh 50mM D-gluconolactone and N-(3-aminopropyl)imidazole in equivalent moles, dissolve the two in 250ml ethanol at the same time, heat to 80°C, reflux for 24h, and place in the refrigerator Set aside for one day to obtain N-imidazolyl propyl glucamide;
[0036] Step 3: Mix and dissolve 6mM N-imidazolyl propyl glucamide and equimolar 3-isocyanatopropyl trimethoxysilane in 50ml ethanol, reflux for 2 days, carry out methylation reaction, and generate N-trimethyl Silylpropyl-N'-glucamidopropylimidazolium + iodide ion;
[0037] Step 4: Add magnets to the solution obtained in Step 3 f...
Embodiment 2
[0040] A preparation method of a glycosyl functionalized imidazole-type ionic liquid stationary phase is carried out according to the following steps:
[0041] Step 1: Heat 3 g of silica gel with concentrated hydrochloric acid to reflux for 4 hours, wash with water until neutral, and dry in vacuum at 120°C for 6 hours to obtain surface-activated silica gel;
[0042] Step 2: Weigh 50mM D-gluconolactone and N-(3-aminopropyl)imidazole in equivalent moles, dissolve the two in 250ml ethanol at the same time, heat to 80°C, reflux for 24h, and place in the refrigerator Set aside for one day to obtain N-imidazolyl propyl glucamide;
[0043]Step 3: Weigh 6mM N-imidazolyl propyl glucamide and equimolar 3-isocyanate propyltrimethoxysilane, mix and dissolve in 50ml ethanol, and reflux for 3 days to generate N-trimethylsilyl propyl -N'-glucamidopropyl imidazole + iodide ion;
[0044] Step 4: Add magnets to the solution obtained in Step 3 for mechanical stirring, and add 20ml of methanol ...
Embodiment 3
[0047] Such as figure 1 Shown, a kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase, operate according to the following steps:
[0048] Step 1: Heat 2.5 g of silica gel with concentrated hydrochloric acid to reflux for 5 hours, wash with water until neutral, and dry in vacuum at 120°C for 6 hours to obtain surface-activated silica gel;
[0049] Step 2: Weigh 40mM D-gluconolactone and N-(3-aminopropyl)imidazole in equivalent moles, dissolve the two in 200ml ethanol at the same time, heat to 75°C, reflux for 24h, and place in the refrigerator Set aside for one day to obtain N-imidazolyl propyl glucamide;
[0050] Step 3: Weigh 8mM N-imidazolyl propyl glucamide and equimolar 3-isocyanate propyl trimethoxysilane, mix and dissolve in 60ml ethanol, and reflux for 2 days to generate N-trimethylsilyl propyl -N'-glucamidopropyl imidazole + iodide ion;
[0051] Step 4: Add magnets to the solution obtained in Step 3 for mechanical stirri...
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