Preparation method of sterol-based chromatographic stationary phase
A chromatographic stationary phase, sterol technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of increased raw material cost, air humidity sensitivity, expensive catalyst, etc., and achieves low cost, good separation selectivity, and simple preparation process. Effect
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Embodiment 1
[0027] Add 5 grams of silica gel microspheres dried at 120°C for 6 hours to anhydrous toluene solution (150mL) dissolved with 5mmol of 3-isocyanatopropyltrimethoxysilane, and use triethylamine as a catalyst in a nitrogen atmosphere, at 100°C reaction under 8 hours, cooling, suction filtration, washing, vacuum drying to obtain isocyanate-bonded silica gel, and then isocyanate-bonded silica gel and cholesterol (5mmol) in anhydrous toluene (150mL), in nitrogen atmosphere to Pyridine was used as catalyst, reacted at 50°C for 24 hours, cooled, suction filtered, washed, and the obtained solid was dried in a vacuum oven at 40°C for 24 hours to obtain a cholesterol-based silica gel chromatography stationary phase. The stationary phase structure is:
[0028]
Embodiment 2
[0030] Add 6-isocyanatohexyltriethoxysilane (5 mmol) dropwise to a solution of cholesterol (40 mmol) in anhydrous toluene (150 mL), use pyridine as a catalyst in an argon atmosphere, and stir the reaction at 100 ° C for 12 hours, then add 5 grams of silica gel microspheres dried at 160°C for 10 hours to the reaction system, use triethylamine as a catalyst, react at 100°C for 8 hours, cool, filter with suction, wash, and the resulting solid is placed in a vacuum oven Dry at 60°C for 12 hours to obtain a cholesteryl silica gel chromatography stationary phase. The stationary phase structure is:
[0031]
Embodiment 3
[0033] Add 5 grams of zirconia microspheres dried at 120°C for 6 hours in anhydrous toluene solution (150 mL) dissolved with 30 mmol 3-isocyanatopropyltrimethoxysilane, and use triethylamine as a catalyst in a nitrogen atmosphere, at 100 Reaction at ℃ for 8 hours, cooling, suction filtration, washing, and vacuum drying to prepare the isocyanate coupling agent bonded zirconia stationary phase, which was then dispersed with campesterol (30 mmol) and dissolved in anhydrous toluene ( 150mL), in a nitrogen atmosphere, use pyridine as a catalyst, stir and react at 75°C for 12 hours, after cooling, suction filtration, and washing, the resulting solid is dried in a vacuum oven at 60°C for 12 hours to obtain campesterol
[0034]
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