新型β-环糊精手性固定相的合成及其对贝凡洛尔的拆分

摘要

A novelβ-cyclodextrin derivative was synthesized and chemically immobilized onto the surface of γ-mercaptopropyl-functionalized silica gel step by step. The products in each step were purified and characterized, and the structure had been confirmed. This chiral stationary phase ( CSP) bonded on sili-ca gel was packed into a column (250 mm × 4. 6 mm × 5 μm) using a slurry-packing procedure. When mobile phase was methanol -25 mmol/L KH2PO4(60/40,V/V), the flow rate was 0. 5 mL/min, the column temperature was 25 ℃ and the detection wavelength was 259 nm, bevantolol enantiomers were completely separated.%采用分步法合成一种新型β-环糊精衍生物并化学键合到γ-巯丙基硅胶上.在合成中的每步均对产物进行纯化及表征,并确证化合物的结构,采用湿法装柱将自制的手性固定相装填成色谱柱(250 mm ×4.6 mm ×5μm).在高效液相色谱中,流动相为甲醇-25 mmol/L KH2PO4(60/40,V/V),流速为0.5 mL/min,检测波长为259 nm,色谱柱温为25℃时,此新型β-环糊精衍生物键合硅胶手性固定相对贝凡洛尔表现出良好的分离特性.