药物曲美布汀对映体在涂敷三(4-甲基苯甲酸)纤维素酯手性固定 相上的HPLC分 离

涂敷15%(wt)三(4-甲基苯甲酸)纤维素酯于大孔硅胶担体上,制备手性固定相,以此手性固定相作填料,湿法装填液相色谱柱,直接分离(±)-曲美布汀对映体。确定对映体在固定相与洗脱液之间分配的自由能变之差值、焓变之差值和熵变之差值,考察洗脱液正己烷-异丙醇(v/v)中异丙醇含量在色谱分离对映体性能方面的影响。当洗脱液中异丙醇含量增加时,对映体的容量因子逐渐降低,分离因子变化不大,分离度逐渐降低。

The separation of 3, 4, 5-trimethoxybenzoic acid 2-(dimethylamino)-2- phenylbutyl ester enantiomers on a cellulose tris(4-methylbenzoate) high-performance liquid chromatographic chiral stationary phase

The cellulose tris(4-methylbenzoate) (CTMB)-coated silanized gel was slurry-packed in stainless steel columns. the complete resolution of racemic 2-(dimethylamino)-2-phenylbutyl ester of 3, 4, 5- trimethoxybenzoic acid by CTMB-CSP (CSP=Chiral Stationary Phase has been achieved. Effects of the 2-propanol content in mobile phase and different temperature on capacity factor, separation factor, resolution in the separation of 2-(dimethylamino)-2-phenylbutyl ester of 3, 4, 5-trimethoxybenzoic acid enantiomers were studied. The thermodynamic parameters ΔΔGⅲ, ΔΔHⅲ, and ΔΔSⅲ have been estimated by the separation factor (α) at a given temperature, where the terms ΔΔGⅲ, ΔΔHⅲ, and ΔΔSⅲ represent the differences in the total free energy, enthalpy, and entropy differences, respectively. It was found that CTMB-CSP is sensitive to small changes in temperature. The resolution increased when the temperature was decreased in the 24.9℃ to 45.0℃ range.