摘要
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 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 △△G°, △△H°, and △△S° have been estimated by the separation factor(α) at a given temperature, where the terms △△G° △△H°, and △△S° 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.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
1999年第2期166-170,共5页
Acta Chimica Sinica
基金
国家自然科学基金(29673052)
关键词
HPLC
手性
固定相
曲美布汀
拆分
对映体分离
chiral stationary phase
resolution of enantiomer of pharmaceutical
HPLC
