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化学学报
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化学学报 ›› 1999, Vol. 57 ›› Issue (2): 166-170. 上一篇    下一篇

研究论文

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

王来来;吕士杰;高平;李树本   

  1. 中国科学院兰州化学物理研究所羰基合成与选择氧化国家重点实;验室
  • 发布日期:1999-02-15

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

Wang Lailai;Lu Shijie;Gao Ping;Li Shuben   

  • Published:1999-02-15

PDF

414

被引次数

5

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。

关键词: 手征性, 固定相, 高速液体色谱, 对映体, 异丙醇, 纤维素酯, 分离, 药物

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.

Key words: CHIRALITY, STATIONARY PHASE, HIGH SPEED LIQUID CHROMATOGRAPHY, ENANTIOMORPH, ISOPROPANOL, CELLULOSE ESTERS, SEPARATION, DRUGS

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