Analytical Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad, India.
J Sep Sci. 2012 Oct;35(20):2671-7. doi: 10.1002/jssc.201200410. Epub 2012 Sep 4.
Liquid chromatographic separation of stereoisomers of darunavir on Chiralpak AD-H, a column containing the stationary phase coated with amylose tris(3,5-dimethylphenylcarbamate) as a chiral selector, was studied under normal-phase conditions at different temperatures between 20 and 50°C. The effect of quality and quantity of different polar organic modifiers viz: methanol, ethanol, 1-propanol, and 2-propanol in the mobile phase as well as column temperature on retention, separation, and resolution was investigated and optimized. The optimum separation was accomplished using a mobile phase composed of n-hexane/ethanol/diethyl amine (80:20:0.1 v/v/v) at 40°C. Apparent thermodynamic parameters ΔH(0) and ΔS* were derived from the Van't Hoff plots (lnk' versus 1/T) and used to explain the strength of interactions between the stereoisomers and amylose tris(3,5-dimethylphenylcarbamate) coated chiral stationary phase.
手性固定相包含涂覆有直链淀粉三（3,5-二甲基苯基氨基甲酸酯）作为手性选择体的阿立哌唑 AD-H 柱上的达鲁那韦对映异构体的液相色谱分离在 20 至 50°C 之间的不同温度下的正相条件下进行了研究。考察并优化了流动相中不同质量和数量的极性有机溶剂（甲醇、乙醇、1-丙醇和 2-丙醇）以及柱温对保留、分离和分辨率的影响。使用由正己烷/乙醇/二乙胺（80:20:0.1v/v/v）组成的流动相在 40°C 下实现了最佳分离。从 Van't Hoff 图（lnk' 对 1/T）推导出表观热力学参数ΔH(0)和ΔS*，并用于解释手性异构体和涂覆有直链淀粉三（3,5-二甲基苯基氨基甲酸酯）的手性固定相之间相互作用的强度。
