Zhou Fan, Zhou Yuxia, Zou Qiaogen, Sun Lili, Wei Ping
College of Food Science and Light Industry, Nanjing Tech University, Nanjing 210009, PR China.
College of Biotechnology and Pharmaceutical Engineering, Nanjing Tech University, Nanjing 210009, PR China.
J Chromatogr Sci. 2015 Sep;53(8):1361-5. doi: 10.1093/chromsci/bmv025. Epub 2015 Mar 29.
Liquid chromatographic separation of mirabegron enantiomers on Chiralpak AY-H, a column coated with amylose tris-(5-chloro-2-methylphenylcarbamate) as a chiral stationary phase, was studied under normal phase conditions. The influence of ethanol content (30-45%) and column temperature (20-40°C) on retention, resolution and separation were evaluated. Apparent thermodynamic parameters deduced from Van't Hoff plots were used to understand chiral separation mechanisms, and the chiral separation was enthalpy driven. The optimized chromatographic conditions were using a mixture solution of n-hexane, ethanol and diethyl amine (55 : 45 : 0.1, v/v/v) as a mobile phase at a flow rate of 1.0 mL/min. The column temperature and UV detector were set at 35°C and 254 nm, respectively. The method was validated to be simple, accuracy, sensitive and robust according to the ICH guidelines, and it was suitable for the routine quality control of mirabegron enantiomers for pharmaceutical industries.
在手性固定相为涂覆有直链淀粉三（5-氯-2-甲基苯基氨基甲酸酯）的Chiralpak AY-H柱上，在正相条件下研究了米拉贝隆对映体的液相色谱分离。评估了乙醇含量（30-45%）和柱温（20-40°C）对保留、分离度和分离的影响。从范特霍夫图推导的表观热力学参数用于理解手性分离机制，且手性分离是由焓驱动的。优化的色谱条件为使用正己烷、乙醇和二乙胺的混合溶液（55 : 45 : 0.1，v/v/v）作为流动相，流速为1.0 mL/min。柱温和紫外检测器分别设置为35°C和254 nm。根据国际协调会议（ICH）指南验证该方法简单、准确、灵敏且稳健，适用于制药行业米拉贝隆对映体的常规质量控制。
