Zhang Panliang, Sun Genlin, Tang Kewen, Yang Weijun, Sui Guoqing, Zhou Congshan
Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Yueyang, China.
J Sep Sci. 2014 Dec;37(23):3443-50. doi: 10.1002/jssc.201400812. Epub 2014 Oct 13.
Recycling high-speed counter-current chromatography was successfully applied to the preparative separation of oxybutynin enantiomers. The two-phase solvent system consisted of n-hexane, methyl tert-butyl ether, and 0.1 mol/L phosphate buffer solution (pH = 5.0) with the volume ratio of 6:4:10. Hydroxypropyl-β-cyclodextrin was employed as the chiral selector. The influence of factors on the chiral separation process, including the concentration of chiral selector, the equilibrium temperature, the pH value of the aqueous phase were investigated. Under optimum separation conditions, 15 mg of oxybutynin racemate was separated with the purities of both the enantiomers over 96.5% determined by high-performance liquid chromatography. Recovery for the target compounds reached 80-82% yielding 6.00 mg of (R)-oxybutynin and 6.15 mg of (S)-oxybutynin. Technical details for recycling elution mode were discussed.
循环高速逆流色谱法成功应用于奥昔布宁对映体的制备分离。两相溶剂体系由正己烷、甲基叔丁基醚和0.1 mol/L磷酸盐缓冲溶液（pH = 5.0）组成，体积比为6:4:10。羟丙基-β-环糊精用作手性选择剂。研究了手性选择剂浓度、平衡温度、水相pH值等因素对手性分离过程的影响。在最佳分离条件下，分离了15 mg奥昔布宁外消旋体，通过高效液相色谱法测定，两种对映体的纯度均超过96.5%。目标化合物的回收率达到80 - 82%，得到6.00 mg的（R）-奥昔布宁和6.15 mg的（S）-奥昔布宁。讨论了循环洗脱模式的技术细节。
