Sun Genlin, Tang Kewen, Zhang Panliang, Yang Weijun, Sui Guoqing
College of Chemistry and Chemical Engineering, Hunan University, Changsha, China.
J Sep Sci. 2014 Jul;37(14):1736-41. doi: 10.1002/jssc.201400281. Epub 2014 Jun 5.
High-speed countercurrent chromatography (HSCCC) combined with biphasic chiral recognition was successfully applied to the resolution of phenylsuccinic acid enantiomers. D-Isobutyl tartrate and hydroxypropyl-β-cyclodextrin were employed as lipophilic and hydrophilic selectors dissolved in the organic stationary phase and aqueous mobile phase, respectively. The two-phase solvent system was made up of n-hexane/methyl tert-butyl ether/water (0.5:1.5:2, v/v/v). Impacts of the type and concentration of chiral selectors, the pH value of the aqueous phase solution as well as the temperature on the separation efficiency were investigated. By means of preparative HSCCC, pure enantiomer was obtained by separating 810 mg of racemate with a purity >99.5% and a recovery rate between 82 and 85%. The experimental results indicate that biphasic recognition HSCCC provide a promising means for efficient separation of racemates.
高速逆流色谱（HSCCC）结合双相手性识别技术成功应用于苯基琥珀酸对映体的拆分。分别以D-酒石酸二异丁酯和羟丙基-β-环糊精作为亲脂性和亲水性选择剂，将其溶解于有机固定相和水相流动相中。两相溶剂体系由正己烷/甲基叔丁基醚/水（0.5:1.5:2，v/v/v）组成。考察了手性选择剂的种类和浓度、水相溶液的pH值以及温度对分离效率的影响。通过制备型HSCCC，分离810 mg外消旋体，得到纯度>99.5%、回收率在82%至85%之间的纯对映体。实验结果表明，双相识别HSCCC为外消旋体的高效分离提供了一种有前景的方法。
