Department of Chemistry, Yeungnam University, Gyeongsan 712-749, South Korea.
J Chromatogr A. 2011 Aug 5;1218(31):5369-73. doi: 10.1016/j.chroma.2011.06.002. Epub 2011 Jun 12.
Cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) is an excellent chiral selector for enantioseparation of a wide variety of chiral compounds. The monolithic chiral columns are becoming popular in liquid chromatography and capillary electrochromatography. In this work, we present the fast separation of chiral β-blockers on a CDMPC-modified zirconia monolithic column by capillary electrochromatography (CEC). The porous zirconia monolithic capillary column was prepared by using the sol-gel technology and then zirconia surface modified with CDMPC. The enantioseparations were performed in reversed-phase (RP) eluents of a phosphate solution (pH 4.4) modified with acetonitrile or alcohol. The enantioseparations of a set of eight chiral β-blockers were achieved in less than one minute. Influences of the applied voltage, column temperature, concentration of acetonitrile and the type of alcohol as the organic modifier in the mobile phase, and sample injection time on enantioseparation were investigated. CEC separations at the applied voltage of 10 kV and 15 °C in the ACN-modified mobile phase provided the best resolutions for the analytes studied. Run-to-run and day-to-day repeatabilities of the column in the RP-CEC separation were less than 1 and 2%, respectively.
三(3,5-二甲基苯基氨基甲酸酯)纤维素(CDMPC)是一种出色的手性选择剂,可用于分离各种手性化合物。整体式手性柱在液相色谱和毛细管电色谱中越来越受欢迎。在这项工作中,我们通过毛细管电色谱(CEC)在手性 CDMPC 修饰的氧化锆整体柱上快速分离手性β受体阻滞剂。多孔氧化锆整体毛细管柱是通过溶胶-凝胶技术制备的,然后用 CDMPC 对氧化锆表面进行修饰。在磷酸盐溶液(pH 4.4)中添加乙腈或醇的反相(RP)洗脱液中进行对映体分离。在不到一分钟的时间内,实现了一组八种手性β受体阻滞剂的对映体分离。考察了施加电压,柱温,乙腈浓度以及流动相中醇的类型以及样品进样时间对对映体分离的影响。在 ACN 改性流动相中施加 10 kV 和 15°C 的 CEC 分离可提供研究分析物的最佳分辨率。在 RP-CEC 分离中,柱的运行间和日间重复性分别小于 1%和 2%。