Flow Innovation-Research for Science and Technology Laboratories (First Labs), Mahidol University, Bangkok, Thailand.
Electrophoresis. 2012 Jan;33(2):388-94. doi: 10.1002/elps.201100370. Epub 2011 Dec 13.
CE methods with capacitively coupled contactless conductivity detection (C(4)D) were developed for the enantiomeric separation of the following stimulants: amphetamine (AP), methamphetamine (MA), ephedrine (EP), pseudoephedrine (PE), norephedrine (NE) and norpseudoephedrine (NPE). Acetic acid (pH 2.5 and 2.8) was found to be the optimal background electrolyte for the CE-C(4)D system. The chiral selectors, carboxymethyl-β-cyclodextrin (CMBCD), heptakis(2,6-di-O-methyl)-β-cyclodextrin (DMBCD) and chiral crown ether (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (18C6H(4)), were investigated for their enantioseparation properties in the BGE. The use of either a single or a combination of two chiral selectors was chosen to obtain optimal condition of enantiomeric selectivity. Enantiomeric separation of AP and MA was achieved using the single chiral selector CMBCD and (hydroxypropyl)methyl cellulose (HPMC) as the modifier. A combination of the two chiral selectors, CMBCD and DMBCD and HPMC as the modifier, was required for enantiomeric separation of EP and PE. In addition, a combination of DMBCD and 18C6H(4) was successfully applied for the enantiomeric separation of NE and NPE. The detection limits of the enantiomers were found to be in the range of 2.3-5.7 μmol/L. Good precisions of migration time and peak area were obtained. The developed CE-C(4)D method was successfully applied to urine samples of athletes for the identification of enantiomers of the detected stimulants.
CE 方法与电容耦合非接触式电导检测(C(4)D)相结合,用于以下兴奋剂对映体的分离:苯丙胺(AP)、甲基苯丙胺(MA)、麻黄碱(EP)、伪麻黄碱(PE)、去甲麻黄碱(NE)和去甲伪麻黄碱(NPE)。研究发现,乙酸(pH 2.5 和 2.8)是 CE-C(4)D 体系的最佳背景电解质。手性选择剂羧甲基-β-环糊精(CMBCD)、七(2,6-二-O-甲基)-β-环糊精(DMBCD)和手性冠醚(+)-(18-冠-6)-2,3,11,12-四羧酸(18C6H(4))被用于研究它们在 BGE 中的对映体分离性能。选择使用单一或两种手性选择剂的组合来获得最佳的对映选择性条件。使用单一手性选择剂 CMBCD 和(羟丙基)甲基纤维素(HPMC)作为修饰剂实现了 AP 和 MA 的对映体分离。EP 和 PE 的对映体分离需要两种手性选择剂 CMBCD 和 DMBCD 以及 HPMC 作为修饰剂的组合。此外,DMBCD 和 18C6H(4)的组合成功应用于 NE 和 NPE 的对映体分离。对映体的检测限发现处于 2.3-5.7 μmol/L 的范围内。迁移时间和峰面积的精密度良好。所开发的 CE-C(4)D 方法成功应用于运动员尿液样本中,用于鉴定检测到的兴奋剂的对映体。