García-Ruiz C, Martín-Biosca Y, Crego A L, Marina M L
Departamento de Química Analítica, Facultad de Química, Universidad de Alcalá, Alcalá de Henares, Madrid, Spain.
J Chromatogr A. 2001 Feb 23;910(1):157-64. doi: 10.1016/s0021-9673(00)01176-6.
Electrokinetic chromatography with cyclodextrin derivatives (CD-EKC) was used to achieve the rapid enantiomeric separation of chiral polychlorinated biphenyls (PCBs). Thirteen of the 19 chiral PCBs stable at room temperature were individually separated into their two enantiomers by using 2-morpholinoethanesulfonic acid (MES) buffer (pH 6.5) containing carboxymethylated gamma-cyclodextrin (CM-gamma-CD) as pseudostationary phase mixed with beta-cyclodextrin (beta-CD) or permethylated beta-cyclodextrin (PM-beta-CD). Urea was also added to increase the solubility of PCBs and cyclodextrins in the aqueous separation buffer. Several experimental parameters such as the nature, concentration, and pH of the buffer, nature and concentration of the cyclodextrin derivatives used, and the addition of different additives were studied in order to improve the enantiomeric separation. In addition, the effect of some instrumental parameters such as separation temperature and applied voltage was also investigated. PCBs were enantiomerically separated in less than 12 min by using a 50 mM MES buffer (pH 6.5) containing 20 mM CM-gamma-CD, 10 mM beta-CD or 20 mM PM-beta-CD, and 2 M urea at a temperature of 45 degrees C and an applied voltage of 20 kV.
采用环糊精衍生物电动色谱法（CD-EKC）实现了手性多氯联苯（PCBs）的快速对映体分离。通过使用含有羧甲基化γ-环糊精（CM-γ-CD）作为假固定相，并与β-环糊精（β-CD）或全甲基化β-环糊精（PM-β-CD）混合的2-吗啉乙磺酸（MES）缓冲液（pH 6.5），将19种在室温下稳定的手性多氯联苯中的13种分别分离为其两种对映体。还添加了尿素以提高多氯联苯和环糊精在水相分离缓冲液中的溶解度。研究了几个实验参数，如缓冲液的性质、浓度和pH值、所用环糊精衍生物的性质和浓度以及不同添加剂的添加，以改善对映体分离。此外，还研究了一些仪器参数如分离温度和施加电压的影响。通过使用含有20 mM CM-γ-CD、10 mM β-CD或20 mM PM-β-CD以及2 M尿素的50 mM MES缓冲液（pH 6.５），在45℃的温度和20 kV的施加电压下，多氯联苯在不到12分钟内实现了对映体分离。
