Serrano Juan Manuel, Silva Manuel
Department of Analytical Chemistry, University of Cordoba, Cordoba, Spain.
Electrophoresis. 2007 Sep;28(18):3242-9. doi: 10.1002/elps.200700016.
This study dealt with the potential of MEKC with LIF detection involving derivatization with sulfoindocyanine succinimidyl ester (Cy5) for the separation and determination of beta-lactam antibiotics (ampicillin, amoxicillin, cephradine, and cephalexin) in environmental water samples. Water samples of 50 mL were enriched by SPE by passage through a weak base-cation Amberlite(R) IRA-93 exchange column. SDS micelles play important roles in the whole analytical process by improving the yield (sensitivity) and the kinetics of the labeling reaction, the elution of the retained antibiotics from the SPE preconcentration system and the electrophoretic resolution of their Cy5-derivatives. The optimum procedure includes a derivatization step of the antibiotics at 25 degrees C for 10 min and direct injection for MEKC analysis, which is conducted within about 15 min using 15 mM SDS in the running buffer (35 mM sodium borate at pH 9.3). LODs from 30 to 45 ng/L and RSDs (within-day precision) from 3.5 to 5.9% were obtained for the antibiotics in water samples with average recoveries ranging from 96.4 to 99.4%. These results indicate that the method proposed is a straightforward and sensitive tool for the determination of these antibiotics in environmental water samples providing similar quantitative results to those using more expensive equipment like LC-electrospray MS/MS.
本研究探讨了采用磺基吲哚菁琥珀酰亚胺酯(Cy5)衍生化的胶束电动毛细管色谱-激光诱导荧光检测法(MEKC-LIF)分离和测定环境水样中β-内酰胺类抗生素(氨苄西林、阿莫西林、头孢拉定和头孢氨苄)的潜力。50 mL水样通过弱碱性阳离子Amberlite® IRA-93交换柱进行固相萃取(SPE)富集。十二烷基硫酸钠(SDS)胶束在整个分析过程中发挥着重要作用,它可提高标记反应的产率(灵敏度)和动力学、促进固相萃取预浓缩系统中保留抗生素的洗脱以及其Cy5衍生物的电泳分离。最佳分析流程包括在25℃下对抗生素进行10分钟的衍生化步骤,然后直接进样进行MEKC分析,分析在约15分钟内完成,运行缓冲液为含15 mM SDS的35 mM硼酸钠(pH 9.3)。水样中抗生素的检测限为30至45 ng/L,日内精密度相对标准偏差(RSD)为3.5%至5.9%,平均回收率为96.4%至99.4%。这些结果表明,所提出的方法是一种直接且灵敏的工具,可用于测定环境水样中的这些抗生素,其定量结果与使用更昂贵设备(如液相色谱-电喷雾串联质谱仪(LC-electrospray MS/MS))获得的结果相似。