College of Chemistry and Chemical Engineering, Chemical Synthesis and Pollution Control Key Laboratory of Sichuan Province, China West Normal University, Nanchong 637000, China.
College of Chemistry and Chemical Engineering, Chemical Synthesis and Pollution Control Key Laboratory of Sichuan Province, China West Normal University, Nanchong 637000, China.
J Chromatogr A. 2014 Jan 17;1325:227-33. doi: 10.1016/j.chroma.2013.11.053. Epub 2013 Dec 3.
This study reports a sweeping and micelle to solvent stacking (MSS) method for fast stacking of nitroimidazoles in capillary zone electrophoresis (CZE). The optimal experimental conditions are run buffer of 25mM sodium phosphate (pH 1.5) and 0.50% (v/v) methanol, micellar solution of 30mM sodium dodecyl sulfate, applied voltage of 28kV, and sample and micellar solution injection of 100s. By applying this new on-line preconcentration technique, the nitroimidazoles content can be determined within 9min with the limit of detection (S/N=3) ranging 2.3-3.0ng/mL, which is lower than that of conventional CZE analysis. The proposed MSS technique affords 20-, 12- and 38-fold improvements in sensitivity for the detection of dimetridazole, metronidazole and secnidazole, respectively. The relative standard deviations (RSDs) of intra-day and inter-day are 2.1-3.6% and 2.7-4.6% (n=6), respectively. The recoveries in pretreated rabbit plasma at spiked levels of 5.0-10.0μg/mL are 92.0-101.1% with RSDs lower than 3.4%. The proposed sweeping and MSS-CZE is a highly sensitive method for the detection of nitroimidazoles in biological and clinical samples and has been successfully applied to analyze nitroimidazoles in pretreated rabbit plasma.
本研究报道了一种在毛细管区带电泳（CZE）中快速堆积硝基咪唑的全扫和胶束到溶剂堆积（MSS）方法。最佳实验条件为运行缓冲液为 25mM 磷酸钠（pH1.5）和 0.50%（v/v）甲醇，胶束溶液为 30mM 十二烷基硫酸钠，施加电压为 28kV，样品和胶束溶液进样时间为 100s。通过应用这种新的在线浓缩技术，可以在 9min 内测定硝基咪唑的含量，检测限（S/N=3）范围为 2.3-3.0ng/mL，低于常规 CZE 分析。所提出的 MSS 技术分别使二甲硝咪唑、甲硝唑和塞克硝唑的检测灵敏度提高了 20 倍、12 倍和 38 倍。日内和日间的相对标准偏差（RSD）分别为 2.1-3.6%和 2.7-4.6%（n=6）。在 5.0-10.0μg/mL 加标水平下预处理兔血浆中的回收率为 92.0-101.1%，RSD 低于 3.4%。所提出的全扫和 MSS-CZE 是一种检测生物和临床样品中硝基咪唑的高灵敏度方法，已成功应用于分析预处理兔血浆中的硝基咪唑。
