Determination of three nitroimidazoles in rabbit plasma by two-step stacking in capillary zone electrophoresis featuring sweeping and micelle to solvent stacking.

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.

Determination of five nitroimidazole residues in artificial porcine muscle tissue samples by capillary electrophoresis.

A capillary electrophoresis (CE) method with ultraviolet detection has been developed for simultaneous detection and quantification of five nitroimidazoles including benzoylmetronidazole, dimetridazole, metronidazole, ronidazole, and secnidazole in porcine muscles. Nitroimidazoles in samples were extracted by ethyl acetate with subsequent clean-up by a strong cation exchange solid phase extraction column. The clean extracts were subjected to CE separation with optimal experimental conditions: pH 3.0 running buffer containing 25mM sodium phosphate and 0.10mM tetrabutylammonium bromide, 5s hydrodynamic injection at 0.5psi and 28kV separation voltage. The nitroimidazoles could be monitored and detected at 320nm within 18min. The limits of detection were below 1.0µg/kg and limits of quantification were lower than 3.2µg/kg for all nitroimidazoles in the muscle samples. The recoveries and relative standard deviations were 85.4-96.0, 83.5-92.5, 1.3-3.9, and 1.1-4.2%, respectively for the intra-day and inter-day analyses. The proposed CE method has been successfully applied to determine nitroimidazoles in artificial porcine muscle samples with good accuracy and recovery, demonstrating that it has potential for detection and quantification of multi-nitroimidazole residue in real muscle samples.