High-sensitivity analysis of anionic sulfonamides by capillary electrophoresis using a synergistic stacking approach

A synergistic stacking approach whereby field-enhanced sample injection and micelle-to-solvent stacking in capillary zone electrophoresis are combined has been developed and has been applied to the separation and quantification of anionic sulfonamides. Electrokinetic injection of the sample in a low conductivity alkaline diluent was performed for 90 s at −15 kV. Micelle-to-solvent stacking was then undertaken by hydrodynamic injection of micellar cetyltrimethylammonium bromide solution prior to the electrokinetic injection of sample that also contained 50% methanol. This combined stacking approach, when compared to a typical hydrostatic injection, provided improvements in peak height and corrected peak area in the range of 397-1024 and 758-1246, respectively. Limits of quantification in the range of 0.01-0.03 μg/mL were obtained for sulfamerazine, sulfamethazine and sulfamethizole and were sufficient for the determination of these analytes in river water. The percentage recovery and accuracy values obtained for a fortified river water sample that had been subjected to sample preparation by evaporation and reconstitution with diluent were 74-135%. Intra-day and inter-day repeatabilities for migration time, peak height, and corrected peak area were in the range 0.5-5.0% (percentage relative standard deviation, n = 8) and these relatively low values were attributed to the use of a stable capillary coating established by the successive multiple ionic-polymer layer technique.