BAIDOO, E. E. K., CLENCH, M. R., SMITH, R. F. and TETLER, L. W. (2003). Determination of nicotine and its metabolites in urine by solid-phase extraction and sample stacking capillary electrophoresis-mass spectrometry. Journal of chromatography B, 796 (2), 303-313.
The combination of capillary electrophoresis (CE) and mass spectrometry (MS) with solid-phase extraction (SPE) has been used for the identification of nicotine and eight of its metabolites in urine. The recovery of cotinine from cotinine-spiked urine, by C18 SPE, was found to be 98%. Smokers urine (200 ml) was preconcentrated 200-fold via SPE prior to analysis. The sample stacking mode of CE, when compared to capillary zone electrophoresis, was shown to improve peak efficiency by 132-fold. The combination of hydrodynamic and electrokinetic injection was studied with sample stacking/CE/MS. The on-column limits of detection (LOD) of nicotine and cotinine, by this technique, were found to be 0.11 and 2.25 μg/ml, respectively. Hence, LODs of nicotine and cotinine in urine after 200-fold preconcentration were 0.55 and 11.25 ng/ml, respectively.
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