This study focused on the chiral characteristics of methamphetamine seizures in Shanghai for inferring the synthetic pathways of drugs. Capillary electrophoresis coupled to time-of-flight mass spectrometry was used for simultaneous chiral separation of amphetamine-type stimulants and ephedrine, including S(+)-amphetamine/R(-)-amphetamine, S(+)-methamphetamine/R(-)-methamphetamine, (±)-MDA (3,4-methylenedioxyamphetamine), (±)-MDMA (3,4-methylenedioxymethamphetamine), (±)-MDEA (3,4-methylenedioxy-N-ethylamphetamine), d,l-N-ethylamphetamine, methylephedrine/methylpseudoephedrine, and 1S,2R(+)-ephedrine/(-)-ephedrine. The running buffer was 50-mM ammonium formate (pH 2.2 was adjusted by 1-M formic acid) containing 0.26% highly sulfated γ-cyclodextrin as the chiral selector. All enantiomers were well resolved within 40 minutes by capillary electrophoresis at 20 kV in an uncoated fused-silica capillary (50-μm I.D. × 375-μm O.D. × 90-cm length) and detected by micro time-of-flight mass spectrometry. Twenty seized methamphetamine samples were determined by the established method. They were classified into two groups through their chiral characteristics.
A novel capillary zone electrophoresis separation coupled to electro spray ionization time-of-flight mass spectrometry method was developed for the simultaneous analysis of six toxic alkaloids: brucine, strychnine, atropine sulfate, anisodamine hydrobromide, scopolamine hydrobromide and anisodine hydrobromide in human plasma and urine. To obtain optimal sensitivity, a solid-phase extraction method using Oasis MCX cartridges (1 mL, 30 mg; Waters, USA) for the pretreatment of samples was used. All compounds were separated by capillary zone electrophoresis at 25 kV within 12 min in an uncoated fused-silica capillary of 75 μm id × 100 cm and were detected by time-of-flight mass spectrometry. This method was validated with regard to precision, accuracy, sensitivity, linear range, limit of detection (LOD), and limit of quantification (LOQ). In the plasma and urine samples, the linear calibration curves were obtained over the range of 0.50-100 ng/mL. The LOD and LOQ were 0.2-0.5 ng/mL and 0.5-1.0 ng/mL, respectively. The intra- and interday precision was better than 12% and 13%, respectively. Electrophoretic peaks could be identified by mass analysis.
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