A rapid and sensitive liquid chromatography/positive ion tandem mass spectrometry method for the determination of cimetropium in human plasma by liquid–liquid extraction

摘要: We have developed and validated a simple detection system with high-performance liquid chromatography (HPLC) positive ion electrospray ionization tandem mass spectrometry (ESI-MS/MS) for determining cimetropium levels in human plasma using scopolamine butyl bromide as an internal standard (I.S.). The acquisition was performed the multiple reaction monitoring (MRM) mode, by transitions: m/z 357.9 > 103.1 359.9 butyl-scopolamine. method involves single-step liquid–liquid extraction dichloromethane. analyte chromatographed on YMC C18 reversed-phase chromatographic column isocratic elution 10 mM ammonium formate buffer–methanol (19 : 81, v/v; adjusted to pH 4.0 formic acid). results were linear over studied range (0.2–100 ng ml−1), r2 = 1.0000, total analysis time each run 2 min. Intra- interassay precisions 0.70–8.54% 1.08–4.85%, respectively, intra- accuracies 97.56–108.23% 97.48–103.91%, respectively. lower limit of quantification (LLOQ) 0.2 ml−1. At this concentration, mean 8.54% 4.85%, 97.56% 98.91%, recovery ranged from 62.71 ± 4.06 64.23 2.32%. Cimetropium found be stable samples under typical storage processing conditions. devised assay successfully applied pharmacokinetic study administered single oral dose (150 mg) healthy volunteers. Copyright © 2006 John Wiley & Sons, Ltd.