title: Screening and confirmation analysis of stimulants, narcotics and beta-adrenergic agents in human urine by hydrophilic interaction liquid chromatography coupled to mass spectrometry.
abstract: The chromatographic behaviour of 44 polar compounds (23 beta-adrenergic agents, 11 stimulants, 4 narcotics and 6 phenolalkylamines) included in the list of prohibited substances and methods of the World Anti-Doping Agency, has been investigated under hydrophilic interaction liquid chromatography conditions by application of different mobile phase compositions (percentage of the organic solvent, type and amount of mobile phase additive and ionic strength) and column temperatures. Detection of analytes was performed by a triple quadrupole mass spectrometer in positive ionization mode and selected reaction monitoring acquisition mode after liquid/liquid extraction. Data collected using as stationary phase type-B silica materials from different producers, showed that the best chromatographic conditions in terms of peak shape, selectivity and chromatographic retention were obtained using an initial percentage of acetonitrile of 90%, a column temperature of 35 °C, a mobile phase pH of 4.5 and ammonium acetate (5 mM) and acetic acid (0.1%) as mobile phase additives. The selected chromatographic conditions were used to develop screening and confirmation analytical procedures to detect polar compounds in human urine for antidoping purpose. The developed methods were validated in terms of specificity, matrix effect, linearity, precision, accuracy, sensitivity, robustness and repeatability of retention times and relative ion abundances. Such methods offer attractive alternatives and considerable advantages over traditional approaches especially for the analysis of the phenolalkylamines.
authors: Laboratorio Antidoping, Federazione Medico Sportiva Italiana, Largo Giulio Onesti 1, 00197 Rome, Italy.
authors: Monica
authors: M
authors: Mazzarino
authors: Ilaria
authors: I
authors: Fiacco
authors: Xavier
authors: X
authors: de la Torre
authors: Francesco
authors: F
authors: Botrè
mesh_terms: D000085:Acetates; D019342:Acetic Acid; D000097:Acetonitriles; D000318:Adrenergic beta-Agonists / Q000652:urine*; D000588:Amines / Q000652:urine; D000697:Central Nervous System Stimulants / Q000652:urine*; D002853:Chromatography, Liquid / Q000379:methods*; D004300:Doping in Sports; D006801:Humans; D057927:Hydrophobic and Hydrophilic Interactions; D013058:Mass Spectrometry / Q000379:methods*; D009294:Narcotics / Q000652:urine*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D015813:Substance Abuse Detection / Q000379:methods; D013696:Temperature
chemical_list: D000085:Acetates; D000097:Acetonitriles; D000318:Adrenergic beta-Agonists; D000588:Amines; D000697:Central Nervous System Stimulants; D009294:Narcotics; D019342:Acetic Acid; C018824:ammonium acetate; C032159:acetonitrile