title: Ultra high performance supercritical fluid chromatography coupled with tandem mass spectrometry for screening of doping agents. II: Analysis of biological samples.
abstract: The potential and applicability of UHPSFC-MS/MS for anti-doping screening in urine samples were tested for the first time. For this purpose, a group of 110 doping agents with diverse physicochemical properties was analyzed using two separation techniques, namely UHPLC-MS/MS and UHPSFC-MS/MS in both ESI+ and ESI- modes. The two approaches were compared in terms of selectivity, sensitivity, linearity and matrix effects. As expected, very diverse retentions and selectivities were obtained in UHPLC and UHPSFC, proving a good complementarity of these analytical strategies. In both conditions, acceptable peak shapes and MS detection capabilities were obtained within 7 min analysis time, enabling the application of these two methods for screening purposes. Method sensitivity was found comparable for 46% of tested compounds, while higher sensitivity was observed for 21% of tested compounds in UHPLC-MS/MS and for 32% in UHPSFC-MS/MS. The latter demonstrated a lower susceptibility to matrix effects, which were mostly observed as signal suppression. In the case of UHPLC-MS/MS, more serious matrix effects were observed, leading typically to signal enhancement and the matrix effect was also concentration dependent, i.e., more significant matrix effects occurred at the lowest concentrations.
authors.affiliation: Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
authors.forename: Lucie
authors.initials: L
authors.lastname: Nováková
authors.affiliation: Waters AG, Taefernstrasse 4, 5405 Baden-Daetwill, Switzerland.
authors.forename: Marco
authors.initials: M
authors.lastname: Rentsch
authors.affiliation: School of Pharmaceutical Sciences, University of Geneva, University of Lausanne, Boulevard D'Yvoy 20, 1211 Geneva 4, Switzerland.
authors.forename: Alexandre
authors.initials: A
authors.lastname: Grand-Guillaume Perrenoud
authors.affiliation: Swiss Laboratory for Doping Analyses, University Center of Legal Medicine, West Switzerland, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.
authors.forename: Raul
authors.initials: R
authors.lastname: Nicoli
authors.affiliation: Swiss Laboratory for Doping Analyses, University Center of Legal Medicine, West Switzerland, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.
authors.forename: Martial
authors.initials: M
authors.lastname: Saugy
authors.affiliation: School of Pharmaceutical Sciences, University of Geneva, University of Lausanne, Boulevard D'Yvoy 20, 1211 Geneva 4, Switzerland.
authors.forename: Jean-Luc
authors.initials: JL
authors.lastname: Veuthey
authors.affiliation: School of Pharmaceutical Sciences, University of Geneva, University of Lausanne, Boulevard D'Yvoy 20, 1211 Geneva 4, Switzerland. Electronic address: davy.guillarme@unige.ch.
authors.forename: Davy
authors.initials: D
authors.lastname: Guillarme
mesh_terms: D000779:Anesthetics, Local / Q000032:analysis / Q000592:standards; D000928:Antidepressive Agents / Q000032:analysis / Q000592:standards; D002851:Chromatography, High Pressure Liquid / Q000592:standards; D025924:Chromatography, Supercritical Fluid / Q000592:standards; D004300:Doping in Sports; D006801:Humans; D007477:Ions / Q000737:chemistry; D058573:Performance-Enhancing Substances / Q000032:analysis* / Q000592:standards; D012015:Reference Standards; D053719:Tandem Mass Spectrometry / Q000592:standards
chemical_list: D000779:Anesthetics, Local; D000928:Antidepressive Agents; D007477:Ions; D058573:Performance-Enhancing Substances
keywords: Biological samples; Doping agents; Matrix effects; Ultra high performance liquid chromatography; Ultra high performance supercritical fluid chromatography; Urine