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.

Department of Analytical Chemistry Faculty of Pharmacy Charles University Prague Heyrovského 1203 500 05 Hradec Králové Czech Republic

School of Pharmaceutical Sciences University of Geneva University of Lausanne Boulevard D'Yvoy 20 1211 Geneva 4 Switzerland

Swiss Laboratory for Doping Analyses University Center of Legal Medicine West Switzerland Chemin des Croisettes 22 1066 Epalinges Switzerland

Waters AG Taefernstrasse 4 5405 Baden Daetwill Switzerland

Citace poskytuje Crossref.org

Ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry for antidoping analyses: Assessment of the inter-laboratory reproducibility with urine samples

Quantification of karrikins in smoke water using ultra-high performance liquid chromatography-tandem mass spectrometry