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Anal Chim Acta. 2015 Jan 1;853:647-59. doi: 10.1016/j.aca.2014.10.007. Epub 2014 Oct 13.

Ultra high performance supercritical fluid chromatography coupled with tandem mass spectrometry for screening of doping agents. II: Analysis of biological samples.

Author information

  • 1Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
  • 2Waters AG, Taefernstrasse 4, 5405 Baden-Daetwill, Switzerland.
  • 3School of Pharmaceutical Sciences, University of Geneva, University of Lausanne, Boulevard D'Yvoy 20, 1211 Geneva 4, Switzerland.
  • 4Swiss Laboratory for Doping Analyses, University Center of Legal Medicine, West Switzerland, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.
  • 5School of Pharmaceutical Sciences, University of Geneva, University of Lausanne, Boulevard D'Yvoy 20, 1211 Geneva 4, Switzerland. Electronic address: davy.guillarme@unige.ch.

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.

KEYWORDS:

Biological samples; Doping agents; Matrix effects; Ultra high performance liquid chromatography; Ultra high performance supercritical fluid chromatography; Urine

PMID:
25467514
DOI:
10.1016/j.aca.2014.10.007
[PubMed - indexed for MEDLINE]
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