Introduction of HPLC/orbitrap mass spectrometry as screening method for doping control

Abstract

A new doping control screening method has been developed, for the analysis of doping agents in human urine, using HPLC/orbitrap with in‐source collision‐induced dissociation and atmospheric pressure chemical ionization. The developed method allows the detection of 29 compounds, including agents with antiestrogenic activity, β₂ agonists, exogenous anabolic steroids, and other anabolic agents. The mass accuracy of this method is better at 2 ppm using an external reference. The detection limit for all compounds tested was better than 100 pg/ml. The recoveries of most analytes were above 70%. The measured median repeatability values for doping agents included in the method at concentrations of 1 and 10 ng/ml were 21 and 17%, respectively. The relative standard deviation (RSD) of the intraday precision (n = 6) ranged from RSD = 16–22%, whereas the interday precision (n = 18), ranged from RSD = 17–26%, depending on the solute concentration investigated. Copyright © 2008 John Wiley & Sons, Ltd.