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Workflow solution for antidoping analysis including steroids in urine with GC-QqQ and GC-HRAM
by Authors: Petra Gerhards1 , Dr Daniela Cavagnino2 1Thermo Fisher Scientific, Dreieich, Germany, 2 , Inge de Dobbeleer3 . Thermo Fisher Scientific, Rodano (MI), Italy, 3 Interscience BV, Breda, The Netherlands.
The analysis and detection of performance-enhancing drugs in sports competitions can be challenging due to the continuous development of new drugs and the continuous abuse of established and discontinued drugs. This article highlights a complete workflow solution including sample preparation for different doping substances, as well as confirmation and quantification using GC-QqQ and GC-HRAM.
Introduction
Gas chromatography combined with mass spectrometry (GC-MS) is widely used for the analysis of sports doping samples [1]. However, these workflows are often highly complex, involving multiple steps from the collection of samples through to the reporting of results. In animal doping analysis especially, the sample matrix can pose a challenge in terms of sample preparation. Horse urine, for example, is often sent to the testing laboratory in gel form since horse urine forms a gel, when exposed to air, and extensive sample preparation is required before analysis can
take place. Following sample preparation, other considerations such as the use of appropriate glass vials and inert glass liners in the GC instrument, both should be made from borosilicate type I glass [2], must be taken into account to ensure analytes do not adsorb to the free silanol groups on the surface and impact on the accuracy and reliability of results.
Triple quadrupole instruments (QqQ) are traditionally used for MS detection in the analysis of sports doping samples. However, advances in high resolution-accurate mass technology (HRAM) mean that this approach offers several benefits over QqQ detection
methods. This article highlights a complete workflow solution for the analysis of a broad range of drugs in urine using GC-QqQ and GC-HRAM methods. An assessment of detection limits and system robustness for a workflow used by the Rio de Janeiro Doping Control Laboratory (LBCD–LADATEC) during the 2016 Summer Olympic Games is presented.
Experimental Sample preparation and derivatisation
Liquid-liquid extraction (LLE) is widely used for the preparation of urine samples
Figure 1. Thermo Scientific HyperSep C18 SPE protocol.
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