Screening method for selected doping substances by gas chromatography - triple quadrupole mass spectrometry : reaching minimum required performance limits

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Deutscher übersetzter Titel:Screening-Methoden für ausgewählte Doping-Substanzen durch Gaschromatograhie - Triple-Quadrupol-Massenspektrometerie : das Erreichen minimal erforderlicher Nachweisgrenzen
Autor:Marcos, J.; Segura, J.; Ventura, R.; Garrostas, L.
Erschienen in:Recent advances in doping analysis (21) : Proceedings of the Manfred-Donike-Workshop ; 31th Cologne Workshop on Dope Analysis ; 24th February to 1st March 2013
Veröffentlicht:Köln: Sportverl. Strauß (Verlag), 2013, S. 98-102, Lit.
Format: Literatur (SPOLIT)
Publikationstyp: Sammelwerksbeitrag
Medienart: Elektronische Ressource (Datenträger)
Sprache:Englisch
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Erfassungsnummer:PU201408007425
Quelle:BISp

Abstract

The minimum performance limits for many forbidden substances have been modified in the latest version of the World Anti-Doping Agency (WADA) technical document (TD2O13MRPL). As a consequence, antidoping laboratories have to re-evaluate their routine screening methods in order to prove that they are capable of reaching these limits. This is not always feasible with the commonly employed GC-MS and LC-MS/MS methodologies. Thus, laboratories may take advantage of recently introduced instruments for some compounds. In particular, the use of gas chromatography coupled to triple quadrupole instruments (GC-QqQ) is becoming an essential tool. In the Barcelona antidoping laboratory, the screening strategy has introduced GC-QqQ in order to cope with the new MRPL for selected analytes which show limitations either when analyzed by GC-MS or LC-MS/MS. The aim of this work was to develop and validate a GC-QqQ method able of reaching the new MRPL for some doping agents. The list of analytes includes anabolic steroids and other doping agents. The final selected reaction monitoring (SRM) GC-QqQ method contains two specific transitions per compound. The method was tested by extracting ten blank urine samples, six samples fortified at low concentration, six at high concentration, and six samples spiked after extraction procedure for recovery calculations. Without modifying the work-up procedure employed for the screening of anabolic steroids by GC-MS, 27 compounds were successfully validated at the new MRPL with adequate intra-assay precisions. No interferences were detected confirming the specificity of the method. Verf.-Referat