Analysis of steroids by on line coupling LC-GC-MS using the TOTAD interface and a fraction collector

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Deutscher übersetzter Titel:Die Analyse von Steroiden mit der Online-LC-GC-MS-Kopplung mittles TOTAD-Schnittstelle und Fraktionssammler
Autor:Toledano, R.; Díaz-Plaza, E.; Blázquez, I.; Vázquez, A.; Villén, J.; Muñoz, J.
Erschienen in:Recent advances in doping analysis (19) : Proceedings of the Manfred-Donike-Workshop ; 29th Cologne Workshop on Dope Analysis ; 13th to 18th February 2011
Veröffentlicht:Köln: Sportverl. Strauß (Verlag), 2011, S. 304-308, Lit.
Format: Literatur (SPOLIT)
Publikationstyp: Sammelwerksbeitrag
Medienart: Elektronische Ressource (Datenträger)
Sprache:Englisch
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Erfassungsnummer:PU201211007423
Quelle:BISp

Abstract

According to the World Antidoping Agency (WADA), the limit of detection for most anabolic steroids must be below 10 ng/mL. In the case of synthetic steroids, the routinely used methods are based in the use of gas chromatography coupled with mass spectrometry (GC-MS). When the potential endogenous steroid misuse should be determined, an analysis by GC hyphenated with combustion isotope ratio mass spectrometry (GC-CIRMS) is mandatory. Attending to the metabolite and the matrix background, to achieve the detection limits required by WADA could be necessary to enhance detection capacities and selectivity of the analytical method. With such aim, some research groups employ off-line consecutive clean-up steps with high performance liquid chromatography (HPLC). The aim of the present work is to achieve these objectives by using the on-line coupling liquid chromatography-gas chromatography with the TOTAD interface. The LC fractions containing the analytes are automatically transferred to a fraction collector and then transferred to the GC. This analytical methodology reduces significantly the sample preparations steps, and provides a better signal/noise ratio because cleaner extracts are obtained. Besides all the LC fraction containing the analytes are transferred to the GC so that a much larger volume is injected. The objective of the present work is to develop a sensitive, robust and reliable analytical method of analysis of steroids in urine, which allows reaching the detection limits required to carry out the efficient control of the misuse of anabolic steroids in sports. Einleitung