Interpretation of high resolution and tandem MS data: two relevant cases of anabolic steroid metabolites at pg level in blood and urine

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Deutscher übersetzter Titel:Interpretation von Daten der Hochaufloesungs- und Tandem-Massenspektrometrie: zwei relevante Faelle des Nachweises von Metaboliten anaboler Steroide auf pg-Ebene im Blut und Urin
Autor:Thieme, D.; Große, Joachim; Lang, R.; Mueller, R.K.; Wahl, A.
Herausgeber:Schänzer, Wilhelm; Geyer, Hans; Gotzmann, Andrea; Marek-Engelke, U.
Erschienen in:Recent advances in doping analysis (5) : Proceedings of the Manfred Donike Workshop ; 15th Cologne Workshop on Dope Analysis ; 23rd to 28th February 1997
Veröffentlicht:Köln: Sport u. Buch Strauß (Verlag), 1998, 1998. S. 157-168, Lit., Lit.
Format: Literatur (SPOLIT)
Publikationstyp: Sammelwerksbeitrag
Medienart: Gedruckte Ressource
Sprache:Englisch
ISBN:3890010164
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Erfassungsnummer:PU199805301841
Quelle:BISp

Abstract des Autors

The identification and confirmation of metabolites of methandienone in urine and of stanozolol in blood and cerebrospinal fluid was possible by application of HRMS and especially of tandem MS. Detection limits of 100pg/ml could be achieved for confirmation of the substances in several cases, where certain hints allowed to direct the analysis to few target substances. Detection and confirmation of two long term metabolites of methandienone were preferably carried out by MS/MS, mainly due to a higher number of undisturbed fragmentation reactions available. The application of an HPLC clean-up permits the reduction of background and the formation of different derivatives for each metabolite. The confirmation of 3'-OH-stanozolol in biological post mortem materials was possible after formation of per-TMS derivatives by HRMS or MS/MS. Only this metabolite could be detected in all specimen (blood, cerebrospinal fluid, liver) after hydrolysis. Signals in HRMS or MS/MS proved to have a much higher uniqueness, compared to conventional MS and allow to improve peak to noise ratios. But the possibility of interferences becomes more relevant with lower abundant signals for lower concentration ranges. The final decision whether peaks or spectra can be considered as 'undisturbed' and enable the identification of substances beyond reasonable doubts are still arbitrary. Verf.-Referat