Norandrosterone analysis by GC/C/IRMS

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Bibliographische Detailangaben
Deutscher übersetzter Titel:Die Analyse von Norandrosteron mittels GC/C/IRMS
Autor:Piper, Thomas; Emery, Caroline; Saugy, Martial
Erschienen in:Recent advances in doping analysis (20) : Proceedings of the Manfred-Donike-Workshop ; 30th Cologne Workshop on Dope Analysis ; 26th February to 2nd March 2012 2. Variante
Veröffentlicht:Köln: Sportverl. Strauß (Verlag), 2012, S. 201-204, Lit.
Format: Literatur (SPOLIT)
Publikationstyp: Sammelwerksbeitrag
Medienart: Gedruckte Ressource
Sprache:Englisch
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Erfassungsnummer:PU201308005825
Quelle:BISp

Abstract

Since nandrolone’s metabolites, 19-norandrosterone (5α-estran-3α-ol-17-one, 19NA) and 19-noretiocholanolone (5β-estran-3α-ol-17-one, 19NE) are known to be also produced endogenously in the human body, the use of GC/C/IRMS (gas chromatography/combustion/isotope ratio mass spectrometry) has become a necessity to detect its abuse in sport. The WADA technical document requests the comparison between δ13C values of 19NA to δ13C of an endogenous reference compound (ERC) for samples showing 19NA concentrations higher than 2 ng/mL in urine. A newly developed method will be presented herein allowing for the detection of 19NA, 19NE, androsterone (5α-androstan-3α-ol-17-one, A), pregnanediol (5β-pregnan-3α,20α-diol, PD) and 16-androstenol (16,(5α)-androsten-3α-ol, 16EN) by GC/C/IRMS. The usual purification steps (solid phase and liquid-liquid extraction, hydrolysis and twofold HPLC purifications) were maintained for sample preparation. However, modifications in the twofold HPLC purification and an additional acetylation step were found to be necessary to improve determination of 19NA and 19NE. The first HPLC purification was performed on a Waters XBridgeTM Shield RP18 column allowing for the complete separation of the ERCs (A, PD and 16EN). Only the fractions containing 19NA and 19NE did necessitate a second HPLC purification with a Waters XBridgeTM RP18 column after acetylation to ensure the purity of compounds. The method was validated and did already demonstrate its benefit to detect the exogenous intake of nandrolone or its precursors in anti-doping samples over the last year. Verf.-Referat