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Detection of formestane abuse by mass spectrometric techniques
Author(s) -
Torre Xavier,
Colamonici Cristiana,
Curcio Davide,
Jardines Daniel,
Molaioni Francesco,
Parr Maria Kristina,
Botrè Francesco
Publication year - 2014
Publication title -
drug testing and analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.065
H-Index - 54
eISSN - 1942-7611
pISSN - 1942-7603
DOI - 10.1002/dta.1759
Subject(s) - chemistry , chromatography , mass spectrometry , gas chromatography–mass spectrometry , derivatization , gas chromatography
Formestane (4‐hydroxy‐androstenedione) is an aromatase inhibitor prohibited in sports and included, since 2004, in the list of prohibited substances updated yearly by the World Anti‐Doping Agency (WADA). Since the endogenous production of formestane has been described, it is mandatory for the anti‐doping laboratories to use isotope ratio mass spectrometry (IRMS) to establish the exogenous origin before issuing an adverse analytical finding. The described IRMS methods for formestane detection are time‐consuming, requiring usually two consecutive liquid chromatographic sample purifications in order to have final extracts of adequate purity before the mass spectrometric analysis. After establishing a procedure for the determination of the origin of formestane by IRMS without the need of derivatization, and integrated in the overall analytical strategy of the laboratory for pseudo‐endogenous steroids, a mass spectrometric analysis by gas chromatography–mass spectrometry (GC‐MS) and gas chromatography‐tandem mass spectrometry (GC‐MS/MS) of formestane metabolites was carried out in order to investigate whether other biomarkers of formestane abuse could be integrated in order to avoid time‐consuming and expensive IRMS confirmations for formestane. From the metabolic studies performed, the inclusion of 3β,4α‐dihydroxy‐5α‐androstan‐17‐one (4α‐hydroxy‐epiandosterone) in the routine GC‐MS procedures has demonstrated to be diagnostic in order to reduce the number of unnecessary confirmations of the endogenous origin of formestane. Copyright © 2014 John Wiley & Sons, Ltd.