Development and validation of a fast gas chromatography combustion isotope ratio mass spectrometry method for the detection of epiandrosterone sulfate in urine

AbstractIn doping control, to confirm the exogenous origin of exogenously administered anabolic androgenic steroids (AAS), a gas chromatography combustion isotope ratio mass spectrometry (GC ‐C‐IRMS) analysis is performed. Recently published work suggests epiandrosterone sulfate (EpiAS) as a promising IRMS target compound for the detection of AAS, capable of prolonging the detection window. However, EpiAS is only excreted in urine in its sulfoconjugated form while all other IRMS tar get compounds are excreted glucuronidated, meaning that EpiAS cannot be incorporated in the existing IRMS methods. A separate extensive sample preparation needs to be performed on this compound with a different hydrolysis and extraction procedure and a different liquid chromatography (LC) clean‐up .The current work presents a new, fast and easy to implement EpiAS IRMS method. The approach was based on the direct GC analysis of non ‐hydrolysed EpiAS, making the solid phase extraction, hydrolysis and acetylation step redundant. Sample preparation consisted of a simple liquid liquid extraction, followed by LC fraction collection.A population study was performed to check the compliance with the criteria drafted by the World Anti ‐Doping Agency (WADA). To verify the applicability of the developed approach, the method was applied to the samples of four administration studies (i.e., dehydroepiandrosterone (DHEA), testosterone gel (T gel), androstenedione (ADION) and intramuscular testosterone u...
Source: Drug Testing and Analysis - Category: Drugs & Pharmacology Authors: Tags: RESEARCH ARTICLE Source Type: research