Comparison of gas chromatography/quadrupole time‐of‐flight and quadrupole Orbitrap mass spectrometry in anti‐doping analysis: I. Detection of anabolic‐androgenic steroids

• Published in: Rapid communications in mass spectrometry Vol. 32; no. 23; pp. 2055 - 2064
• Main Authors: Abushareeda, Wadha, Tienstra, Marc, Lommen, Arjen, Blokland, Marco, Sterk, Saskia, Kraiem, Suhail, Horvatovich, Peter, Nielen, Michel, Al‐Maadheed, Muhammad, Georgakopoulos, Costas
• Format: Journal Article
• Language: English
• Published: England Wiley Subscription Services, Inc 15-12-2018
• Subjects: Androgens - urine; BU Contaminanten & Toxines; BU Contaminants & Toxins; BU Dierbehandelingsmiddelen; BU Veterinary Drugs; Chromatography; Doping; Doping in Sports - prevention & control; Gas chromatography; Gas Chromatography-Mass Spectrometry - methods; Humans; Laboratorium voor Organische chemie; Laboratory for Organic Chemistry; Limit of Detection; Mass spectrometry; Mathematical analysis; Monsteradministratie & Coördinatie; Organic Chemistry; Organische Chemie; Platforms; Quadrupoles; RIKILT - Business unit Contaminanten & Toxines; RIKILT - Business unit Contaminants & Toxins; RIKILT - Business unit Dierbehandelingsmiddelen; RIKILT - Monsteradministratie & Coördinatie; RIKILT - Sample Administration and Coordination; Scientific imaging; Screening; Spectroscopy; Steroids; Steroids - urine; Substance Abuse Detection - methods; Tandem Mass Spectrometry - methods; Testing laboratories; Testosterone Congeners - urine; Urine; VLAG
• ISSN: 0951-4198; 1097-0231
• DOI: 10.1002/rcm.8281

Rationale
The World Anti‐Doping Agency (WADA) encourages drug‐testing laboratories to develop screening methods that can detect as many doping substances as possible in urine. The use of full‐scan high‐resolution acquisition (FS/HR) with gas chromatography/mass spectrometry (GC/MS) for the detection of known and unknown trimethylsilyl (TMS) derivatives of anabolic‐androgenic steroids (AAS) provides anti‐doping testing bodies with a new analytical tool.
Methods
The AAS were extracted from urine samples by generic liquid–liquid extraction, after enzymatic hydrolysis, and TMS derivatization. The extracted urine was analyzed by GC/Q‐TOF and GC/Q‐Orbitrap to compare the performance of the two instrument types for the detection of 46 AAS in human urine. The quantitation of endogenous anabolic steroids and the ability of the two analytical platforms to comply with the requirements for testing as part of the WADA Athlete Biological Passport (ABP) were also assessed.
Results
The data presented show that the analytical performance for both instruments complies with the WADA specifications. The limits of detection (LODs) for both instruments are well below the WADA 50% Minimum Required Performance Levels. The mass errors in the current study for the GC/Q‐Orbitrap platform are lower than those obtained for the GC/Q‐TOF instrument.
Conclusions
The data presented herein proved that both molecular profiling platforms can be used for antidoping screening. The mass accuracies are excellent in both instruments; however, the GC/Q‐Orbitrap performs better as it provides higher resolution than the GC/Q‐TOF platform.