title: An improved gas chromatography screening method for doping substances using triple quadrupole mass spectrometry, with an emphasis on quality assurance.
abstract: A GC-QqQ-MS method was developed for the detection of over 150 compounds from different classes (steroids, narcotics, stimulants, β-blockers, β-2-agonists and hormone antagonists) in a qualitative way. In the quantitative part, the traditional steroid profile with the most important endogenous steroids is expanded with six minor metabolites, which further improves the detection and identification of endogenous steroid abuse. In addition to these, norandrosterone, salbutamol and the major metabolite of cannabis are also quantified. Methods developed for anti-doping purposes should be subjected to the highest level of quality. Here, the addition of a combination of (deuterated) internal standards allows for an accurate quality control of every single step of the methodology: hydrolysis efficiency, derivatization efficiency and microbiological degradation are monitored in every single sample. Additionally, special attention is paid to the relationships between parameters indicating degradation by micro-organisms and the reliability of the steroid profile. The impact of the degradation is studied by evaluation of the quantities and percentages of 5α-androstane-3,17-dione and 5β-androstane-3,17-dione. The concept of measurement uncertainty was introduced for the evaluation of relative abundances of mass-to-charge ratios and the obtained ranges were compared with the World Anti-Doping Agency regulations on tolerance windows for relative ion intensities. The results indicate that the approaches are similar.
authors.affiliation: Doping Control Laboratory, Ghent University, Technologiepark 30, B-9052, Zwijnaarde, Belgium. Nik.DeBrabanter@UGent.be
authors.forename: Nik
authors.initials: N
authors.lastname: De Brabanter
authors.forename: Wim
authors.initials: W
authors.lastname: Van Gansbeke
authors.forename: Lore
authors.initials: L
authors.lastname: Geldof
authors.forename: Peter
authors.initials: P
authors.lastname: Van Eenoo
mesh_terms: D004300:Doping in Sports; D004355:Drug Stability; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods* / Q000592:standards*; D006801:Humans; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism / Q000652:urine*; D011786:Quality Control; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013048:Specimen Handling; D015813:Substance Abuse Detection / Q000379:methods* / Q000592:standards*; D014556:Urine / Q000382:microbiology
chemical_list: D004364:Pharmaceutical Preparations