A fast, comprehensive screening method for doping agents in urine by gas chromatography–triple quadrupole mass spectrometry

Improved sensitivity by use of gas chromatography—positive chemical ionization triple quadrupole mass spectrometry for the analysis of drug related substances

“…In all these cases the most abundant form is monitored. As mentioned in our previous publications, the derivatization efficiency and reproducibility is controlled by monitoring the monoTMS/bisTMS androsterone ratio in every sample [17,20].…”

“…Acetonitrile and methyl tert-butyl ether were from Biosolve (Valkenswaard, The Netherlands) and ammoniumiodide (NH 4 I) and dodecane were from Sigma Aldrich (Bornem, Belgium). The origin of all the reference standards is described in detail in our previous work [17,20].…”

“…The mass spectrometer was in both cases programmed in MS1Scan mode (scan range m/z 40-800) or MRM mode. Details of the transitions and collision energies can be found in Table 1 and reference [17].…”

“…In routine analysis, this results in a substantial decrease of urine samples that exhibit endogenous steroid concentrations outside the linear range that otherwise would have to be reanalyzed (after dilution). If the linear range is lower (48-4800 ng/ml, as in the previously used and published EI method) about 25-30% of the routine samples has to be reanalyzed to match WADA criteria, which is an obvious economical disadvantage [16,17]. In effect, the increased sensitivity allows the set up of a balanced screening method that meets the requirements for both quantitative and qualitative compounds: sufficient capacity and resolution and a high sensitivity with a short analysis time.…”

“…In 2011, a fast GC-(EI-)MS/MS method for doping substances in urine was published [17]. Thirteen endogenous steroids could be quantified and over 140 exogenous doping substances could be detected qualitatively in accordance with the minimum required performance levels (MRPLs) of the World Anti-Doping Agency (WADA) [18].…”