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Urine analysis concerning xenon for doping control purposes
Author(s) -
Thevis Mario,
Piper Thomas,
Geyer Hans,
Schaefer Maximilian S.,
Schneemann Julia,
Kienbaum Peter,
Schänzer Wilhelm
Publication year - 2014
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.7080
Subject(s) - xenon , chemistry , chromatography , urine , detection limit , analyte , isotopes of xenon , gas chromatography , biochemistry , organic chemistry
RATIONALE On September 1 st 2014, a modified Prohibited List as established by the World Anti‐Doping Agency (WADA) became effective featuring xenon as a banned substance categorized as hypoxia‐inducible factor (HIF) activator. Consequently, the analysis of xenon from commonly provided doping control specimens such as blood and urine is desirable, and first data on the determination of xenon from urine in the context of human sports drug testing, are presented. METHODS In accordance to earlier studies utilizing plasma as doping control matrix, urine was enriched to saturation with xenon, sequentially diluted, and the target analyte was detected as supported by the internal standard d 6 ‐cyclohexanone by means of gas chromatography/triple quadrupole mass spectrometry (GC/MS/MS) using headspace injection. Three major xenon isotopes at m/z 128.9, 130.9 and 131.9 were targeted in (pseudo) selected reaction monitoring mode enabling the unambiguous identification of the prohibited substance. Assay characteristics including limit of detection (LOD), intraday/interday precision, and specificity as well as analyte recovery under different storage conditions were determined. Proof‐of‐concept data were generated by applying the established method to urine samples collected from five patients before, during and after (up to 48 h) xenon‐based general anesthesia. RESULTS Xenon was traceable in enriched human urine samples down to the detection limit of approximately 0.5 nmol/mL. The intraday and interday imprecision values of the method were found below 25%, and specificity was demonstrated by analyzing 20 different blank urine samples that corroborated the fitness‐for‐purpose of the analytical approach to unequivocally detect xenon at non‐physiological concentrations in human urine. The patients' urine specimens returned 'xenon‐positive' test results up to 40 h post‐anesthesia, indicating the limits of the expected doping control detection window. CONCLUSIONS Since xenon has been considered a prohibited substance according to WADA regulations in September 2014, its analysis from common specimens of routine sports drug testing is desirable. In previous studies, its traceability in whole blood and plasma was shown, and herein a complementary approach utilizing doping control urine samples for the GC/MS/MS analysis of xenon was reported. Copyright © 2014 John Wiley & Sons, Ltd.