Doping control analysis of 13 steroids and structural-like analytes in human urine using Quadrupole-Orbitrap LC-MS/MS...

Anabolic androgenic steroids (AASs) and structural-like substances are commonly prohibited substances found in doping control studies that can be difficult to accurately detect. In the present study, 11 AASs and 2 structural-like substances that are commonly detected were examined. Currently, such analytes are detected using low resolution GC-MS/MS or LC-MS/MS, with detection not always possible. Herein, the high resolution Quadrupole-Orbitrap liquid chromatography-tandem mass spectrometry LC-MS/MS system Q Exactive was utilized to increase the specificity. This approach was then combined for the first time with parallel reaction monitoring (PRM) during the screening procedure. The results confirmed high specificity, with the LODs of all 13 analytes being at least 25-fold lower than corresponding MRPLs as defined by WADA. Furthermore, the extraction recoveries were above 70% and the intra- and inter-day precisions were lower than 15%. This approach was successfully applied to analyze over 10,000 samples with no false-positive or false-negative results, thus suggesting that Quadrupole-Orbitrap LC-MS/MS when combined with PRM is an effective method for doping control analysis.