Correlation of Androstenedione and Testosterone Measurements by LC–MS/MS and GC‐qTOF

This work assessed the correlation between the measurements of A4 and T in serum obtained by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-high resolution mass spectrometry (GC-qTOF). Both procedures using LC-MS/MS and GC-qTOF instruments were validated using the 6PLUS1Multilevel Serum Calibrator Set MassChrom Steroid Panel 2. Positive and negative quality controls and human serum samples were used to check the correlation between these two approaches. Correlation between T and A4 concentrations measured by GC-qTOF and LC-MS/MS was found to be adequate when correlation tests, regression analysis, and Bland-Altman tests were applied. Although the LOQs required in the WADA technical documents for both analytes were not reached under the described assay conditions, the advantages provided by high-resolution mass spectrometry for the detection and quantification of steroids should not be discarded. The technical document for the identification of substances using mass spectrometry instruments does not include acceptance criteria when using HRMS platforms but should be considered due to the recent increase in its use in anti-doping laboratories.