David Cowan

Supercritical fluid chromatography‐mass spectrometry (SFC‐MS) has proved to be a beneficial tool for sample analysis for a wide variety of compounds and, as such, has recently gained the attention of the anti‐doping community. We have tested the applicability of SFC‐MS for routine doping control analysing approximately 3 × 1000 identical anti‐doping samples utilising SFC‐MS instruments from three different vendors: Agilent Technologies, Waters Corporation and Shimadzu Corporation. A ‘dilute and inject’ approach either without or after hydrolysis of glucuronide metabolites was applied. Most of the compounds included in our study demonstrated excellent chromatography, whereas some showed co‐elution with endogenous interferences requiring MS discrimination. Retention times typically were very stable within batches (%CV ≤ 0.5%), although this appeared to be analyte and column dependent. Chromatographic peak shape was good (symmetrical) and stable over the period of the testing without any change of column. Our results suggest that SFC‐MS is a sensitive, reproducible and robust analytical tool ready to be used in anti‐doping laboratories alongside the currently applied techniques such as gas and liquid chromatography coupled to mass spectrometry. Even if instruments are designed slightly differently, all three setups demonstrated their fitness for the purpose in anti‐doping testing.