Analysis of doping control samples using supercritical fluid chromatography‐tandem mass spectrometry: Ready for routine use

Abstract

Supercritical fluid chromatography is proving to be a good separation and sample preparation tool for various analytical applications and, as such, has gained the attention of the anti‐doping community. Here, the applicability of supercritical fluid chromatography hyphenated to tandem mass spectrometry for routine doping control analysis was tested. A multi‐analyte method was developed to cover 197 drugs and metabolites that are prohibited in sport. More than 1000 samples were analyzed by applying a “dilute and inject” approach after hydrolysis of glucuronide metabolites. Additionally, a comparison with routinely used liquid chromatography‐mass spectrometry was performed with 250 of the 1000 samples and a number of past positive anti‐doping samples. It revealed some features where supercritical fluid chromatography‐tandem mass spectrometry was found to be complementary or advantageous to liquid chromatography‐mass spectrometry for anti‐doping purposes, such as better retention of analytes that are poorly retained in reversed‐phase liquid chromatography. Our results suggest that supercritical fluid chromatography‐tandem mass spectrometry is sensitive (limit of detection <50% relevant minimum required performance level required by the World Anti‐Doping Agency for anti‐doping analysis), reproducible, robust, precise (analytes of interest area coefficient of variation <5%; retention time difference coefficient of variation <1%) and complementary to existing techniques currently used for routine analysis in the World Anti‐Doping Agency accredited laboratories.