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

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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,… Click to show full 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 MS/MS 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 analysed applying a "dilute and inject" approach after hydrolysis of glucuronide metabolites. Additionally, a comparison with routinely used LC-MS 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 MS/MS was found to be complementary or advantageous to LC-MS for anti-doping purposes, such as better retention of analytes that are poorly retained in reversed-phase LC. Our results suggest that supercritical fluid chromatography tandem mass spectrometry is sensitive (LOD <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. This article is protected by copyright. All rights reserved.

Keywords: anti doping; supercritical fluid; analysis; fluid chromatography

Journal Title: Journal of separation science
Year Published: 2023

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