Ion mobility-high resolution mass spectrometry in anti-doping analysis. Part I: Implementation of a screening method with the assessment of a library of substances prohibited in sports

In this series of two papers, 192 doping agents belonging to the classes stimulants, narcotics, cannabinoids, diuretics, β2-agonists, β-blockers, anabolic agents, and hormone metabolic modulators were investigated, with aim assess benefits limitations ion mobility spectrometry (IMS) in combination ultra-high performance liquid chromatography (UHPLC) high resolution mass (HRMS) anti-doping analysis. first part, a generic UHPLC-IM-HRMS method was successfully developed analyze these standard solutions urine samples, an exhaustive database including retention times, TWCCSN2 values, m/z ratios constructed. Urine samples analyzed using either simple “dilute shoot” procedure or supported liquid-liquid extraction (SLE) procedure, depending on physicochemical properties compounds sensitivity criteria established by World Anti-Doping Agency (WADA) as minimum required levels (MRPL). Then, precision assessed intraday, interday well interweek variation UHPLC times for which RSD values always lower than 2% samples. The possibility filter MS data IMS dimension also average, application filtration provided low energy spectra 86% less interfering peaks both Therefore, filtered allowed easier interpretation risk false positive result interpretations. Finally, offers additional selectivity UHPLC-HRMS enabling separate isobaric isomeric substances. Among selected set there 30 pairs compounds, only could not be resolved under conditions. This illustrates potential adding analyses.