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.

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Version: Final published version
License: CC BY 4.0
Serval ID
serval:BIB_E4C07E3B5A72
Type
Article: article from journal or magazin.
Collection
Publications
Institution
Title
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.
Journal
Analytica chimica acta
Author(s)
Plachká K., Pezzatti J., Musenga A., Nicoli R., Kuuranne T., Rudaz S., Nováková L., Guillarme D.
ISSN
1873-4324 (Electronic)
ISSN-L
0003-2670
Publication state
Published
Issued date
01/04/2021
Peer-reviewed
Oui
Volume
1152
Pages
338257
Language
english
Notes
Publication types: Journal Article
Publication Status: ppublish
Abstract
In this series of two papers, 192 doping agents belonging to the classes of stimulants, narcotics, cannabinoids, diuretics, β2-agonists, β-blockers, anabolic agents, and hormone and metabolic modulators were investigated, with the aim to assess the benefits and limitations of ion mobility spectrometry (IMS) in combination with ultra-high performance liquid chromatography (UHPLC) and high resolution mass spectrometry (HRMS) in anti-doping analysis. In this first part, a generic UHPLC-IM-HRMS method was successfully developed to analyze these 192 doping agents in standard solutions and urine samples, and an exhaustive database including retention times, <sup>TW</sup> CCS <sub>N2</sub> values, and m/z ratios was constructed. Urine samples were analyzed using either a simple "dilute and shoot" procedure or a supported liquid-liquid extraction (SLE) procedure, depending on the physicochemical properties of the compounds and sensitivity criteria established by the World Anti-Doping Agency (WADA) as the minimum required performance levels (MRPL). Then, the precision of the generic UHPLC-IM-HRMS method was assessed as intraday, interday as well as interweek variation of UHPLC retention times and <sup>TW</sup> CCS <sub>N2</sub> values, for which RSD the values were always lower than 2% in urine samples. The possibility to filter MS data using IMS dimension was also investigated, and in average, the application of IMS filtration provided low energy MS spectra with 86% less interfering peaks in both standard and urine samples. Therefore, the filtered MS spectra allowed for an easier interpretation and a lower risk of false positive result interpretations. Finally, IMS also offers additional selectivity to the UHPLC-HRMS enabling to separate isobaric and isomeric substances. Among the selected set of 192 doping agents, there were 30 pairs of isobaric or isomeric compounds, and only two pairs could not be resolved under the developed conditions. This illustrates the potential of adding ion mobility to UHPLC-HRMS in anti-doping analyses.
Keywords
Anabolic Agents, Chromatography, High Pressure Liquid, Doping in Sports, Ion Mobility Spectrometry, Mass Spectrometry, Substance Abuse Detection, Collision cross section, Doping analysis, High resolution mass spectrometry, Ion mobility spectrometry, Ultra-high performance liquid chromatography
Pubmed
Web of science
Open Access
Yes
Create date
03/03/2021 13:15
Last modification date
28/07/2022 6:14
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