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Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath

RATIONALE: Continuously refining and advancing the strategies and methods employed in sports drug testing is critical for efficient doping controls. Besides improving and expanding the spectrum of target analytes, alternative test matrices have warranted in‐depth evaluation as they commonly allow fo...

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Autores principales: Thevis, Mario, Krug, Oliver, Geyer, Hans, Schänzer, Wilhelm
Formato: Online Artículo Texto
Lenguaje:English
Publicado: John Wiley and Sons Inc. 2017
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5519941/
https://www.ncbi.nlm.nih.gov/pubmed/28508503
http://dx.doi.org/10.1002/rcm.7903
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author Thevis, Mario
Krug, Oliver
Geyer, Hans
Schänzer, Wilhelm
author_facet Thevis, Mario
Krug, Oliver
Geyer, Hans
Schänzer, Wilhelm
author_sort Thevis, Mario
collection PubMed
description RATIONALE: Continuously refining and advancing the strategies and methods employed in sports drug testing is critical for efficient doping controls. Besides improving and expanding the spectrum of target analytes, alternative test matrices have warranted in‐depth evaluation as they commonly allow for minimal‐/non‐invasive and non‐intrusive sample collection. In this study, the potential of exhaled breath (EB) as doping control specimen was assessed. METHODS: EB collection devices employing a non‐woven electret‐based air filter unit were used to generate test specimens, simulating a potential future application in doping controls. A multi‐analyte sports drug testing approach configured for a subset of 12 model compounds that represent specific classes of substances prohibited in sports (anabolic agents, hormone and metabolic modulators, stimulants, and beta‐blockers) was established using unispray liquid chromatography/tandem mass spectrometry (LC/MS/MS) and applied to spiked and elimination study EB samples. The test method was characterized concerning specificity, assay imprecision, and limits of detection. RESULTS: The EB collection device allowed for retaining and extracting all selected model compounds from the EB aerosol. Following elution and concentration, LC/MS/MS analysis enabled detection limits between 5 and 100 pg/filter and imprecisions ranging from 3% to 20% for the 12 selected model compounds. By means of EB samples from patients and participants of administration studies, the elimination of relevant compounds and, thus, their traceability in EB for doping control purposes, was investigated. Besides stimulants such as methylhexaneamine and pseudoephedrine, also the anabolic‐androgenic steroid dehydrochloromethyltestosterone, the metabolic modulator meldonium, and the beta‐blocker bisoprolol was detected in exhaled breath. CONCLUSIONS: The EB aerosol has provided a promising proof‐of‐concept suggesting the expansion of this testing strategy as a complement to currently utilized sports drug testing programs.
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spelling pubmed-55199412017-08-03 Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath Thevis, Mario Krug, Oliver Geyer, Hans Schänzer, Wilhelm Rapid Commun Mass Spectrom Research Articles RATIONALE: Continuously refining and advancing the strategies and methods employed in sports drug testing is critical for efficient doping controls. Besides improving and expanding the spectrum of target analytes, alternative test matrices have warranted in‐depth evaluation as they commonly allow for minimal‐/non‐invasive and non‐intrusive sample collection. In this study, the potential of exhaled breath (EB) as doping control specimen was assessed. METHODS: EB collection devices employing a non‐woven electret‐based air filter unit were used to generate test specimens, simulating a potential future application in doping controls. A multi‐analyte sports drug testing approach configured for a subset of 12 model compounds that represent specific classes of substances prohibited in sports (anabolic agents, hormone and metabolic modulators, stimulants, and beta‐blockers) was established using unispray liquid chromatography/tandem mass spectrometry (LC/MS/MS) and applied to spiked and elimination study EB samples. The test method was characterized concerning specificity, assay imprecision, and limits of detection. RESULTS: The EB collection device allowed for retaining and extracting all selected model compounds from the EB aerosol. Following elution and concentration, LC/MS/MS analysis enabled detection limits between 5 and 100 pg/filter and imprecisions ranging from 3% to 20% for the 12 selected model compounds. By means of EB samples from patients and participants of administration studies, the elimination of relevant compounds and, thus, their traceability in EB for doping control purposes, was investigated. Besides stimulants such as methylhexaneamine and pseudoephedrine, also the anabolic‐androgenic steroid dehydrochloromethyltestosterone, the metabolic modulator meldonium, and the beta‐blocker bisoprolol was detected in exhaled breath. CONCLUSIONS: The EB aerosol has provided a promising proof‐of‐concept suggesting the expansion of this testing strategy as a complement to currently utilized sports drug testing programs. John Wiley and Sons Inc. 2017-07-10 2017-08-15 /pmc/articles/PMC5519941/ /pubmed/28508503 http://dx.doi.org/10.1002/rcm.7903 Text en © 2017 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd. This is an open access article under the terms of the Creative Commons Attribution‐NonCommercial‐NoDerivs (http://creativecommons.org/licenses/by-nc-nd/4.0/) License, which permits use and distribution in any medium, provided the original work is properly cited, the use is non‐commercial and no modifications or adaptations are made.
spellingShingle Research Articles
Thevis, Mario
Krug, Oliver
Geyer, Hans
Schänzer, Wilhelm
Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath
title Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath
title_full Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath
title_fullStr Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath
title_full_unstemmed Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath
title_short Expanding analytical options in sports drug testing: Mass spectrometric detection of prohibited substances in exhaled breath
title_sort expanding analytical options in sports drug testing: mass spectrometric detection of prohibited substances in exhaled breath
topic Research Articles
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5519941/
https://www.ncbi.nlm.nih.gov/pubmed/28508503
http://dx.doi.org/10.1002/rcm.7903
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