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Title: The determination of salivary oxypurines before and after exercise by combined liquid chromatography-field asymmetric waveform ion mobility spectrometry-time-of-flight mass spectrometry
Authors: Arthur, Kayleigh L.
Wilson, Lynsey S.
Turner, Matthew A.
Lindley, Martin R.
Reynolds, James C.
Creaser, Colin S.
Keywords: FAIMS
Differential mobility spectrometry
Mass spectrometry
Oxidative stress
Oxypurines
Xanthine
Hypoxanthine
Issue Date: 2018
Publisher: © Springer
Citation: ARTHUR, K.L. ...et al., 2018. The determination of salivary oxypurines before and after exercise by combined liquid chromatography-field asymmetric waveform ion mobility spectrometry-time-of-flight mass spectrometry. International Journal for Ion Mobility Spectrometry, 21(3), pp 87–95.
Abstract: © 2018 Springer-Verlag GmbH Germany, part of Springer Nature A method combining field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry (LC-FAIMS-MS) has been developed for the analysis of the oxypurine compounds hypoxanthine (HX) and xanthine (XA) in saliva. Separation of the oxypurines from interfering matrix components was investigated using FAIMS-MS. The selected FAIMS parameters were then applied to the rapid LC-FAIMS-MS analysis of HX and XA using a short chromatographic separation method (7 min). A comparison of the LC-MS method with and without FAIMS applied, resulted in improved discrimination from saliva matrix interferences and improved chromatographic peak integration for both HX and XA using a FAIMS separation. A quantitative evaluation of the LC-FAIMS-MS method was performed giving limits of detection of 2.0 ng mL −1 for HX and 1.8 ng mL −1 for XA, and limits of quantification of 6.6 ng mL −1 for HX and 6.0 ng mL −1 for XA. The developed LC-FAIMS-MS method was applied to the targeted analysis of the oxypurine metabolites in saliva collected from healthy male athletes (n = 11) before and after exercise designed to induce oxidative stress; post-exercise collection time-points included immediately after exercise, one hour and twenty-four hours’ post-exercise. The salivary concentrations of both HX and XA were lower after physical exercise, compared to the pre-exercise (rest) concentrations and returned to approximately pre-exercise levels after twenty-four hours. The method reported has the potential for monitoring the salivary oxypurines, HX and XA, as biomarkers of oxidative stress and in other clinical applications.
Description: This paper is in closed access until 19th May 2019.
Sponsor: This work was supported by Owlstone Ltd. and Loughborough University.
Version: Accepted for publication
DOI: 10.1007/s12127-018-0232-4
URI: https://dspace.lboro.ac.uk/2134/33435
Publisher Link: https://doi.org/10.1007/s12127-018-0232-4
Related Resource: https://doi.org/10.17028/rd.lboro.6551114
ISSN: 1435-6163
Appears in Collections:Closed Access (Sport, Exercise and Health Sciences)
Closed Access (Chemistry)

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