%0 Generic %A Arthur, Kayleigh %A James, Lynsey %A Turner, Matthew %A Lindley, Martin %A Reynolds, Jim %A Creaser, Colin %D 2018 %T Supplementary data files for "The determination of salivary oxypurines before and after exercise by combined liquid chromatography-field asymmetric waveform ion mobility spectrometry-time-of-flight mass spectrometry" %U https://repository.lboro.ac.uk/articles/dataset/Supplementary_data_files_for_The_determination_of_salivary_oxypurines_before_and_after_exercise_by_combined_liquid_chromatography-field_asymmetric_waveform_ion_mobility_spectrometry-time-of-flight_mass_spectrometry_/6551114 %R 10.17028/rd.lboro.6551114.v1 %2 https://ndownloader.figshare.com/files/12031340 %K FAIMS %K Differential Mobility Spectrometry %K Mass spectrometry %K Oxidative stress %K Oxypurines %K Xanthine %K Hypoxanthine %K Biochemistry and Cell Biology not elsewhere classified %X Article abstract:
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.
%I Loughborough University