High resolution full scan liquid chromatography mass spectrometry comprehensive screening in sports antidoping urine analysis

Wadha Abushareeda, Ariadni Vonaparti, Khadija Al Saad, Moneera Almansoori, Mbarka Meloug, Amal Saleh, Rodrigo Aguilera, Yiannis Angelis, Peter L. Horvatovich, Arjen Lommen, Mohammed Alsayrafi, Costas Georgakopoulos*

*Corresponding author for this work

Research output: Contribution to journalArticleAcademicpeer-review

20 Citations (Scopus)

Abstract

The aim of this paper is to present the development and validation of a high-resolution full scan (HR-FS) electrospray ionization (ESI) liquid chromatography coupled to quadrupole Orbitrap mass spectrometer (LC/Q/Orbitrap MS) platform for the screening of prohibited substances in human urine according to World Antidoping Agency (WADA) requirements. The method was also validated for quantitative analysis of six endogenous steroids (epitestosterone, testosterone, 5α-dihydrotestosterone, dehydroepiandrosterone, androsterone and etiocholanolone) in their intact sulfates form. The sample preparation comprised a combination of a hydrolyzed urine liquid–liquid extraction and the dilute & shoot addition of original urine in the extracted aliquot. The HR-FS MS acquisition mode with Polarity Switching was applied in combination of the Quadrupole-Orbitrap mass filter. The HR-FS acquisition of analytical signal, for known and unknown small molecules, allows the inclusion of all analytes detectable with LC–MS for antidoping investigations to identify the use of known or novel prohibited substances and metabolites after electronic data files’ reprocessing. The method has been validated to be fit-for-purpose for the antidoping analysis.
Original languageEnglish
Pages (from-to)10-24
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume151
DOIs
Publication statusPublished - 20 Mar 2018

Keywords

  • Full scan high-resolution
  • Human urine
  • Liquid chromatography
  • Mass spectrometry
  • Small molecule prohibited substances
  • Sulfo-conjugate steroids

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    Abushareeda, W., Vonaparti, A., Saad, K. A., Almansoori, M., Meloug, M., Saleh, A., Aguilera, R., Angelis, Y., Horvatovich, P. L., Lommen, A., Alsayrafi, M., & Georgakopoulos, C. (2018). High resolution full scan liquid chromatography mass spectrometry comprehensive screening in sports antidoping urine analysis. Journal of Pharmaceutical and Biomedical Analysis, 151, 10-24. https://doi.org/10.1016/j.jpba.2017.12.025