Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

Wadha Abushareeda, Emmanouil Lyris, Suhail Kraiem, Aisha Al Wahaibi, Sameera Alyazidi, Najib Dbes, Arjen Lommen, Michel Nielen, Peter L. Horvatovich, Mohammed Alsayrafi, Costas Georgakopoulos

Research output: Contribution to journalArticleAcademicpeer-review

9 Citations (Scopus)

Abstract

This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World Antidoping Agency (WADA) enlists AAS as prohibited doping agents in sports, and our method has been developed to comply with the qualitative specifications of WADA to be applied for the detection of sports antidoping prohibited substances, mainly for AAS. The method also comprises of the quantitative analysis of the WADA's Athlete Biological Passport (ABP) endogenous steroidal parameters. The applied preparation of urine samples includes enzymatic hydrolysis for the cleavage of the Phase II glucuronide conjugates, generic liquid–liquid extraction and trimethylsilyl (TMS) derivatization steps. Tandem mass spectrometry (MS/MS) acquisition was applied on few selected ions to enhance the specificity and sensitivity of GC/TOF signal of few compounds. The full scan high resolution acquisition of analytical signal, for known and unknown TMS derivatives of AAS provides the antidoping system with a new analytical tool for the detection designer drugs and novel metabolites, which prolongs the AAS detection, after electronic data files’ reprocessing. The current method is complementary to the respective liquid chromatography coupled to mass spectrometry (LC/MS) methodology widely used to detect prohibited molecules in sport, which cannot be efficiently ionized with atmospheric pressure ionization interface.

LanguageEnglish
Pages74-83
JournalJournal of Chromatography. B, Analytical technologies in the biomedical and life sciences
Volume1063
DOIs
Publication statusPublished - 2017

Fingerprint

Testosterone Congeners
Mass Screening
Screening
Gases
Steroids
Urine
Sports
Mass spectrometry
Mass Spectrometry
Doping in Sports
Designer Drugs
Liquid-Liquid Extraction
Impact ionization
Atmospheric Pressure
Enzymatic hydrolysis
Information Storage and Retrieval
Glucuronides
Liquid chromatography
Liquids
Metabolites

Keywords

  • Anabolic steroids
  • Full scan high resolution
  • Gas chromatography
  • Human urine
  • Mass spectrometry

Cite this

Abushareeda, Wadha ; Lyris, Emmanouil ; Kraiem, Suhail ; Wahaibi, Aisha Al ; Alyazidi, Sameera ; Dbes, Najib ; Lommen, Arjen ; Nielen, Michel ; Horvatovich, Peter L. ; Alsayrafi, Mohammed ; Georgakopoulos, Costas. / Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis. In: Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences. 2017 ; Vol. 1063. pp. 74-83.
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abstract = "This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World Antidoping Agency (WADA) enlists AAS as prohibited doping agents in sports, and our method has been developed to comply with the qualitative specifications of WADA to be applied for the detection of sports antidoping prohibited substances, mainly for AAS. The method also comprises of the quantitative analysis of the WADA's Athlete Biological Passport (ABP) endogenous steroidal parameters. The applied preparation of urine samples includes enzymatic hydrolysis for the cleavage of the Phase II glucuronide conjugates, generic liquid–liquid extraction and trimethylsilyl (TMS) derivatization steps. Tandem mass spectrometry (MS/MS) acquisition was applied on few selected ions to enhance the specificity and sensitivity of GC/TOF signal of few compounds. The full scan high resolution acquisition of analytical signal, for known and unknown TMS derivatives of AAS provides the antidoping system with a new analytical tool for the detection designer drugs and novel metabolites, which prolongs the AAS detection, after electronic data files’ reprocessing. The current method is complementary to the respective liquid chromatography coupled to mass spectrometry (LC/MS) methodology widely used to detect prohibited molecules in sport, which cannot be efficiently ionized with atmospheric pressure ionization interface.",
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Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis. / Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas.

In: Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences, Vol. 1063, 2017, p. 74-83.

Research output: Contribution to journalArticleAcademicpeer-review

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AU - Abushareeda, Wadha

AU - Lyris, Emmanouil

AU - Kraiem, Suhail

AU - Wahaibi, Aisha Al

AU - Alyazidi, Sameera

AU - Dbes, Najib

AU - Lommen, Arjen

AU - Nielen, Michel

AU - Horvatovich, Peter L.

AU - Alsayrafi, Mohammed

AU - Georgakopoulos, Costas

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KW - Full scan high resolution

KW - Gas chromatography

KW - Human urine

KW - Mass spectrometry

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M3 - Article

VL - 1063

SP - 74

EP - 83

JO - Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences

T2 - Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences

JF - Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences

SN - 1570-0232

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