Validation of an Ultra-Sensitive Detection Method for Steroid Esters in Plasma for Doping Analysis Using Positive Chemical Ionization GC-MS/MS

Validation of an Ultra-Sensitive Detection Method for Steroid Esters in Plasma for Doping Analysis Using Positive Chemical Ionization GC-MS/MS / Pieter Van Renterghem, Wouter Viaene, Wim Van Gansbeke, Juliana Barrabin, Michele Iannone, Michael Polet, Guy T'Sjoen, Koen Deventer, Peter Van Eenoo. - (Journal of Chromatography B 1141 (2020) 122026 (15 March)).
- PMID: 32109748
- DOI: 10.1016/j.jchromb.2020.122026


Abstract

The standard approach to detect misuse with testosterone in sport is based on the determination and evaluation of the urinary steroid profile followed by the confirmation of atypical profiles using isotope ratio mass spectrometry. The detection capacity of these methods can be attenuated by confounding factors or testosterone preparations with endogenous isotopic fingerprints. An alternative detection method for misuse of an endogenous steroid in sports is the direct detection of the administered steroid ester present in most preparations. Thus unambiguous proof for doping misuse can be delivered. In this work, the sensitivity of gas chromatography coupled to a triple quadrupole with chemical ionization (GC-CI-MS/MS) is applied to detect trace levels of 10 testosterone and 2 nandrolone esters in plasma for in human doping analysis. The detection method was developed employing a liquid-liquid extraction and HPLC cleanup step before analysis on the GC-CI-MS/MS. The quantitative method was validated in a linear range of 100-2000 pg/ml and proved to be selective, reproducible and very sensitive with limits of detection as low as to 10 pg/ml. A clinical study with the administration of testosterone undecanoate in 3 volunteers was carried out and the compound was detectable up to 86 days after administration.

Parameters

Science
Study
Date
15 March 2020
People
Barrabin, Juliana
Deventer, Koen
Iannone, Michele
Polet, Michael
T'Sjoen, Guy
Van Eenoo, Peter
Van Gansbeke, Wim
Van Renterghem, Pieter
Viaene, Wouter
Country
Belgium
Brazil
Italy
Language
English
ADRV
Adverse Analytical Finding / presence
Other organisations
Universitair Ziekenhuis Gent (UZ Gent) - Ghent University Hospital
Universiteit Gent (UGent) - Ghent University
Laboratories
Ghent, Belgium: DoCoLab Universiteit Gent-UGent
Rio de Janeiro, Brazil: Laboratório Brasileiro de Controle de Dopagem – LBCD – LADETEC / IQ - UFRJ
Roma, Italia: Laboratorio Antidoping FMSI
Analytical aspects
Isotope-ratio mass spectrometry (IRMS)
Testing method development
Doping classes
S1. Anabolic Agents
Substances
Testosterone
Document category
Abstract
Date generated
24 March 2020
Date of last modification
27 March 2020
Category
  • Legal Source
  • Education
  • Science
  • Statistics
  • History
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  • Country
  • Language
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  • ADRV
  • Legal Terms
  • Sport/IFs
  • Other organisations
  • Laboratories
  • Analytical aspects
  • Doping classes
  • Substances
  • Medical terms
  • Various
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