A comprehensive UHPLC-MS/MS method for the analysis of endogenous and exogenous steroids in serum for anti-doping purposes.
anti-doping
oral testosterone undecanoate
steroid esters
steroid profiling
Journal
Drug testing and analysis
ISSN: 1942-7611
Titre abrégé: Drug Test Anal
Pays: England
ID NLM: 101483449
Informations de publication
Date de publication:
Nov 2022
Nov 2022
Historique:
revised:
04
10
2022
received:
29
08
2022
accepted:
04
10
2022
pubmed:
8
10
2022
medline:
17
12
2022
entrez:
7
10
2022
Statut:
ppublish
Résumé
In the context of steroid analyses, the use of blood could represent a valuable complement to urine. While the blood steroid profile is currently being established to aid unveiling testosterone (T) doping, this matrix is also well suited for detection of exogenous anabolic steroids and steroid esters. In this study, a method to determine a simplified blood steroid profile in combination with the direct detection of exogenous anabolic steroids and steroid esters using just one serum aliquot was developed to obtain a comprehensive analytical workflow. Following the first chromatographic analysis of endogenous and exogenous steroids, samples were derivatised with Girard's reagent T (GT) to improve the ionisation of steroid esters and re-injected. The quantitative performance for T, androstenedione (A4) and 5α-dihydrotestosterone (DHT) was evaluated and the method was validated for qualitative analysis of exogenous analogues with estimated limits of detection (LOD) between 50 and 500 pg/ml. To demonstrate the applicability of the method, samples collected from a clinical study with an oral administration of testosterone undecanoate (TU) to 19 male volunteers were then analysed. The individual serum steroid profiles with the endogenous markers T, A4 and DHT were established as well as the concentrations of TU. TU was detected in all 19 volunteers up to 24 h, while DHT represented the most promising biomarker in endogenous steroid profile for the detection of oral TU administration. These results showed that the selected approach to combine exogenous and endogenous steroid analysis has the potential to strengthen T doping detection in the future.
Substances chimiques
Steroids
0
Testosterone
3XMK78S47O
Dihydrotestosterone
08J2K08A3Y
Androstenedione
409J2J96VR
Esters
0
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
1904-1919Subventions
Organisme : World Anti-Doping Agency
ID : 21A07RN
Informations de copyright
© 2022 John Wiley & Sons Ltd.
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