Targeting the administration of ecdysterone in doping control samples

Targeting the administration of ecdysterone in doping control samples / Maria Kristina Parr, Gabriella Ambrosio, Bernhard Wuest, Monica Mazzarino, Xavier de la Torre, Francesca Sibilia, Jan Felix Joseph, Patrick Diel, Francesco Botrè. - (Forensic Toxicology (2019) 15 October; p. 1-13).
- DOI: 10.1101/685230


Abstract

Purpose
The phytosteroid ecdysterone was recently reported to enhance performance in sports and may thus be considered as a substance of relevance in anti-doping control. To trace back an administration of ecdysterone from urine samples, analytical properties have been investigated to assess its integration into initial testing procedures (ITP) in doping control laboratories.

Methods
Analytical properties of ecdysterone were evaluated using gas chromatography-quadrupole/time-of-flight-mass spectrometry (GC–QTOF–MS) and liquid chromatography (LC)–QTOF–MS. Its metabolism and elimination in human were studied using urines collected after administration.

Results
The detectability of ecdysterone by GC–MS (after derivatization) and/or LC–MS(/MS) has been demonstrated and sample preparation methods were evaluated. Dilute-and-inject for LC–MS(/MS) or solid phase extraction using Oasis HLB for GC–MS or LC–MS were found most suitable, while liquid–liquid extraction was hampered by the high polarity of ecdysteroids.

Most abundantly, ecdysterone was detected in the post administration urines as parent compound besides the metabolite desoxy-ecdysterone. Additionally, desoxy-poststerone was tentatively assigned as minor metabolite, however, further investigations are needed.

Conclusion
An administration of ecdysterone can be targeted using existing procedures of anti-doping laboratories. Ecdysterone and desoxy-ecdysterone appeared as suitable candidates for integration in ITP. Using dilute-and-inject a detection of the parent compound was possible for more than 2 days after the administration of a single dose of ~ 50 mg.

Original document

Parameters

Science
Study
Date
15 October 2019
People
Ambrosio, Gabriella
Botrè, Francesco
de la Torre, Xavier
Diel, Patrick
Joseph, Jan Felix
Mazzarino, Monica
Parr, Maria Kristina
Sibilia, Francesca
Wuest, Bernhard
Country
Germany
Italy
United States of America
Language
English
Other organisations
Deutsche Sporthochschule Köln (DSHS) - German Sport University Cologne
Freie Universität Berlin (FU Berlin) - Free University of Berlin
Sapienza Università di Roma - Sapienza University of Rome
Laboratories
Roma, Italia: Laboratorio Antidoping FMSI
Analytical aspects
New substance, not on prohibited list
Testing method development
Document category
Scientific article
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Pdf file
Date generated
19 November 2019
Date of last modification
4 December 2019
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  • Education
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  • Analytical aspects
  • Doping classes
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