dc.contributor.author
Bredendiek, Felix
dc.contributor.author
Parr, Maria Kristina
dc.date.accessioned
2024-07-29T11:20:46Z
dc.date.available
2024-07-29T11:20:46Z
dc.identifier.uri
https://refubium.fu-berlin.de/handle/fub188/41848
dc.identifier.uri
http://dx.doi.org/10.17169/refubium-41568
dc.description.abstract
Because of their performance-enhancing effect, anabolic androgenic steroids (AAS) are often misused in sports. Nearly half of the adverse analytical findings (AAF) in 2022 doping controls are correlated to AAS misuse. Metabolites play a crucial role in the bioanalysis of endogenous and exogenous steroids. Therefore, one important field in antidoping research is the investigation on drug metabolizing and steroidogenic enzymes. The introduction of a hydroxy group is the most common reaction, which is catalyzed by cytochrome P450 (CYP) enzymes in phase-I metabolism. Analysis of AAS metabolites is commonly performed using gas chromatography mass spectrometry (GC-MS) systems. Laborious sample preparation and extended run times compared to liquid chromatography (tandem) mass spectrometry (LC-MS/MS) methods are usually correlated with this type of analysis. On the other hand, liquid chromatography (tandem) mass spectrometry (LC-MS[/MS]) methods have a lower separation efficiency than GC-MS methods. Both techniques lack selectivity for hydroxylated 17α-methyltestosterone metabolites. Therefore, as an orthogonal analytical approach, a supercritical fluid chromatography tandem mass spectrometry method was developed to separate four hydroxy metabolites of 17α-methyltestosterone (2α-/2β-/4-/6β-hydroxy-17α-methyltestosterone). This project aimed to get a more in-depth look at the metabolization and analysis of 17α-methyltestosterone and its hydroxylated metabolites. The developed method revealed lower limits of quantitation between 0.6 and 6 ng/ml at an accuracy of 85–115% using a matrix matched calibration. An in vitro study with human liver microsomes shows 6β-hydroxy-17α-methyltestosterone as main metabolite (15.9%) as well as the metabolite 2β-hydroxy-17α-methyltestosterone (0.5%). The results show that the developed method is sensitive and robust. In addition, the method allows a previously missing discrimination of the hydroxylated metabolites in a short analysis time without prior, complex derivatizations.
en
dc.format.extent
9 Seiten
dc.rights.uri
https://creativecommons.org/licenses/by/4.0/
dc.subject
methyltestosterone
en
dc.subject
tandem mass spectrometry
en
dc.subject.ddc
500 Naturwissenschaften und Mathematik::540 Chemie::540 Chemie und zugeordnete Wissenschaften
dc.title
SFC-MS/MS for orthogonal separation of hydroxylated 17α-methyltestosterone isomers
dc.type
Wissenschaftlicher Artikel
dcterms.bibliographicCitation.doi
10.1002/dta.3620
dcterms.bibliographicCitation.journaltitle
Drug Testing and Analysis
dcterms.bibliographicCitation.number
7
dcterms.bibliographicCitation.pagestart
717
dcterms.bibliographicCitation.pageend
725
dcterms.bibliographicCitation.volume
16
dcterms.bibliographicCitation.url
https://doi.org/10.1002/dta.3620
refubium.affiliation
Biologie, Chemie, Pharmazie
refubium.affiliation.other
Institut für Pharmazie

refubium.funding
DEAL Wiley
refubium.note.author
Die Publikation wurde aus Open Access Publikationsgeldern der Freien Universität Berlin gefördert.
refubium.resourceType.isindependentpub
no
dcterms.accessRights.openaire
open access
dcterms.isPartOf.eissn
1942-7611