Τίτλος:
Determination of anabolic androgenic steroids as imidazole carbamate derivatives in human urine using liquid chromatography–tandem mass spectrometry
Γλώσσες Τεκμηρίου:
Αγγλικά
Περίληψη:
Anabolic androgenic steroids are widely abused substances in sports doping. Their detection present limitations regarding the use of soft ion sources such as electrospray or atmospheric pressure chemical ionization by liquid chromatography–tandem mass spectrometry. In the current study, a novel derivatization method was developed for the ionization enhancement of selected anabolic androgenic steroids. The proposed method aims at the introduction of an easily ionizable moiety into the steroid molecule by converting the hydroxyl groups into imidazole carbamates using 1,1′-carbonyldiimidazole as derivatization reagent. The proposed method was applied to water and urine samples spiked with exogenous anabolic androgenic steroids in various concentration levels. Steroid imidazole carbamate derivatives have shown intensive [M+H]+ signals under electrospray ionization and common fragmentation patterns in tandem mass spectrometry mode with [M-CO2+H]+ and [M-ΙmCO2+H]+ as major ions with low collision energy. The obtained results showed that the majority of steroids were detectable at concentrations equal or lower to their minimum required performance level according to the World Anti-Doping Agency technical document. The proposed method is sensitive with a preparation procedure that could be easily applied to the analysis of doping control samples. © 2020 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Συγγραφείς:
Fragkaki, A.G.
Petropoulou, G.
Athanasiadou, I.
Kiousi, P.
Kioukia-Fougia, N.
Archontaki, H.
Bakeas, E.
Angelis, Y.S.
Περιοδικό:
Journal of High Resolution Chromatography (now called Journal of Separation Science)
Εκδότης:
Wiley-VCH Verlag
Λέξεις-κλειδιά:
Atmospheric ionization; Atmospheric pressure; Chemical detection; Drug products; Electrospray ionization; Ion sources; Lipids; Mass spectrometry, Atmospheric pressure chemical ionization; Derivatization method; Derivatization reagent; Fragmentation patterns; Ionization enhancement; Preparation procedures; Tandem mass spectrometry; World Anti-Doping Agency, Liquid chromatography, 1,1' carbonyldiimidazole; anabolic androgenic steroid; carbamic acid derivative; hydroxyl group; hydroxysteroid; imidazole carbamate derivative; imidazo[1,2 a]benzimidazole derivative; reagent; steroid; steroid imidazole carbamate derivative; unclassified drug; water; androgen; imidazole; imidazole derivative; steroid, analytical parameters; Article; collision energy; concentration (parameter); controlled study; derivatization; electrospray mass spectrometry; energy; ionization; liquid chromatography-mass spectrometry; performance; priority journal; sensitivity analysis; tandem mass spectrometry; urinalysis; urine; chemistry; conformation; doping; human; liquid chromatography; stereoisomerism; substance abuse; urine, Androgens; Chromatography, Liquid; Doping in Sports; Humans; Imidazoles; Molecular Conformation; Stereoisomerism; Steroids; Substance Abuse Detection; Tandem Mass Spectrometry
DOI:
10.1002/jssc.202000036
