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Determination of anabolic androgenic steroids as imidazole carbamate derivatives in human urine using liquid chromatography–tandem mass spectrometry
Author(s) -
Fragkaki Argyro G.,
Petropoulou Georgia,
Athanasiadou Ioanna,
Kiousi Polyxeni,
KioukiaFougia Nassia,
Archontaki Helen,
Bakeas Evangelos,
Angelis Yiannis S.
Publication year - 2020
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.202000036
Subject(s) - chemistry , chromatography , derivatization , mass spectrometry , tandem mass spectrometry , electrospray ionization , liquid chromatography–mass spectrometry , electrospray , nandrolone , atmospheric pressure chemical ionization , anabolic steroid , chemical ionization , anabolism , ionization , organic chemistry , ion , biochemistry
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‐CO 2 +H] + and [M‐ΙmCO 2 +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.