High-temperature high-performance liquid chromatography on a porous graphitized carbon column coupled to an Orbitrap mass spectrometer with atmospheric pressure photoionization for screening exogenous anabolic steroids in human urine

Rapid Communications in Mass Spectrometry : RCM
E D VirusAslan A Kubatiev

Abstract

The presence in a urinary matrix of a large number of endogenous steroids and corticosteroids with similar structures can hamper the detection of specific exogenous steroids using liquid chromatography/mass spectrometry (LC/MS) with reversed-phase columns. Therefore, the development of LC/MS methods using alternative columns is of great interest. Porous graphitized carbon is a unique stationary phase for high-performance liquid chromatography (HPLC), with properties differing from traditional silica-based and polymeric stationary phases. The new method involves enzymatic hydrolysis, liquid-liquid extraction, and determination by high-temperature HPLC/Orbitrap mass spectrometry (HTLC/Orbitrap MS) with atmospheric pressure photoionization (APPI). To achieve APPI of doping substances, the mobile phase consisted of 0.1% CF3COOH (A) and a mixture of acetonitrile/2-propanol (25:75 v/v), containing 0.1% CF3COOH (B), which was used as an effective proton source. A screening method for the detection of 57 exogenous steroids has been developed. The method was validated by spiking 10 different blank urine samples at different concentration levels. Validation parameters included limit of detection (LOD), selectivity, ion suppression, extra...Continue Reading

References

Nov 29, 2002·Journal of Chromatography. a·Esther Forgács
Oct 24, 2006·Journal of Chromatography. a·Lance A Riddle, Georges Guiochon
Sep 19, 2008·Journal of Chromatography. a·Risto Kostiainen, Tiina J Kauppila
Mar 23, 2011·Analytical and Bioanalytical Chemistry·Mario ThevisWilhelm Schänzer
Jul 12, 2011·Analytical and Bioanalytical Chemistry·Byoung Wook JeonJaeick Lee
Mar 19, 2014·British Journal of Sports Medicine·Hans GeyerMario Thevis

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Citations

Nov 26, 2016·Drug Testing and Analysis·Mario ThevisWilhelm Schänzer

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