Analysis of anabolic androgenic steroids as sulfate conjugates using high performance liquid chromatography coupled to tandem mass spectrometry. Issue 11 (16th October 2015)

• Record Type: Journal Article
• Authors: Rzeppa, S.; Heinrich, G.; Hemmersbach, P.
• Is Part Of: Drug testing and analysis. Volume 7:Issue 11/12(2015:Nov.)
• Page Start: 1030
• Page End: 1039
• Publication Date: 2015-10-16
• Subjects: doping analysis -- anabolic androgenic steroids -- sulfate conjugates -- liquid chromatography‐mass spectrometry -- metabolism; Drugs -- Analysis -- Periodicals; Drug testing -- Periodicals; Chemistry, Forensic -- Periodicals; 615.1901
• DOI: 10.1002/dta.1895
• Languages: English
• ISSNs: 1942-7603

Abstract

Abstract : Improvements in doping analysis can be effected by speeding up analysis time and extending the detection time. Therefore, direct detection of phase II conjugates of doping agents, especially anabolic androgenic steroids (AAS), is proposed. Besides direct detection of conjugates with glucuronic acid, the analysis of sulfate conjugates, which are usually not part of the routine doping control analysis, can be of high interest. Sulfate conjugates of methandienone and methyltestosterone metabolites have already been identified as long‐term metabolites. This study presents the synthesis of sulfate conjugates of six commonly used AAS and their metabolites: trenbolone, nandrolone, boldenone, methenolone, mesterolone, and drostanolone. In the following these sulfate conjugates were used for development of a fast and easy analysis method based on sample preparation using solid phase extraction with a mixed‐mode sorbent and detection by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC‐MS/MS). Validation demonstrated the suitability of the method with regard to the criteria given by the technical documents of the World Anti‐Doping Agency (WADA). In addition, suitability has been proven by successful detection of the synthesized sulfate conjugates in excretion urines and routine doping control samples. Copyright © 2015 John Wiley & Sons, Ltd. Abstract : Direct detection of phase II metabolites of anabolic androgenic steroids (AAS) can be of high interest because of extended detection times and easier sample preparation. This study presents the development of a fast analysis method for the direct detection of the sulfate conjugates of six commonly used AAS by high performance liquid chromatography tandem mass spectrometry.