Universität zu Köln

Goergens, Christian, Guddat, Sven, Thomas, Andreas ORCID: 0000-0003-1199-0743, Wachsmuth, Philipp, Orlovius, Anne-Katrin, Sigmund, Gerd, Thevis, Mario and Schaenzer, Wilhelm (2016). Simplifying and expanding analytical capabilities for various classes of doping agents by means of direct urine injection high performance liquid chromatography high resolution/high accuracy mass spectrometry. J. Pharm. Biomed. Anal., 131. S. 482 - 497. AMSTERDAM: ELSEVIER SCIENCE BV. ISSN 1873-264X

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Abstract

So far, in sports drug testing compounds of different classes are processed and measured using different screening procedures. The constantly increasing number of samples in doping analysis, as well as the large number of substances with doping related, pharmacological effects require the development of even more powerful assays than those already employed in sports drug testing, indispensably with reduced sample preparation procedures. The analysis of native urine samples after direct injection provides a promising analytical approach, which thereby possesses a broad applicability to many different compounds and their metabolites, without a time-consuming sample preparation. In this study, a novel multi-target approach based on liquid chromatography and high resolution/high accuracy mass spectrometry is presented to screen for more than 200 analytes of various classes of doping agents far below the required detection limits in sports drug testing. Here, classic groups of drugs as diuretics, stimulants, beta(2)-agonists, narcotics and anabolic androgenic steroids as well as various newer target compounds like hypoxia-inducible factor (HIF) stabilizers, selective androgen receptor modulators (SARMs), selective estrogen receptor modulators (SERMs), plasma volume expanders and other doping related compounds, listed in the 2016 WADA prohibited list were implemented. As a main achievement, growth hormone releasing peptides could be implemented, which chemically belong to the group of small peptides (<2 kDa) and are commonly determined by laborious and time-consuming stand-alone assays. The assay was fully validated for qualitative purposes considering the parameters specificity, robustness (rRT: <2%), intra- (CV: 1.7-18.4 %) and inter-day precision (CV: 2.3-18.3%) at three concentration levels, linearity (R-2 > 0.99), limit of detection (0.1-25 ng/mL; 3'OH-stanozolol glucuronide: 50 pg/mL; dextran/HES: 10 mu g/mL) and matrix effects. (C) 2016 Elsevier B.V. All rights reserved.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Goergens, Christian UNSPECIFIED UNSPECIFIED UNSPECIFIED Guddat, Sven UNSPECIFIED UNSPECIFIED UNSPECIFIED Thomas, Andreas UNSPECIFIED orcid.org/0000-0003-1199-0743 UNSPECIFIED Wachsmuth, Philipp UNSPECIFIED UNSPECIFIED UNSPECIFIED Orlovius, Anne-Katrin UNSPECIFIED UNSPECIFIED UNSPECIFIED Sigmund, Gerd UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED Schaenzer, Wilhelm UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-255323
DOI:	10.1016/j.jpba.2016.09.015
Journal or Publication Title:	J. Pharm. Biomed. Anal.
Volume:	131
Page Range:	S. 482 - 497
Date:	2016
Publisher:	ELSEVIER SCIENCE BV
Place of Publication:	AMSTERDAM
ISSN:	1873-264X
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language ANDROGEN RECEPTOR MODULATORS; TOREMIFENE METABOLITES; SCREENING METHOD; PHYSIOLOGICAL DISPOSITION; P-HYDROXYMETHAMPHETAMINE; HYDROXYETHYL STARCH; CONTROL PURPOSES; LC-MS/MS; EXCRETION; SPORTS Multiple languages Chemistry, Analytical; Pharmacology & Pharmacy Multiple languages
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/25532