Universität zu Köln

Putz, Marlen, Piper, Thomas, Dubois, Michel, Delahaut, Philippe and Thevis, Mario (2019). Analysis of endogenous steroids in urine by means of multi-immunoaffinity chromatography and isotope ratio mass spectrometry for sports drug testing. Anal. Bioanal. Chem., 411 (28). S. 7563 - 7572. HEIDELBERG: SPRINGER HEIDELBERG. ISSN 1618-2650

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Abstract

Detecting the administration of naturally occurring but synthetically derived steroids (e.g., testosterone) in routine doping controls is particularly laborious and time-consuming. Carbon isotope signatures determined by isotope ratio mass spectrometry (IRMS) have been established as the method of choice to generate confirmatory evidence in case of suspicious or atypical findings in steroid profile analyses; however, IRMS measurements require sophisticated sample preparation methods employing up to two high-performance liquid chromatography (HPLC) purification steps. Here, an alternative sample preparation approach is presented. Immunoaffinity chromatography (IAC) was employed to reduce the batch analysis time by omitting the time-consuming HPLC purification steps, while pre- and post-IAC sample handling followed published protocols. IAC exploits specific antibody-immunogen interactions, and the option of combining three immunoaffinity gels containing specific antibodies for testosterone, pregnanediol, and 11-ketoetiocholanolone into a multi-immunoaffinity sample preparation approach was assessed. Due to cross reactivities, also etiocholanolone, androsterone, 5 beta-androstanediol, and 5 alpha-androstanediol were co-extracted and included in the testing protocol. The method was validated by determining precision, recovery, and carry over, and performing linear mixing models. IAC was found to be applicable to the determination of carbon isotope ratios in doping controls and the approach allowed for an accelerated sample preparation.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Putz, Marlen UNSPECIFIED UNSPECIFIED UNSPECIFIED Piper, Thomas UNSPECIFIED UNSPECIFIED UNSPECIFIED Dubois, Michel UNSPECIFIED UNSPECIFIED UNSPECIFIED Delahaut, Philippe UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-130561
DOI:	10.1007/s00216-019-02169-3
Journal or Publication Title:	Anal. Bioanal. Chem.
Volume:	411
Number:	28
Page Range:	S. 7563 - 7572
Date:	2019
Publisher:	SPRINGER HEIDELBERG
Place of Publication:	HEIDELBERG
ISSN:	1618-2650
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language BOVINE URINE; REFERENCE POPULATION; C-13/C-12 RATIOS; TESTOSTERONE; CLEANUP; PURIFICATION; 19-NORANDROSTERONE; ANDROSTADIENEDIONE; CORTICOSTEROIDS; NORTESTOSTERONE Multiple languages Biochemical Research Methods; Chemistry, Analytical Multiple languages
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/13056