Universität zu Köln

Casilli, Alessandro, Piper, Thomas ORCID: 0000-0002-7462-6693, de Oliveira, Fabio Azamor, Padilha, Monica Costa, Pereira, Henrique Marcelo, Thevis, Mario and de Aquino Neto, Francisco Radler (2016). Optimization of an online heart-cutting multidimensional gas chromatography cleanup step for isotopic ratio mass spectrometry and simultaneous quadrupole mass spectrometry measurements of endogenous anabolic steroid in urine. Drug Test. Anal., 8 (11-12). S. 1204 - 1212. HOBOKEN: WILEY. ISSN 1942-7611

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Abstract

Measuring carbon isotope ratios (CIRs) of urinary analytes represents a cornerstone of doping control analysis and has been particularly optimized for the detection of the misuse of endogenous steroids. Isotope ratio mass spectrometry (IRMS) of appropriate quality, however, necessitates adequate purities of the investigated steroids, which requires extensive pre-analytical sample clean-up steps due to both the natural presence of the target analytes and the high complexity of the matrix. In order to accelerate the sample preparation and increase the automation of the process, the use of multidimensional gas chromatography (MDGC) prior to IRMS experiments, was investigated. A well-established instrumental configuration based on two independent GC ovens and one heart-cutting device was optimized. The first dimension (1D) separation was obtained by a non-polar column which assured high efficiency and good loading capacity, while the second dimension (2D), based on a mid-polar stationary phase, provided good selectivity. A flame ionization detector monitored the 1D, and the 2D was simultaneously recorded by isotope ratio and quadrupole mass spectrometry. The assembled MDGC set-up was applied for measuring testosterone, 5 alpha- and 5 beta-androstanediol, androsterone, and etiocholanolone as target compounds and pregnanediol as endogenous reference compound. The urine sample were pretreated by conventional sample preparation steps comprising solid-phase extraction, hydrolysis, and liquid-liquid extraction. The extract obtained was acetylated and different aliquots were injected into the MDGC system. Two high performance liquid chromatography steps, conventionally adopted prior to CIR measurements, were replaced by the MDGC approach. The obtained values were consistent with the conventional ones. Copyright (C) 2016 John Wiley & Sons, Ltd.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Casilli, Alessandro UNSPECIFIED UNSPECIFIED UNSPECIFIED Piper, Thomas UNSPECIFIED orcid.org/0000-0002-7462-6693 UNSPECIFIED de Oliveira, Fabio Azamor UNSPECIFIED UNSPECIFIED UNSPECIFIED Padilha, Monica Costa UNSPECIFIED UNSPECIFIED UNSPECIFIED Pereira, Henrique Marcelo UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED de Aquino Neto, Francisco Radler UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-256189
DOI:	10.1002/dta.2119
Journal or Publication Title:	Drug Test. Anal.
Volume:	8
Number:	11-12
Page Range:	S. 1204 - 1212
Date:	2016
Publisher:	WILEY
Place of Publication:	HOBOKEN
ISSN:	1942-7611
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language C-13/C-12 RATIOS; METABOLITES Multiple languages Biochemical Research Methods; Chemistry, Analytical; Pharmacology & Pharmacy Multiple languages
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/25618