Universität zu Köln

Lehmann, Sabrina, Kieliba, Tobias, Beike, Justus, Thevis, Mario and Mercer-Chalmers-Bender, Katja ORCID: 0000-0002-3843-9065 (2017). Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry. J. Chromatogr. B, 1064. S. 124 - 139. AMSTERDAM: ELSEVIER SCIENCE BV. ISSN 1873-376X

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Abstract

A detailed description is given of the development and validation of a fully automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method capable of detecting 90 central-stimulating new psychoactive substances (NPS) and 5 conventional amphetamine-type stimulants (amphetamine, 3,4-methylenedioxy-methamphetamine (MDMA), 3,4-methylenedioxy-amphetamine (MDA), 3,4-methylenedioxy-N-ethyl-amphetamine (MDEA), methamphetamine) in serum. The aim was to apply the validated method to forensic samples. The preparation of 150 mu L of serum was performed by an Instrument Top Sample Preparation (ITSP)-SPE with mixed mode cation exchanger cartridges. The extracts were directly injected into an LC MS/MS system, using a biphenyl column and gradient elution with 2 mM ammonium formate/0.1% formic acid and acetonitrile/0.1% formic acid as mobile phases. The chromatographic run time amounts to 9.3 min (including re-equilibration). The total cycle time is 11 min, due to the interlacing between sample preparation and analysis. The method was fully validated using 69 NPS and five conventional amphetamine-type stimulants, according to the guidelines of the Society of Toxicological and Forensic Chemistry (GTFCh). The guidelines were fully achieved for 62 analytes (with a limit of detection (LOD) between 0.2 and 4 mu g/L), whilst full validation was not feasible for the remaining 12 analytes. For the fully validated analytes, the method achieved linearity in the 5 mu g/L (lower limit of quantification, LLOQ) to 250 mu g/L range (coefficients of determination > 0.99). Recoveries for 69 of these compounds were greater than 50%, with relative standard deviations <= 15%. The validated method was then tested for its capability in detecting a further 21 NPS, thus totalling 95 tested substances. An LOD between 0.4 and 1.6 mu g/L was obtained for these 21 additional qualitatively -measured substances. The method was subsequently successfully applied to 28 specimens from routine forensic case work, of which 7 samples were determined to be positive for NPS consumption.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Lehmann, Sabrina UNSPECIFIED UNSPECIFIED UNSPECIFIED Kieliba, Tobias UNSPECIFIED UNSPECIFIED UNSPECIFIED Beike, Justus UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED Mercer-Chalmers-Bender, Katja UNSPECIFIED orcid.org/0000-0002-3843-9065 UNSPECIFIED
URN:	urn:nbn:de:hbz:38-215592
DOI:	10.1016/j.jchromb.2017.09.003
Journal or Publication Title:	J. Chromatogr. B
Volume:	1064
Page Range:	S. 124 - 139
Date:	2017
Publisher:	ELSEVIER SCIENCE BV
Place of Publication:	AMSTERDAM
ISSN:	1873-376X
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language RECEPTOR INTERACTION PROFILES; DESIGNER DRUGS; LC-MS/MS; MONOAMINE TRANSPORTER; SYNTHETIC CATHINONES; SCREENING METHOD; WHOLE-BLOOD; URINE; STIMULANTS; 25I-NBOME Multiple languages Biochemical Research Methods; Chemistry, Analytical Multiple languages
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/21559