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Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Oct 01; 1064:124-138.JC

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 150μL 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 2mM ammonium formate/0.1% formic acid and acetonitrile/0.1% formic acid as mobile phases. The chromatographic run time amounts to 9.3min (including re-equilibration). The total cycle time is 11min, 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 4μg/L), whilst full validation was not feasible for the remaining 12 analytes. For the fully validated analytes, the method achieved linearity in the 5μg/L (lower limit of quantification, LLOQ) to 250μg/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 1.6μg/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.

Authors+Show Affiliations

Institute of Legal Medicine, Medical Faculty, University of Cologne, Cologne, Germany.Institute of Legal Medicine, Medical Faculty, University of Cologne, Cologne, Germany.Institute of Legal Medicine, Medical Faculty, University of Cologne, Cologne, Germany.Institute of Biochemistry, German Sport University Cologne, Cologne, Germany.Institute of Legal Medicine, Medical Faculty, University of Cologne, Cologne, Germany; Institute of Forensic Medicine, University of Basel - Health Department Basel, Switzerland. Electronic address: katja.bender@bs.ch.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

28922649

Citation

Lehmann, Sabrina, et al. "Determination of 74 New Psychoactive Substances in Serum Using Automated In-line Solid-phase Extraction-liquid Chromatography-tandem Mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1064, 2017, pp. 124-138.
Lehmann S, Kieliba T, Beike J, et al. Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2017;1064:124-138.
Lehmann, S., Kieliba, T., Beike, J., Thevis, M., & Mercer-Chalmers-Bender, K. (2017). Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1064, 124-138. https://doi.org/10.1016/j.jchromb.2017.09.003
Lehmann S, et al. Determination of 74 New Psychoactive Substances in Serum Using Automated In-line Solid-phase Extraction-liquid Chromatography-tandem Mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Oct 1;1064:124-138. PubMed PMID: 28922649.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry. AU - Lehmann,Sabrina, AU - Kieliba,Tobias, AU - Beike,Justus, AU - Thevis,Mario, AU - Mercer-Chalmers-Bender,Katja, Y1 - 2017/09/07/ PY - 2017/04/14/received PY - 2017/08/18/revised PY - 2017/09/01/accepted PY - 2017/9/19/pubmed PY - 2017/10/11/medline PY - 2017/9/19/entrez KW - In-line SPE-LC–MS/MS KW - New psychoactive substances (NPS) KW - Rapid determination KW - Serum SP - 124 EP - 138 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 1064 N2 - 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 150μL 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 2mM ammonium formate/0.1% formic acid and acetonitrile/0.1% formic acid as mobile phases. The chromatographic run time amounts to 9.3min (including re-equilibration). The total cycle time is 11min, 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 4μg/L), whilst full validation was not feasible for the remaining 12 analytes. For the fully validated analytes, the method achieved linearity in the 5μg/L (lower limit of quantification, LLOQ) to 250μg/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 1.6μg/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. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/28922649/Determination_of_74_new_psychoactive_substances_in_serum_using_automated_in_line_solid_phase_extraction_liquid_chromatography_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(17)30666-9 DB - PRIME DP - Unbound Medicine ER -