A fully automated approach for the analysis of 37 psychoactive substances in raw wastewater based on on-line solid phase extraction-liquid chromatography-tandem mass spectrometry

Abstract

This work presents a multi-residue method for the simultaneous determination of 37 legal and illicit psychoactive substances in wastewater, including the most common illicit drugs (cocaine-related compounds, amphetamine-type stimulants, hallucinogens, opiates/opioids, and cannabinoids), new psychoactive substances (two synthetic cathinones, the synthetic opioid AH-7921, and the arylcyclohexylamine methoxetamine), and legal but controlled psychoactive substances (stimulants, benzodiazepines, antidepressants, sedatives, antipsychotics, and hypnotics). To this end a fully automated analytical approach based on solid phase extraction coupled in series to liquid chromatography tandem mass spectrometry detection (on-line SPE- LC-MS/MS) was used. The methodology developed was validated in terms of linearity, recovery, repeatability, and sensitivity in wastewater. Method linearity was between 0.1 ng/L (or the analyte limit of quantification if higher) and 2,000 ng/L (10,250 ng/L in the case of caffeine). Absolute recoveries were variable (between 5% and 132%), depending on the analyte. However, the use of isotopically labeled compounds corrected for analyte losses during the extraction process and matrix effects (relative recoveries within the range of 80-120%). Repeatability of the method was satisfactory for all analytes, with RSD values lower than 13% for most compounds. Limits of detection and quantification in wastewater were below 7 and 23 ng/L, respectively, for all analytes except lormetazepam (10 and 32 ng/L), caffeine (13 and 44 ng/L), and the cannabinoids 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (18 and 61 ng/L) and 11-hydroxy-Delta(9)- tetrahydrocannabinol (69 and 228 ng/L). The method was applied to the analysis of wastewater samples collected daily in Barcelona for one week. Twenty-five of the 37 analytes were detected in the samples analyzed. Average concentrations ranged from 7 ng/L in the case of zolpidem to 54 mu g/L in the case of caffeine. (C) 2018 Elsevier B.V. All rights reserved.

Keywords

Drugs of abuse; Psychotropic pharmaceuticals; New psychoactive substances; On-line solid phase extraction; Liquid chromatography-tandem mass spectrometry; Sewage water

Published in

Journal of Chromatography A
2018, Volume: 1576, pages: 80-89 Publisher: ELSEVIER SCIENCE BV

SLU Authors

• Postigo, Cristina

  • Department of Aquatic Sciences and Assessment, Swedish University of Agricultural Sciences
    
  • Institute of Environmental Assessment and Water Research (IDAEA-CSIC)

Sustainable Development Goals

SDG3 Good health and well-being
SDG6 Clean water and sanitation


UKÄ Subject classification

Analytical Chemistry


Publication identifier

DOI: https://doi.org/10.1016/j.chroma.2018.09.038

Permanent link to this page (URI)

https://res.slu.se/id/publ/100889