Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1569, Issue -, Pages 91-100Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2018.07.045
Keywords
Benzodiazepines; Antidepressants; Substances of abuse; Sewage analysis; Solid-phase extraction; Ultra-high performance liquid chromatography
Funding
- Spanish Ministry of Economy and Competitiveness [CTM2014-56628-C3-2-R]
- Galician Council of Culture, Education and Universities [ED431C2017/36, ED481D 2017/003]
- FEDER/ERDF
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This study presents a new multi-residue analytical method for the simultaneous determination of 38 psychoactive drugs (including benzodiazepines, antidepressants and drugs of abuse) and related metabolites in raw wastewater. Potential analyte losses during sample filtration and stability in wastewater were evaluated. Analyte losses, especially for 12 compounds, were observed during filtration, indicating a strong sorption onto the filter material. In order to overcome this effect, filtered water samples were combined with methanolic washes of the corresponding filters and the resulting solutions were solid-phase extracted on mixed-mode (reverse-phase plus cation-exchange) sorbents. Extracts were analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry. Quantification was performed by the internal standard method with isotopic labeled analogs. Recovery percentages varied between 65% and 137%; method quantification limits ranged between 0.2 and 22 ng/L in ultrapure water and between 0.3 and 30 ng/L in wastewater for all the analytes but three (for which they were similar to 60-80 ng/L). The analysis of 24 h-composite samples collected during one week in the city of Santiago de Compostela demonstrated the ubiquity of 31 analytes, which were positively quantified in all samples. The highest concentrations were found for some of the antidepressants, with mean and maximum levels exceeding, in some cases, the levels previously reported in literature. This fact could be related to the additional washing step of the filters using methanol, which allowed to desorb retained analytes highlighting the importance of this step during the sample preparation protocol. (C) 2018 Elsevier B.V. All rights reserved.
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