Simultaneous determination of 148 pharmaceuticals and illicit drugs in sewage sludge based on ultrasound-assisted extraction and liquid chromatography–tandem mass spectrometry

Abstract

This paper describes the development and validation of a new method for the simultaneous determination of 148 substances in sewage sludge. The selected compounds belong to different classes of pharmaceuticals, including antibiotics, analgesic and/or anti-inflammatory drugs, antiepileptics, benzodiazepines, antipsychotics, and antidepressants, among others, and illicit drugs, including opiates, opioids, cocaine, amphetamines, cannabinoids, and their metabolites. As far as the authors are aware, this is the first method in the peer-reviewed literature covering such a large number of target drugs for determination in a complex matrix like sewage sludge. The method presented herein combines ultrasound-assisted extraction (USE) and liquid chromatography coupled to tandem mass spectrometry. Good analytical performance was achieved, with limit-of-detection values below 10 ng g−1 d.w. for 91 % of the analytes and absolute recovery in the range 50–110 % for more than 77 % of the studied compounds. A combination of methanol and acidified water, also containing EDTA, proved to be the optimum solvent mixture to perform the extractions. An extra solid-phase-extraction clean-up step was not required, substantially reducing sample-preparation time and solvent consumption. Finally, the developed method was applied to the analysis of different sewage-sludge samples from five wastewater treatment plants of Santorini Island (Greece). Out of the 148 target compounds, 36 were detected. Several compounds, including acetylsalicylic acid, citalopram, and ciprofloxacin among others, had maximum concentrations above 100 ng g−1 d.w.

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Acknowledgments

This project was implemented under the Operational Program «Education and Lifelong Learning» and funded by the European Union (European Social Fund) and National Resources – ARISTEIA 624.

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Correspondence to Νikolaos S. Τhomaidis.

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Published in the topical collection Advances in LC-MS/MS Analysis with guest editors Damià Barceló and Mira Petrovic.

Pablo Gago-Ferrero and Viola Borova contributed equally to this work.

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Gago-Ferrero, P., Borova, V., Dasenaki, M.E. et al. Simultaneous determination of 148 pharmaceuticals and illicit drugs in sewage sludge based on ultrasound-assisted extraction and liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 407, 4287–4297 (2015). https://doi.org/10.1007/s00216-015-8540-6

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Keywords

  • Sewage sludge
  • Pharmaceuticals
  • Illicit drugs
  • LC-MS/MS
  • USE