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Development of a modified acetonitrile-based extraction procedure followed by ultra-high performance liquid chromatography–tandem mass spectrometry for the analysis of psychiatric drugs in sediments

Santos, Lúcia H. M. L. M. and Ramalhosa, Maria João and Ferreira, Marta and Delerue-Matos, Cristina (2016) Development of a modified acetonitrile-based extraction procedure followed by ultra-high performance liquid chromatography–tandem mass spectrometry for the analysis of psychiatric drugs in sediments. Journal of Chromatography A, 1437 . pp. 37-48. ISSN 0021-9673

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    Abstract

    An analytical method based on a modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction procedure followed by ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) was developed for the analysis of psychiatric drugs in sediments. An optimized approach was applied in sample preparation by using basic acetonitrile as extraction solvent. Extraction was followed by a clean-up using dispersive solid phase extraction (dSPE) to remove matrix interfering compounds. The analytical method was validated in terms of sensitivity, linearity, recovery, intra- and inter-day precisions and method detection and quantification limits. Under optimized conditions, limits of detection ranged from 0.01 ng g−1 to 2.08 ng g−1; and recoveries between 47 and 110% with relative standard deviation (RSD) below 5%. The developed methodology was applied to sediments of two Portuguese rivers (Douro and Lima rivers) and nine out of eleven psychiatric drugs were detected in sediments at concentrations up to 26.4 ng g−1 (dry weight). To the best of our knowledge, it was the first time that the human metabolites norfluoxetine and norsertraline were detected in river sediments at levels of few nanograms per gram.

    Item Type: Journal Article
    Subjects: Q Science > Q Science (General)
    Q Science > QD Chemistry
    Divisions: Faculty of Science, Technology and Environment (FSTE) > School of Marine Studies
    Depositing User: Marta Ferreira
    Date Deposited: 19 Sep 2016 14:14
    Last Modified: 19 Sep 2016 14:14
    URI: http://repository.usp.ac.fj/id/eprint/8882
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