title: 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.
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 0.01ngg(-1) to 2.08ngg(-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 26.4ngg(-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.
authors.affiliation: REQUIMTE/LAQV/Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4200-072 Porto, Portugal; CIIMAR/CIMAR-Interdisciplinary Centre of Marine and Environmental Research, Coastal and Marine Environmental Toxicology Group, University of Porto, Rua dos Bragas, 289, 4050-123, Portugal. Electronic address: luciahelena.santos@sapo.pt.
authors.forename: Lúcia H M L M
authors.initials: LHMLM
authors.lastname: Santos
authors.affiliation: REQUIMTE/LAQV/Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4200-072 Porto, Portugal.
authors.forename: Maria João
authors.initials: MJ
authors.lastname: Ramalhosa
authors.affiliation: CIIMAR/CIMAR-Interdisciplinary Centre of Marine and Environmental Research, Coastal and Marine Environmental Toxicology Group, University of Porto, Rua dos Bragas, 289, 4050-123, Portugal; School of Marine Studies, Faculty of Science, Technology and Environment, The University of South Pacific, Laucala Bay Road, Suva, Fiji.
authors.forename: Marta
authors.initials: M
authors.lastname: Ferreira
authors.affiliation: REQUIMTE/LAQV/Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4200-072 Porto, Portugal.
authors.forename: Cristina
authors.initials: C
authors.lastname: Delerue-Matos
mesh_terms: D000097:Acetonitriles / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D004784:Environmental Monitoring / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry*; D057230:Limit of Detection; D011174:Portugal; D011619:Psychotropic Drugs / Q000032:analysis*; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry
chemical_list: D000097:Acetonitriles; D011619:Psychotropic Drugs; C032159:acetonitrile
keywords: Metabolites; Psychiatric drugs; QuEChERS; Sediment; UHPLC-ESI-MS CID-MS/MS