title: Determination of tricyclic antidepressants in biota tissue and environmental waters by liquid chromatography-tandem mass spectrometry.
abstract: This work describes the optimization, validation, and application in real samples of accurate and precise analytical methods to determine tricyclic antidepressants (TCAs), including amitriptyline, nortriptyline, imipramine, and clomipramine in different environmental matrices, such as water (estuary, seawater, and wastewater treatment plant effluent) and biota (fish muscle, fish liver, and mussels), which would lead to supplement the scarce information on the presence of TCAs in aquatic organisms. The analysis step performed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was fully optimized to improve the sensitivity of the separation and detection steps. The extraction of solid samples was accomplished using focused ultrasonic solid-liquid extraction (FUSLE), which required a low amount of sample (0.5 g), solvent (7 mL acetonitrile/H2O, 95:5 v/v) and short extraction time (30 s). In the optimisation of the clean-up step, mixed mode solid-phase extraction (SPE) using a strong cation exchanger rendered clean extracts and the best results in terms of extraction efficiency and matrix effect. The same SPE mode was also used for the extraction and pre-concentration of TCAs from environmental water matrices. The methods afforded satisfactory apparent recovery values (86-122%) and repeatability (RSD < 5%), regardless of the matrix. Finally, the developed methods were applied to the analysis of real samples from the Biscay Coast, where TCAs were detected in both water and biota samples up to 25.9 ng/L and 1.8 ng/g, respectively. Up to our knowledge, this is the first work using FUSLE for the determination of TCAs and one of the few analyzing TCAs in biota samples.
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), PK. 644, 48080, Bilbao, Spain.
authors.forename: Haizea
authors.initials: H
authors.lastname: Ziarrusta
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), PK. 644, 48080, Bilbao, Spain.
authors.forename: Leire
authors.initials: L
authors.lastname: Mijangos
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), PK. 644, 48080, Bilbao, Spain.
authors.forename: Ailette
authors.initials: A
authors.lastname: Prieto
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), PK. 644, 48080, Bilbao, Spain.|Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/EHU), Areatza z/g, 48620, Plentzia, Basque Country, Spain.
authors.forename: Nestor
authors.initials: N
authors.lastname: Etxebarria
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), PK. 644, 48080, Bilbao, Spain. olatz.zuloaga@ehu.eus.|Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/EHU), Areatza z/g, 48620, Plentzia, Basque Country, Spain. olatz.zuloaga@ehu.eus.
authors.forename: Olatz
authors.initials: O
authors.lastname: Zuloaga
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), PK. 644, 48080, Bilbao, Spain.
authors.forename: Maitane
authors.initials: M
authors.lastname: Olivares
mesh_terms: D000818:Animals; D000929:Antidepressive Agents, Tricyclic / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D063366:Estuaries; D005399:Fishes; D005506:Food Contamination / Q000032:analysis; D057230:Limit of Detection; D008099:Liver / Q000737:chemistry; D018482:Muscle, Skeletal / Q000737:chemistry; D049878:Mytilus / Q000737:chemistry; D012623:Seawater / Q000032:analysis; D052616:Solid Phase Extraction / Q000379:methods; D013030:Spain; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D062065:Wastewater / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D000929:Antidepressive Agents, Tricyclic; D062065:Wastewater; D014874:Water Pollutants, Chemical
keywords: Environmental samples; Focused ultrasound solid–liquid extraction; Liquid chromatography-tandem mass spectrometry; Mix-mode cation exchange solid-phase extraction; Tricyclic antidepressants