title: Determination of endocrine disrupting compounds in fish liver, brain, and muscle using focused ultrasound solid-liquid extraction and dispersive solid phase extraction as clean-up strategy.
abstract: This study describes a new method for the simultaneous extraction of several endocrine disrupting compounds, including alkylphenols (APs), estrogen, bisphenol-A (BPA) and one phthalate metabolite (mono-2-ethylhexyl ester, MEHP) in fish liver, brain, and muscle. Parameters affecting the extraction (extraction solvent and temperature) and the clean-up (dispersive phase nature and amount) steps were evaluated. The extraction was performed by means of focused ultrasound solid-liquid extraction (FUSLE) using 10 mL of n-hexane:acetone (50:50, v/v) for 5 min at ~0 °C, and the clean-up was done by means of dispersive solid phase extraction (dSPE) using 100 mg of ENVI-CARB and 100 mg of MgSO4 for the cleaning of brain and muscle extracts together with 100 mg of PSA in the case of liver extracts. Good apparent recoveries were obtained in the case of liver (62-132 %), brain (66-120 %), and muscle (74-129 %), relative standard deviation (RSD%) was always below 26 %, and the method detection limits (MDLs) were at low ng/g level. The developed method was applied to fish captured in Urdaibai estuary (Bay of Biscay) in December 2015, and the concentrations obtained were in the range MDL-1115 ng/g in brain, MDL-962 ng/g in muscle, and MDL-672 ng/g in liver. In general, the highest concentrations were measured in liver, followed by brain and muscle. In addition, diethylstilbestrol was only detected in fish brain. Graphical Abstract MS method scheme for the/MS method scheme for the determination of EDCs in fish liver, brain and muscle.
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Basque Country, Spain. oihana.ros@ehu.eus.
authors.forename: Oihana
authors.initials: O
authors.lastname: Ros
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Basque Country, Spain.
authors.forename: Asier
authors.initials: A
authors.lastname: Vallejo
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Basque Country, Spain.
authors.forename: Maitane
authors.initials: M
authors.lastname: Olivares
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, 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), P.O. Box 644, 48080, Bilbao, Basque Country, Spain.
authors.forename: Ailette
authors.initials: A
authors.lastname: Prieto
mesh_terms: D000818:Animals; D001559:Benzhydryl Compounds / Q000032:analysis; D001921:Brain / Q000378:metabolism; D052244:Endocrine Disruptors / Q000032:analysis*; D004967:Estrogens / Q000032:analysis; D005399:Fishes / Q000378:metabolism*; D057230:Limit of Detection; D008099:Liver / Q000378:metabolism; D009132:Muscles / Q000378:metabolism; D010636:Phenols / Q000032:analysis; D010795:Phthalic Acids / Q000032:analysis; D052616:Solid Phase Extraction / Q000379:methods*; D013010:Sonication / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D052244:Endocrine Disruptors; D004967:Estrogens; D010636:Phenols; D010795:Phthalic Acids; D014874:Water Pollutants, Chemical; C032279:phthalic acid; C006780:bisphenol A; D000098826:Bisphenol A Compounds
keywords: Biota; Dispersive solid phase extraction; Endocrine disrupting compounds; Fish; Focused ultrasound solid–liquid extraction