Abstract
Ultrasound-assisted extraction of As, Se, Ni and V from fish and shellfish has been applied as a fast and reliable sample pre-treatment method for accurate determination of the four elements by electrothermal atomic absorption spectrometry with Zeeman (As, Se) or Deuterium (Ni, V) background correction. A multivariate optimization approach has been employed for establishing the effect of variables influencing the extraction process. Under suitable conditions, quantitative extractions occurred from a 10 mass sample (particle size <100 μm) suspended in 1.5 mL of acidic extractant (0.5 or 3% v/v HNO 3) and subjected to high intensity ultrasound (50% amplitude; 3 min). The method was successfully validated against the following certified reference materials: NRCC-DORM-2 dogfish muscle, NRCC-DOLT-2 dogfish liver, NRCC-TORT-2 lobster hepatopancreas, NIST-SRM 1566b oyster tissue and BCR 627 tuna fish. The following seafood samples were analyzed: hake ( Merluccius merluccius), sole ( Solea solea), clam ( Venerupis rhomboides), prawn ( Panaeus kerathurus), cuttlefish ( Sepia officinalis), shrimp ( Palaemon elegans), razor shell ( Ensis ensis), cockle ( Cardium edule), Mussel ( Mytilus galloprovincialis), edible crab ( Cancer pagurus), meagrin ( Lepidorhombus whiffiagonis). The concentration ranges (μg/g, dry weight) for the elements determined were as follows: As (12.6–190), Se (0.73–2.34), Ni (2.94–46) and V (0.82–5.14). The detection limits (LODs), defined as 3 s/m ( s being the standard deviation of 10 blank and m the slope of the calibration graph), in dry tissue were 0.6, 0.3, 0.2 and 0.4 μg/g for As, Se, Ni and V, respectively. Between-batch precision was expressed as relative standard deviation from three separate extractions was in the range 3–10%.
Published Version
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