title: Development and validation of an SPE HG-AAS method for determination of inorganic arsenic in samples of marine origin.
abstract: The present paper describes a novel method for the quantitative determination of inorganic arsenic (iAs) in food and feed of marine origin. The samples were subjected to microwave-assisted extraction using diluted hydrochloric acid and hydrogen peroxide, which solubilised the analytes and oxidised arsenite (As(III)) to arsenate (As(V)). Subsequently, a pH buffering of the sample extract at pH 6 enabled selective elution of As(V) from a strong anion exchange solid-phase extraction (SPE) cartridge. Hydride generation atomic absorption spectrometry (HG-AAS) was applied to quantify the concentration of iAs (sum of As(III) and As(V)) as the total arsenic (As) in the SPE eluate. The results of the in-house validation showed that mean recoveries of 101-104% were achieved for samples spiked with iAs at 0.5, 1.0 and 1.5 mg·kg(-1), respectively. The limit of detection was 0.08 mg kg(-1), and the repeatability (RSD(r)) and intra-laboratory reproducibility (RSD(IR)) were less than 8% and 13%, respectively, for samples containing 0.2 to 1.5 mg kg(-1) iAs. The trueness of the SPE HG-AAS method was verified by confirming results obtained by parallel analysis using high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry. It was demonstrated that the two sets of results were not significantly different (P < 0.05). The SPE HG-AAS method was applied to 20 marine food and feed samples, and concentrations of up to 0.14 mg kg(-1) of iAs were detected.
authors.affiliation: National Food Institute, Division of Food Chemistry, Technical University of Denmark, Søborg, Denmark.
authors.forename: Rie R
authors.initials: RR
authors.lastname: Rasmussen
authors.forename: Rikke V
authors.initials: RV
authors.lastname: Hedegaard
authors.forename: Erik H
authors.initials: EH
authors.lastname: Larsen
authors.forename: Jens J
authors.initials: JJ
authors.lastname: Sloth
mesh_terms: D059001:Aquatic Organisms / Q000737:chemistry*; D001151:Arsenic / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D005502:Food; D005504:Food Analysis / Q000379:methods* / Q000592:standards*; D057230:Limit of Detection; D013058:Mass Spectrometry; D015203:Reproducibility of Results
chemical_list: D001151:Arsenic