期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 403, 期 10, 页码 2825-2834出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-012-6006-7
关键词
Inorganic arsenic; Marine samples; SPE HG-AAS; Microwave-assisted extraction; Food and feed control; Speciation
资金
- European Community's Seventh Framework Programme [211326]
- Committe Europeenne de Normalisation (CEN)
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 center dot kg(-1), respectively. The limit of detection was 0.08 mg kg(-1), and the repeatability (RSDr) and intra-laboratory reproducibility (RSDIR) 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.
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