An analytical method for the determination of inorganic arsenic in fish samples using HPLC-ICP-MS has been developed. The fresh homogenised sample was subjected to microwave-assisted dissolution by sodium hydroxide in ethanol, which dissolved the sample and quantitatively oxidised arsenite (As(III)) to arsenate (As(V)). This allowed for the determination of inorganic arsenic as a single species, i.e. As(V), by anion-exchange HPLC-ICP-MS. The completeness of the oxidation was verified by recovery of As(V) which was added to the samples as As(III) prior to the dissolution procedure. The full recovery of As(V) at 104 +/- 7% (n=5) indicated good analytical accuracy. The uncertified inorganic arsenic content in the certified reference material TORT-2 was 0.186 +/- 0.014 ng g(-1) (n=6). The method was employed for the determination of total arsenic and inorganic arsenic in 60 fish samples including salmon from fresh and saline waters and in plaice. The majority of the results for inorganic arsenic were lower than the LOD of 3 ng g(-1), which corresponded to less than one per thousand of the total arsenic content in the fish samples. For mackerel, however, the recovery of As(III) was incomplete and the method was not suited for this fat-rich fish.
Analytical and Bioanalytical Chemistry, 2005, Vol 381, Issue 2, p. 339-346