Measurement of arsenic species in marine macroalgae by microwave-assisted extraction and high performance liquid chromatography–inductively coupled plasma mass spectrometry Original Research Article

The measurement of arsenic species (arsenoribosides, arsenate, dimethyl arsenic and monomethyl arsenic) in marine macroalgae by microwave-assisted extraction and HPLC–ICP-MS is described. The extraction of arsenic from three different macroalgae classes was optimised using a chemometric approach, with solvent composition and sample mass being the two significant factors influencing the extraction of arsenic. Extraction temperature and extraction time did not significantly influence the extraction of arsenic from macroalgae. The optimised conditions for arsenic extraction (methanol (%)) were: 56% for phaeophyta, 66% for rhodophyta and 78% for chlorophyta, (sample mass in 10 ml of solvent) 0.05 g for phaeophyta, 0.07 g for rhodophyta and 0.08 g for chlorophyta. When two extractions were used, the percentage of arsenic extracted from macroalgae was greater than 88%. Unambiguous separation and identification of three arsenoribosides (phosphate-, sulfonate- and sulfate-arsenoriboside) was achieved by chromatographing extracts on a Hamilton PRP X-100 anion exchange column with ammonium phosphate buffer as the mobile phase at a pH of 9.2. The unambiguous separation and identification of the glycerol-arsenoriboside was achieved by chromatographing extracts on a Supelcosil SCX cation exchange column with a pyridine–formic acid buffer as the mobile phase at a pH of 2.6.