The use of microwave-assisted extraction for the extraction of arsenic species from fish tissue is described. Quantitative extraction of arsenic from spiny dogfish muscle (CRM, DORM-2) was achieved using methanol-water (80+20, v/v) with microwave heating at 65 °C in a closed-vessel microwave system. Extractions were performed with a variety of solvents including water, two different methanol-water mixtures, and a 5% tetramethylammonium hydroxide solution. Extracted arsenic species were separated using both ion-exchange and ion-pair chromatography with ICP-MS detection. The DORM-2 along with three different varieties of fish purchased from a local market were analyzed for arsenic. In all samples, the majority of arsenic present was in the form of arsenobetaine, a nontoxic arsenic species. arsenic species of interest in seafood samples. Inductively
The enantiomeric separation of three underivatized seleno-amino acids, D,L-selenocystine, and D,L-selenomethionine, and D,L-selenomethionine, with UV and ICP-MS detection is described. An HPLC column with a chiral crown ether stationary phase and a mobile phase of 0.10 M HCIO4 was used. Absolute detection limits obtained with UV detection ranged from 34.5 to 47.1 ng whereas those obtained with the plasma detector were ca. 40-400 times better. The separations with either detector were good, with the little detector effect on the resolution. Ten commercially available dietary selenium supplements were analyzed using the chiral column to identify and quantify the selenium species present with both detection modes. Selenium species were easily identified using ICP-MS detection, whereas UV detection was not viable because of interferences from the sample matrix and inadequate sensitivity. Selenium species that were unretained using the chiral column were identified using anion exchange chromatography. Total amounts in the samples were also measured using a conventional digestion and enzymatic digestion with ICP-MS detection.
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