This study developed and optimized a liquid chromatography hyphenated with inductively coupled plasma mass spectrometry (LC-ICP-MS) method for the simultaneous determination of iodine (iodide and iodate) and bromine species (bromide and bromate) in dairy products. Samples were extracted with a 10 mM ammonium carbonate solution containing 0.5 mM Mg-EDTA, then analyzed by LC–ICP–MS using an anion-exchange column (Shodex NI-424, 5 µm × 4.6 mm × 150 mm) and a mobile phase of 50 mM ammonium carbonate containing 1% methanol (pH = 10). The limits of quantification (LOQs) for iodate, iodide, bromate, and bromide in liquid milk matrices were established at 1.10, 1.77, 8.50, and 12.2 µg/100g, respectively. The corresponding values for solid samples were found to be 5.50, 8.90, 42.5, and 61.0 µg/100g. The method repeatability ranged from 1.90% to 6.01%, with recoveries between 86.3% and 109.8%, meeting AOAC performance criteria. Analysis of 26 commercial milk samples from Hanoi showed no detectable iodate or bromate. Iodide concentrations were highest in powdered milk (13.5 – 203 µg/100g) and lowest in liquid milk (1.29–34.4 µg/100g). Bromide was detected in most products, with the highest levels in powdered milk (996– 2229 µg/100g), followed by liquid milk (5.60 – 397 µg/100g) and yogurt (259 – 383 µg/100g). The results confirm that LC-ICP-MS is a robust and reliable technique for the simultaneous determination of iodine and bromine species in dairy products, providing essential data for nutritional evaluation and food safety assessment.
iodate, iodide, bromate, bromide, LC-ICP-MS, dairy products.
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