Analytical Method for the Determination of Trace Toxic Elements in Milk Based on Combining Fe₃O₄ Nanoparticles Accelerated UV Fenton-like Digestion and Solid Phase Extraction

Abstract

A UV Fenton-like digestion method was developed first time for a complete digestion of milk samples by using 1.6 g L(-1) Fe3O4 magnetic nanoparticles, 0.2% (v/v) nitric acid, and 6% (w/w) H2O2. During the digestion, the liberated As-, Sb-, and Bi-containing species were preconcentrated onto the surface of Fe3O4 magnetic nanoparticles, which were conveniently separated with a hand-held magnet and subsequently dissolved in hydrochloric acid prior to hydride generation atomic fluorescence spectrometric detection. Owing to the integration of UV Fenton-like digestion, solid phase extraction, and magnetic separation into a single step, the developed method significantly simplifies sample preparation steps and reduces chemical consumption and hazardous waste. Limits of detection of 0.0015, 0.0022, and 0.0025 μg L(-1) were obtained for As, Sb, and Bi, respectively, using a 50 mL milk sample. The method was applied to the determination of these elements in a Certified Reference Material and milk samples.