A new magnetic adsorbent, 2,2 0 -thiodiethanethiol grafted with tetraethyl orthosilicate modified Fe 3 O 4 nanoparticles, was developed for the separation and preconcentration of Hg, Pb, and Cd in environmental and food samples. The concentrations of Pb and Cd were determined by inductively coupled plasma-optical emission spectrometry; Hg was determined by cold vapor atomic absorption spectrometry. A comprehensive study on the factors affecting the extraction and desorption efficiencies was performed. Under the optimized conditions, the method was linear in the 0.01-750 ng mL À1 range (before preconcentration) with detection limits of 4, 8, and 2 ng L À1 for Hg, Pb, and Cd, respectively. Relative standard deviations of 2.3, 2.9, and 2.4% (concentration 50 ng mL À1 , n ¼ 7) and high preconcentration factors of 291, 285, and 288 were also obtained for Hg, Pb, and Cd. The accuracy of the proposed method was validated by analyzing a water certified reference material with satisfactory recoveries. The method was successfully applied to the determination of the analytes in tap and mineral waters and canned tuna fish samples.