Herein, at first, a magnetite@MIL-53(Fe)-NH 2 core-shell nanocomposite was fabricated and then modified via postsynthetic modification by dithiocarbamate moieties to obtain a magnetite@MIL-53(Fe)-NH-CS 2 nano-adsorbent.The constructed material was used for extraction/separation of ultra-trace Hg (II) from seawater, river water, and fish samples, and then the enriched mercury was quantified by CVAAS instrument. Characterization of magnetite@MIL-53(Fe)-NH-CS 2 nano-adsorbent was carried out by scanning electron microscopy, X-ray diffraction analysis, CHNS analysis, FT-IR spectroscopy, and magnetometry. Optimization of the affecting variables was conducted via the design of experiment methodology. After that, adsorption isotherms and kinetic studies were carried out. The experimental data were well fitted to the Langmuir and pseudo second-order kinetic models for adsorption study and kinetic study, respectively. Accordingly, a maximum adsorption capacity and a Langmuir constant (K L ) of 250 mg g À1 and 0.102 L mg À1 were obtained, respectively. The LOD and linearity of the preconcentration method were