In the present study, magnetic ion-imprinted polymer (MIIP) synthesized by Pickering emulsion polymerization has been introduced as a selective adsorbent for ultrasonic-assisted solid phase extraction and preconcentration of Nickel (II). At the first step 2-acetyl benzofuran thiosemicarbazone as a chelating agent and core-shell hydrophobic magnetic nanoparticles (Fe3O4@OA) were synthesized. The polymerization process was carried out in the presence of stoichiometric ratio of ligandnickel ion, methacrylic acid, 2, 2′ azobisisobutyronitrile, chitosan nanoparticles and coreshell hydrophobic magnetic nanoparticles as the template, functional monomer, radical initiator, stabilizer agent, and water/oil emulsion magnetic carrier, respectively. The synthesized ligand and polymer were also characterized by FTIR analysis, Optical microscopy, SEM, EDX, vibrating sample magnetometer, XRD, Nitrogen adsorption– desorption isotherms, and the static water contact angles. The stoichiometric ratio of ligand to metal ion was investigated by the mole ratio method. The optimum conditions of the experiment was obtained by the multivariable design of experiments (BoxBehnken design) as 46 min for ultrasonic time, 7. 87 for pH and 78. 85 mg for adsorbent dosage. The selectivity, reusability, equilibrium, kinetic, and thermodynamic studies were also investigated in this research. Isotherm data of MIIPs well fitted the Langmuir model which indicated heterogeneous adsorption for Ni (II). Dynamic linear range, detection limit, and relative standard deviation (RSD) of the proposed method were reported as 0. 001 – 70 mg/l, 0. 004 and 3. 21%, respectively by atomic absorption technique. Trace determination of Ni (II) in some fish samples such as salmon, Tuna, Tilapia, butter fish was successfully carried out by the proposed method.