In this research study, the combination of Fe3O4@SiO2 nanocomposite as the nanostructure and a deep eutectic solvent (oceanic acid: cumarine) and dispersive solid phase extraction was used as a green method for simultaneous separation and preconcentartion of nickel and cobalt which determined by MP-AES. The effect of important parameters was studied. At optimum conditions, the linear range of 10-500 µg kg-1, LOD of 3.2 and 3.1 µg kg-1 and LOQ of 10.5, 10.3 µg kg-1 were achieved for nickel and cobalt respectively. The repeatability (intra–day precision (n=5)) of ≤ 2.6 and 2.5 % for nickel and cobalt respectively and reproducibility (inter–day precision, days=5, n=3) of ≤3.3 % and were appraise at two concentration levels (50 and 100 μg kg-1). High relative recoveries of 91.2-99.3 % confirmed high potential of the presented method.