A hierarchical nickel shell anchored on silica coated magnetic Fe 3 O 4 @SiO 2 nanospheres (MNPs) has been designed and constructed that combined the capacity of effective adsorption for protein bovine hemoglobin (BHb) and selective deletion BHb from the bovine blood real sample. Firstly, -NH 2 modified silica/ magnetite nanoparticles (Fe 3 O 4 @SiO 2 -NH 2 ) were synthesized by the combination of a sol-gel method and refluxing process. The Fe 3 O 4 @SiO 2 -NH 2 composites revealed a core-shell structure, and the thickness of silica shell can be 10 easily adjusted by controlling the amount of ammonium solution. Then, hierarchical nickel shell were anchored on the surface of Fe 3 O 4 @SiO 2 -NH 2 by reducing Ni 2+ between the Fe 3 O 4 @SiO 2 -NH 2 solid and nickel solution with NaBH 4 . By taking advantages of the high affinity of Ni 2+ on the shell surface toward His-tagged proteins and the fast response toward an assistant magnet, the heteronanoparticles can be applied to selectively bind to and magnetically separate of BHb from the bovine blood. Significantly, it is expected that this approach can be extended to other bimolecular separation and purification.