This work deals with preparation and characterization of metal complex hydrogels based on crosslinked chitosan with hyperbranched polyester generation 2. These materials were prepared using miniemulsion technique with different ratios. Besides, the metal complexes using Co, Ni and Fe salts were investigated. All the prepared materials were characterized using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), particle size and zeta potential analysis using dynamic light scattering (DLS) technique. Moreover, XRF was also carried out. The results indicated that the successful network structures were obtained with particle size ranged between 118 and 148 nm. In addition, high performance metal complexes were prepared with metal percentages about 6.55, 7.01 and 6.56 (wt%), in the case of Co, Ni and Fe, respectively. Moreover, thermal analysis revealed that hydrogen bonds played an important role for hydrogel networks formation.