In this paper a novel and simple route for the preparation of magnesium aluminate (MgAl 2 O 4 ) is proposed. The method was developed with the objective of obtaining a material with more porous structure and greater surface area compared with other spinel preparation methods, based on the formation of a metal–chitosan complex. The structural properties of the material were investigated by X-ray diffraction (XRD), N 2 adsorption/desorption isotherms (BET and BJH methods), infra-red (IR) spectroscopy and thermogravimetric analysis (TGA). Through this route, porous MgAl 2 O 4 powder with a high specific surface area was obtained at low temperature.