Here, we synthesized bimetallic Ni/Fe MOFs using 2-aminoterephthalic acid (NH2-BDC) as ligand by a facile hydrothermal route. After calcination, spindle-like Ni/Fe MOFs are transferred into porous NiFe2O4 nanorods. The resulting NiFe2O4 based sensor shows an excellent sensitivity (almost 60-500 ppm), good selectivity against various VOCs, and a good linearity in wide concentration and stability for toluene detection. Three major aspects of good catalytic activity, large surface area, and porous structures of NiFe2O4 are significantly attributed to the excellent gas-sensing performances. These findings demonstrate a new perspective of bimetallic Ni/Fe MOFs-derived NiFe2O4 for the promising application in toluene gas sensor.