A NiFe2O4 and reduced graphene oxide (RGO) composite has been synthesized by one-pot microwave-assisted combustion method, characterized and tests for thiophenes capture from model diesels. The composite exhibits excellent performance for adsorption desulfurization. When 100 mg-S/Kg of thiophenes in n-octane used as model fuel, the maximal adsorption capacities are about 1.05 mmol-S/g (which are 3-4 times higher than that of RGO) and less affected by the competitive adsorption of the added p-xylene. The adsorption kinetics and the equilibrium isotherm data for all species over the composite are well compliant with the pseudo-second order model and the Freundlich model, respectively. Additionally, the composite could be easily separated by external magnetic field. The regeneration of the composite by solvent extraction afforded 89-80% of the initial adsorption capacities after the first three regeneration cycles.