The development of promising magnetic nanocatalysts is one of the key research topics in the field of catalysis. This is because of their versatile surface physicochemical, magnetic, and size-dependent catalytic properties. Herein, an optimization strategy for the synthesis of high-value fuel grade chemicals from hydro-deoxygenation of biomass-derived furfural and vanillin using a nanostructured magnetic Fe(NiFe)O 4 -SiO 2 catalyst, synthesized by a facile one-pot procedure, was presented. Accordingly, effects of calcination temperature from 400, 500, 600 to 700 °C on the structure-activity properties of the magnetic Fe(NiFe)O 4 -SiO 2 catalyst was systematically studied. The magnetic Fe(NiFe)O 4 -SiO 2 catalyst calcined at 500 °C exhibited the best catalytic performance, giving full conversions of vanillin and furfural, with good selectivity of 63 and 59% to cyclohexane and n-pentane (fuel grade chemicals), respectively. The prowess of this catalyst was attributed to its abundant acid properties in addendum to high BET surface area. © 2019 by the authors.