Hybrid nanocomposites (NCs) of Mn3O4 nanorods and 2D materials (MoS2 or graphene) nanosheets are successfully deposited on nickel foam porous substrate at room temperature using a one-step kinetic spray process in low-vacuum conditions. Mn3O4-based NCs are utilized for the electrocatalytic detection of H2O2 in 0.1 M NaOH. The synergy improvement between the Mn3O4 nanorods and either MoS2 or graphene nanosheets improved the non-enzymatic detection of H2O2. All modified electrodes exhibit a wide linear detection range from 0.2 to 1 mM. The working electrodes with Mn3O4 nanorods reveal high sensitivity of 2320 μA mM?1 cm?2 toward H2O2 reduction. The hybridization between Mn3O4 nanorods and either MoS2 or graphene enhances the electrocatalytic reduction sensitivity to 3220 or 5400 μA mM?1 cm?2, respectively. Furthermore, the modified electrodes with the Mn3O4-2D material hybrid NCs exhibited high electrocatalytic reduction selectivity for H2O2 in 0.1 M NaOH compared with other interfering species.