In this work facile one step synthesis of magnesium ferrite (MgFe2O4) nanoparticles decorated on reduced graphene oxide (MgFe@RGO) using a microwave assisted hydrothermal procedure is reported. The synthesized material was characterized with help of several techniques and applied for the modification of glassy carbon electrode. Such prepared electrode was utilized for successive simultaneous detection of structurally similar compounds, 1,2‐ and 1,4‐dihydroxibenzenes (catechol (CC) and hydroquinone (HQ)), using differential pulse voltammetry technique. It was found that oxidation current increases linearly with the concentrations of both investigated compounds. Detection limits for both species are ≤0.31 μM. The best analytical response in the presence of both CC and HQ, taking into account peak shape and peak current, was obtained at pH 5.6 utilizing acetate buffer solution. The often‐presented species in the surface waters as well as gallic acid and caffeine do not interfere with determination of CC and HQ, while ascorbic acid shows high interference. The method is successfully applied for detection of catechol and hydroquinone in real samples analyses.