The flexible, free-standing and durable highly rough nickel metal-organic framework/reduced graphene oxide (NiMOF/ rGO) composite paper electrode was prepared with a simple electrochemical deposition of NiMOF structures on the surface of the rGO paper electrode. NiMOF/rGO composite paper electrode was characterized by using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy and electrochemical impedance spectroscopy (EIS) techniques. As-prepared NiMOF/ rGO composite paper was used in the electrochemical detection of catechol (CC). The rough and flower-like three-dimensional (3D) NiMOF nanostructures on the rGO paper electrode surface greatly increased the catalytic performance of the paper electrode by providing a large active surface area. CC was detected on NiMOF/rGO composite paper in a very wide linear range from 0.02 to 760 μM, a low detection limit of 1.8 nM (S/N = 3), with a high sensitivity of 0.158 mA μM cm À 2 and very high selectivity, especially in the presence of phenolderived materials. Furthermore, it was determined that NiMOF/ rGO composite paper also had high stability, flexibility, and durability, which may enable this material to be used in-vivo applications.[a] Dr. durability, which makes it possible to use this material in in vivo applications. The interference study performed with the rGO paper electrode was shown to prove that the NiMOF/rGO composite paper electrode was very selective for CC compared to rGO paper.