In the present study, a facile method was proposed to prepare nickel sulfide (NiS) nanoparticles well-dispersed on the surface of montmorillonite/graphene oxide (MMT/GO). The NiS/MMT/GO nanocomposites were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), fluorescence spectrophotometry, etc. Significantly, the novel NiS/MMT/GO nanocomposites exhibited high peroxidase-like activity toward the typical chromogenic substrate, 3,3′,5,5′-tetramethylbenzidine (TMB). However, glutathione (GSH) could inhibit the peroxidase-like activity of NiS/ MMT/GO along with a visible color variation. Based on the color change of the system of nanocomposites-H 2 O 2 -TMB, a novel colorimetric sensor was designed and conveniently used to quantitatively detect H 2 O 2 as well as GSH. The limit of detection (LOD) of H 2 O 2 and GSH is 9.73 and 0.5043 μM, respectively. The proposed H 2 O 2 sensor has potential application in the field of biosensing, food, and environment.