Nanozymes as one of artificial enzymes show many advantages than natural enzymes. The high Michaelis-Menten constant () to HO is the drawback for nanozymes, which means a high HO concentration to oxidize 3,3',5,5'-tetramethylbenzidine (TMB). For this problem, FeS/SiO double mesoporous hollow spheres (DMHSs) were first synthesized as an artificial peroxidase through a solid reaction. The experimental results demonstrate that FeO vulcanization and DMHS formation were effective strategies to enhance affinity to HO for the nanozyme. The of FeS/SiO DMHSs (HO as the substrate) is 18-fold smaller than that of FeS nanoparticles (NPs). The catalytic efficiency (/) of FeS/SiO DMHSs is about 16 times higher than that of FeS NPs. FeS/SiO DMHSs can be used as a nanozyme to sensitively and rapidly detect HO and glutathione within 1 min at room temperature.