In this study, contaminations of metol (or Elon) in environmental water and industrial wastewater are the major causes of toxicity, which is very harmful to human health and other living things. Hence the determination of metol in high demand is more important. Further, the Mobil Composition of Matter (MCM-41) mesoporous silica nanoparticles incorporated with cobalt nickel oxide (CoNiO2) complex to form MCM-41/CoNiO2 composite modifying the glassy carbon electrode (GCE) used for metol detection. The MCM-41/CoNiO2 composite coated on the GCE surface exhibited fast electron transfer kinetics, improved conductivity, a large surface area, active stability, and improved catalytic efficiency. The structural morphology of the MCM-41/CoNiO2 composite was investigated using several spectroscopic and microscopic techniques. Here, the MCM-41/CoNiO2 composite was verified using different characterization studies such as Field Emission Scanning Electron Microscopy, Transmission Electron Microscopy, Energy Dispersive X-ray Analysis, X-ray Diffraction Analysis, and X-ray Photoelectron Spectroscopy. Additionally, the electrochemical investigations have included Electrochemical Impedance Spectroscopy, Cyclic Voltammetry, and Differential Pulse Voltammetry studies. The GCE/MCM-41/CoNiO2 electrode shows a low detection limit of 10 nM and the LOQ value is 0.1 μM with a broad linear response range of 0.1–750 μM, and greater sensitivity of 0.411 μA μM−1 cm−2 under optimal voltammetry.