Development of highly efficient and potential material for toxic p-nitrophenol is an important design for sensitive detection of hazardous species from ecology and environment. Here it is developed, an efficient as well as selective of p-nitrophenol using binary material by electrochemical performances, including good linearity, lower detection limit, good stability, higher reproducibility and extreme sensitivity. The prepared electrode was fabricated by immobilization of SnO2/CdO microcubes (MCs) with conducting coating binders by using well-known glassy carbon electrode (GCE). The proposed MCs with SnO2/CdO were well-functionalized and prepared by facile hydrothermal technique. The general instrumentation namely, FTIR, UV/vis, FESEM, XPS, TEM, EDS, and powder XRD were employed for the morphological evaluation of the prepared doped MCs, structural, optical and elemental analyses. The large dynamic range (LDR) from 1.0 to 0.01 mM with 0.13 pM detection limit (S/N = 3), limit of quantification (LOQ; 0.43 pM), and an excellent sensitivity of 7.12 µAµM−1cm−2 were exhibited by the fabricated binary material based on SnO2/CdO MCs for selective p-nitrophenol capturing. In shortly, the SnO2/CdO MCs can be employed as an efficient electron mediator with binary materials fabricated GCE for capturing the p-nitrophenol at ultra-trace amounts. Then the binary synthesized material of SnO2/CdO MCs is used as potential and sensitive sensor layer by stable electrochemical approach for sensitive capturing of toxic p-nitrophenol from environmental samples.