The fabrication of hierarchical nanostructure based on metal–organic frameworks (MOFs)-derived transition-metal phosphides (TMPs) has become a hot topic in electrochemical sensor application owing to its unique properties. Herein, a scalable and facile strategy was proposed to prepare MOF-derived bimetallic Zn-Ni-P nanostructures. The material characterization showed that MOFs-derived Zn-Ni-P has flower-like structure that built from small 2D nanosheets. The MOFs-derived Zn-Ni-P was prepared via a facile phosphorization of Zn-Ni-MOF precursor in N2 atmosphere. This MOF-derived TMPs electrode materials offer excellent electrocatalytic activity toward isoprenaline (IPN) oxidation. In addition, the electrode shows wide two linear range (0.2 µM −5 mM and 5 mM-14 mM), short response time (<1s), low detection limit (0.06 µM), good sensitivity (66.748 μA mM−1), desirable repeatability and reproducibility (RSD < 3.5%), and capability for measuring IPN in real sample, which are comparable or better than most reported works for measuring IPN. This improvement can be due to the synergistic effects of multiple catalytic centers, high surface area, facilitated mass, and electron transfer.