In this research, bimetallic supported CNT modified electrode (Fe,Ni/CNTs/GCE) has been developed for sensitive, stable and highly elctroactive sensing of glucose, ascorbic acid and hydrogen peroxide. Transition metals such as Iron (Fe) and Nickel (Ni) offer high electrical and thermal conductance, high active surface‐to‐volume ratio and presence of d‐band electrons gives enhanced electrocatalytic behavior. While, CNTs provide high surface area, stability and excellent conductivity. Synthesized material is characterized by SEM, EDS, XRD and FTIR to access morphology, elemental composition and structure. This unique combination is employed for the electrochemical sensing of ascorbic acid, glucose and hydrogen peroxide and different experimental parameters are optimized. Fe,Ni/CNTs/GCE shows good sensing efficiency at pH 7.4 which is ideally suitable for variety of analytes. The modified electrode also show good reproducibility and sensitivity under optimized conditions and can be reused upto 30 cycles without compromising the efficiency. With good linearity, reproducibility and limit of detection, this material possess significant potential as non‐enzymatic biosensor for variety of analytes.