A renewable three-dimensional chemically modified carbon ceramic electrode (CCE) containing nickel powder and K4[Mo(CN)8] was constructed by sol–gel technique. The electrochemical properties and stability of modified electrode was evaluated by cyclic voltammetry in pH range 4–10. The redox couple of [Mo(CN)8] 4−/3− was shown both as a solute in electrolyte solution and as a component of a carbon based conducting composite electrode. The apparent electron transfer rate constant (ks) and transfer coefficient (α) were determined by cyclic voltammetry and they were about 17.1 and 0.57 s−1, respectively. The catalytic activity of the modified CCE toward insulin oxidation was investigated at pH range of 3–8 by cyclic votammetry. The modified electrode showed excellent electrocatalytic activity toward insulin electroxidation at physiological pH value. The modified electrode was used for insulin detection chronoamperometrically at pH 7. Under optimized condition in amperometry method, the concentration calibration range, detection limit and sensitivity were 0.5–500 nM, 0.45nM and 6140 nA/M, respectively. Flow injection amperometric determination of insulin at pH 7.4, at this modified electrode yielded a calibration curve with the following characteristics, linear dynamic range 100–500 pM; sensitivity 8.1 nA/nM and detection limit 40pM (based on S/N = 3). The inherent stability at wide pH range, high sensitivity, low detection limit, low cost and ease of preparation are of advantageous of this insulin sensor. This sensor indicates great promise for monitory insulin in chromatographic effluents.