We developed the zirconium dioxide anchored carbon nanofiber (ZrO2/CNF) composite modified glassy carbon electrode (GCE) for the enhanced and selective electrochemical determination of chloramphenicol (CPL). The as-prepared composite was characterized by different analytical and spectroscopic techniques. The voltammetry techniques were used to evaluate the electrochemical activity of ZrO2/CNF composite. Its electrochemical behavior and the roles of ZrO2 and CNF in the composite toward electrochemical reduction of CPL were elucidated and demonstrated using voltammetry techniques. The ZrO2/CNF modified GCE displayed the enhanced electrocatalytic behavior and reduction peak current response toward for the detection of CPL than that of other modified electrodes. The detailed electrochemical reasons on such excellent performance were also discussed. Differential pulse voltammetry (DPV) is a suitable electrochemical technique to measure CPL reduction, which determined the CPL in the linear range from 0.005 to 903.76 mu Mand with the lowest detection limit (LOD) of 0.0018 mu M. The ZrO2/CNF modified GCE shows its excellent selectivity toward CPL in the presence of antibiotics and sulfa drug. Also, the viability of the raised method has been preliminarily examined by the analysis of CPL in real spiked samples. All these features indicate that the ZrO2/CNF composite is a promising candidate as a new class of electrocatalyst in the development of highly selective CPL electrochemical sensor. (c) 2018 The Electrochemical Society.