A sensitive and selective sensor was fabricated to determine melamine (Mel), based on MIL-53@XC-72 nanohybrid modified glassy carbon electrode (GCE). The MIL-53@XC-72 nanohybrid was synthesized from MIL-53 via hydrothermal method, followed by adulterating with XC-72. The prepared sensor possessed high sensitivity and selectivity due to the synergistic effect of the large surface of MIL-53, the bonding interaction between Mel and MIL-53 as well as the high conductivity of XC-72. Under the optimal conditions, the sensor exhibited rapid electrochemical response to Mel at the potential of 0.7 V in 0.1 M HCl solution. A linear concentration range of Mel was obtained from 0.04 to 10 mu M with a linear correlation coefficient of 0.998 and detection limit of 0.005 mu M (S/N = 3). In addition, the sensor presented excellent reproducibility, high stability and selectivity, and was successfully applied for the determination of Mel in liquid milk with a good recoveries. Hence, the MOFs@XC-72-Nafion-GCE sensor could be considered as promising applicability for the determination of other electrochemically inactive analytes. (C) 2016 Elsevier Ltd. All rights reserved.