In this work, we propose a bimetallic Ni-Co based MOF attached to graphene oxide (GO) by a one-step hydrothermal approach which may be employed as an electrochemical enzyme-free glucose sensor. Due to the obvious synergistic catalysis of Ni and Co, as well as the combination of NiCo-MOF and GO, NiCo-MOF/GO not only enhances energy transfer and electrocatalytic performance but also provides a larger surface area and more active sites. Electrochemical studies show that NiCo-MOF/GO exhibits outstanding electrochemical activity, with a sensitivity of 11 177 μA mM-1 cm-2 and 4492 μA mM-1 cm-2 in the linear ranges of 1-497 μM and 597-3997 μM, a detection limit of 0.23 μM, and a response time of 2 seconds. More importantly, the newly fabricated sensor is successfully applied for glucose determination in huangshui. This method provides a novel strategy for the controlled fermentation process and product quality of Chinese baijiu.