金属-有机框架（MOF）纳米材料因其独特性质显著促进了电化学传感器的发展。合理设计双金属MOF并集成与微电极对于提高电化学性能至关重要，但仍然面临巨大挑战。本工作中通过原位电沉积方法将双金属FeCo-MOF纳米材料组装于金超微电极（Au UME，直径约为5.2 µm）表面，并应用于肾上腺素（EP）的电化学检测。FeCo-MOF呈现类纳米花结构，均匀分散在超微电极基底上。FeCo-MOF/Au UME在EP检测中表现出较好的电化学性能，具有高灵敏度36.93 μA μM^-1 cm^-2和低检测限1.28 μM。这可归因于EP在超微电极基底的非线性快速传质特点，以及基于MOF结构中Fe、Co双金属的协同催化效应。此外，我们将FeCo-MOF/Au UME成功应用于人血清样本中EP的检测，且表现出较高回收率。本研究工作不仅有助于扩展电化学传感器研究领域，还将为设计开发基于MOF纳米敏感材料的微纳电化学传感器件提供指导和借鉴。

Metal-organic framework (MOF) nanostructures have emerged as a prominent class of materials in the advancement of electrochemical sensors. The rational design of bimetallic MOF-functionalized microelectrode is of importance for improving the electrochemical performance but still in great challenge. In this work, bimetallic FeCo-MOF nanostructures were assembled onto a gold disk ultramicroelectrode (Au UME, 5.2 µm in diameter) via an in-situ electrodeposition method, which enhanced the sensitive detection of epinephrine (EP). The FeCo-MOF, characterized by a nanoflower-like morphology, was uniformly dispersed on the ultra-micro substrate. The FeCo-MOF/Au UME demonstrated excellent electrochemical performance on the detection of EP with a high sensitivity of 36.93 μA μM^-1 cm^-2 and a low detection limit of 1.28 μM. It can be attributed to the non-linear diffusion of EP onto the ultra-micro working substrate, coupled with synergistical catalytic activity of the bimetallic Fe, Co within MOF structure. Furthermore, FeCo-MOF/Au UME has been successful applied to the analysis of EP in human serum samples, yielding high recovery rates. These results not only contribute to the expansion of the research area of electrochemical sensors but also provide novel insights and directions for the development of high-performance MOF-based electrochemical sensors.