The rapid and accurate detection of hydrogen peroxide (H 2 O 2 ) has recently been a fascinating research topic in electrochemical sensing. Herein, spinel CuMn 2 O 4 nanoflakes were synthesized through coprecipitation and pyrolysis methods and then dropcoated onto the surface of a bare glassy carbon electrode (GCE), successfully generating an enzymatic-free electrochemical sensor (CuMn 2 O 4 /GCE) for good amperometric detection ability of H 2 O 2 . In comparison with the reported spinel AB 2 O 4 -based electrocatalysts in a phosphate buffer solution, the CuMn 2 O 4 /GCE sensor exhibits a high sensitivity of 3.420 A M −1 cm −2 and a low detection limit of 12 nM. This excellent sensing performance is mainly derived from the inherent porous structure and the large electrochemical active area of spinel CuMn 2 O 4 nanoflakes, as well as the synergistic effect between Cu and Mn that facilitates electron transfer and increases active sites. Especially, the high contents of Cu + and Mn 3+ ions in the nanocatalyst are useful for promoting the capture and reduction of trace H 2 O 2 . In addition, the CuMn 2 O 4 /GCE sensor presents a satisfactory recovery in monitoring H 2 O 2 derived from rat serum, commercial milk, and disinfectors, indicating its potential applications in related environmental, food, and biological fields. KEYWORDS: spinel oxides, CuMn 2 O 4 , H 2 O 2 , electrochemical sensor, nanoflakes