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Copper-based nanomaterials have been widely used in catalysis, electrodes, and other applications due to their unique electron-transfer properties. In this work, an efficient electrochemical sensor based on an electrode modified with one-dimensional Cu(OH)2/carboxymethyl cellulose (CMC) composite nanofibers was fabricated and investigated for the detection of aspirin. Scanning electron microscopy was employed to examine the morphological characteristics of these composite nanofibers. Cyclic voltammetry and electrochemical impedance spectroscopy were used to assess the electrochemical performance of a Cu(OH)2/CMC composite nanofiber-modified electrode. The findings indicate that the modified electrode has a very high sensitivity to aspirin. The observed enhanced performance could be a result of the high surface-to-volume ratio of the composite nanofibers and their superior electron-transport characteristics, which may hasten electron transfer between aspirin and the surfaces of the modified electrode. This detection technique also demonstrated strong selectivity for aspirin. These findings imply that the technique can be applied as a highly effective and selective approach to aspirin measurement in biological science.