A novel electrochemically activated ZrO2 nanoparticles modified carbon paste electrode (CPE) (ZrO2-CPE(ox)) was prepared and applied for selective and sensitive determination of hyperin. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectra and electrochemical experiment were used to characterize the ZrO2 nanoparticles and investigate the electrochemical performance of the ZrO2-CPE(ox). Compared with bare CPE and electrochemically activated CPE (CPE(ox)), the ZrO2-CPE(ox) got more reactive sites by electrochemical treatment and exhibited larger effective surface area and more excellent electrochemical catalytic activity toward the redox of hyperin. Under the optimum conditions, the oxidation peak currents showed a linear relationship with the concentrations of hyperin in the range of [Formula: see text]–[Formula: see text][Formula: see text]mol[Formula: see text]L[Formula: see text] and [Formula: see text]–[Formula: see text][Formula: see text]mol[Formula: see text]L[Formula: see text], and a low detection limit of [Formula: see text][Formula: see text]mol[Formula: see text]L[Formula: see text] was achieved for hyperin. Moreover, the proposed method exhibited an excellent selectivity, stability, reproducibility and repeatability, which make it very suitable for a potential choice for determining the concentrations of hyperin in drug matrices.
