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A novel electrochemical sensor based on ZrO2 and ZnO hybrid nanocomposites was developed for simultaneous determination of epinephrine (EA), uric acid (UA) and folic acid (FA) with the highly selective and ultrasensitive. The nanocomposites have been synthesized by chemical precipitation and thermal calcine method with economical, eco-friendly and practical nature. Their structure and electrochemical properties were investigated by X-ray diffraction (XRD), X-ray photo electron spectroscopy (XPS), scanning electron microscopy (SEM) and e