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A flower-like CePO4 (F-CePO4) with a hierarchical structure was hydrothermally prepared. Comparative experiments showed that the amounts of hydrazine hydrate and urea as well as the reaction time significantly affect the formation of nanoflowers. Due to its large specific surface area and high electron transfer efficiency, F-CePO4 was utilized for the selective detection of dopamine (DA), uric acid (UA) and acetaminophen (APAP) with wide linear ranges, low detection limits, high stability, and good repeatability. Fascinatingly, when DA, UA and APAP were detected simultaneously, the high sensitivity of F-CePO4 can be maintained. Further studies showed that different electrostatic and hydrogen bonding interactions between the detected substrates and F-CePO4 lead to different shifts of their oxidative peak potential. Then, DA, UA and APAP were well identified. In addition, F-CePO4 can also be used for real sample detection. This work provides a simple strategy for the construction of new effective electrochemical sensing materials. [ABSTRACT FROM AUTHOR]