In the present study, the synthesis of sea urchin-like α-FeOOH (U-FeOOH) and NiO microspheres (MSs) was performed, and their in uence on a chemiluminescence (CL) reaction, namely the luminol – O2 reaction, was demonstrated. This research marks the rst application of U-FeOOH MSs as a catalyst in a CL reaction. The comparison of catalytic characteristics of U-FeOOH and NiO MSs revealed that both types of MSs exhibit a comparable enhancement in light intensity of CL reaction. Two novel methods employing U-FeOOH MSs and NiO MSs were utilized to measure sunitinib malate (SM), an anti-cancer medication, using a luminol – O2 CL reaction. This study presents an initial report regarding the quantitative determination of SM by applying a CL method. The foundation of the CL methods lies in the quenching property exhibited by SM towards CL reactions. The method utilizing the U-FeOOH MSs – luminol – O2 system demonstrated a linear range between 2.00 × 10− 7 and 2.00 × 10− 5 mol/L. Similarly, the method employing NiO MSs – luminol – O2 system displayed a linear range spanning from 1.00 × 10− 7 and 1.00 × 10− 5 mol/L. The aforementioned systems were employed for the quanti cation of SM in both bulk powder SM and human plasma samples. The mechanism underlying the CL reactions was concisely elucidated.
