In this study, the fluorescent carbon dots (CDs) of good biocompatibility and low toxicity was prepared by a carbonation route, and a strong enhancement effect of CDs on the luminol-K 3 Fe (CN) 6 chemiluminescence (CL) system was observed. 5 ± 1 nm CDs were used as catalysts to enhance the reaction sensitivity. In the presence of 2-methoxyestradiol (2-ME), the CL intensity of CDs-luminol-K 3 Fe(CN) 6 was significantly inhibited. The relative CL intensity was linearly related to the 2-ME concentration in the range of 1.0 × 10 −9-1.0 × 10 −7 g mL −1 with a lower detection limit of 4.1 × 10 −10 g mL −1. As a preliminary application, the highly sensitive method was successfully applied to the determination of 2-ME in both pharmaceutical preparation and serum samples with satisfactory results. The possible mechanism of CL reaction catalyzed by CDs was investigated and the CDs played a role of catalyst in the reaction which could promote the generation of oxygen radicals. It could be concluded that the enhancement effect on CL by CDs was attributed to the formation of oxygen radicals. The oxidation reaction of luminol was accelerated by oxygen radicals, which led to the enhanced CL emission.
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