Abstract：Terbium(Ⅲ) can react with Pefeoxacin(PEFX) to form 1∶2 coordination compound in a near neutral medium. Based on this reaction, we proposed a simple, rapid, and sensitive new method for the fluorimetric determination of Pefeoxacin and investigated the reaction conditions in detail;meanwhile we discussed the efficiency and mechanism of the intramolecular energy transfer. The results show that in the range of 0.01-1.67 μg·mL-1, there is a linear relationship between the concentration of PEFX and its fluorescence intensity, and the regression equation is F=120.01 C+2.608，with the detection limit of 0.01 μg·mL-1, the recovery within the range of 95.2%-101.7%，and the RSD of 2.9%-3.0%. This method has been successfully applied to the determination of Pefeoxacin in untreated human serum and gelatine capsule.
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