In the present paper, the technology of time-resolved fluorescence spectra was investigated in order to improve the sensitivity of the solid-phase time-resolved fluorescence immunoassay. The fluorescence properties, fluorescence intensity and detection method of the novel complexes 4,4′-dibromo-6,6′-bis(N,N-bis(ethoxycarbonylmethyl)amino methyl)-2,2′-bipyridine were investigated through self-developed solid-phase time-resolved fluorescence immunoassay instrument. At the same time, the Eu-TTA-phen and Eu-β-NTA-TOPO series of Eu(Ⅲ) compounds were detected.