摘要： A simple and sensitive derivative synchronous fluorescence spectrometry with double scans (DS-DSFS) method was developed for simultaneous determination of dissolved Phenanthrene (Phe) and its metabolites 1-hydroxy-2-naphthoic acid (1H2NA) and salicylic acid (SA) in aqueous solution. The value of 69 nm was selected as the optimal Δλ conditions for Phe and 1H2NA, and the Δλ value of 55 nm was selected for SA. The overlapping fluorescence emission spectra of Phe, 1H2NA and SA were resolved by DS-DSFS. The signals detected at wavelength of 296 nm for Phe, 352 nm for 1H2NA and 307 nm for SA vary linearly when the concentrations in the range of 4.0–1.0 × 103 μg L?1, 4.0–1.2 × 103 μg L?1 and 4.0–8.0 × 102 μg L?1, respectively. The detection limits were 0.08, 0.07 and 0.88 μg L?1 for Phe, 1H2NA and SA, with the relatively standard deviations less than 5.0%. The established method was successfully applied in the determination of Phe and the metabolites during the biodegradation of dissolved Phe in the lab. It was evidenced that the method has potential for the in situ investigation of PAH biodegradation.