A sensitive method was developed for the purification and determination of bisphenol A and alkylphenols in river sediments by using 2-(9H-carbazol-9-yl)ethyl carbonochloridate (CEOC) as pre-column labeling reagent followed by high performance liquid chromatography (HPLC) with fluorescence detection. Solid phase extraction with Bond Elute Carbon cartridges was applied to sample purification procedure and proved to be simple and effective. The average recoveries of the three target compounds were higher than 80%, with relative standard deviation (RSD) of less than 10%. The sensitivity of the proposed method was about two orders of magnitude higher than traditional HPLC method. When 5.0 g soil sample was used for analysis, the limits of quantification of the analytes were in the range of 0.3–0.6 μg kg−1. Investigation of the concentrations in sediment samples indicated that all three analytes were found at levels ranging from 1.1 to 6.1 μg kg−1.
