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A fast and accurate derivatization method was developed for simultaneous HPLC-UV/MS determination of perfluorocarboxylic acids (PFCAs).The PFCAs were simply conversed to corresponding esters in alkaline solutions, in which p-bromophenacyl bromide (BPBr) and 18-crown-6 are respectively used as derivatization reagent and catalyst.The derivatives had high ultraviolet molar absorption and ionization ability, which allowed subsequent chromatography analysis of trace levels targets.Compared with other commonly used methods, the method could simultaneously HPLC-UV/MS determine the PFCAs, and it was greatly favored on qualitative and quantitative analysis of PFCAs.First, the method could effectively eliminate the background noise generated from components comprised by fluorated substance of HPLC.And then the characteristic isotope ratio of bromine contained in the derivatives could assure accurate qualitative analysis.Several parameters that influenced the derivatization yield were optimized, and the best derivatization yield was obtained when the reaction was carried out under no-moisture condition at 80℃ for 30 min.The LODs of the optimized method reached 5 ng mL-1.We also applied the optimized method to real water samples to evaluate the applicability and reliability.