| Perfluorinated organic acids (PFCAs) are an emerging environmental pollutants, they are resistant to hydrolysis, photolysis, biodegradation and to metabolic processes in living organisms. These properties make them both water-and fat-repellent ("supersurfactants") and thus they have been used for treatment of textiles and paper, in paints, lubricants, polishes, PTFE precursors, food packages, insecticide formulations, fire-fighting foams, and in the photographic and the semi-conductor industries. As results, the pollutants were ubiquitous in many kinds of environmental media. The HPLC/MS is a major analytical technique in the study of their environmental fate. Unfortunately, high background signal of the PFCAs is commonly found in the HPLC/MS analysis due to containing of them in the HPLC system. It is decreasing accuracy of the analytical results.In order to overcome this problem, the derivatization/HPLC/UV/MS analytical method was proposed in this study. The p-bromo-benzoyl bromide (BPBr),18-crown-6 and PFOA was used as derivatization reagent, catalyst and target analyte, respectively. The reaction was carried out in the alkaline solution and corresponding ester derivative products was easily obtained. The product has a strong UV absorption, and it is possible simultaneous determination of HPLC-UV/MS. Comparison to common HPLC/MS, the derivatization/HPLC/UV/MS technique demonstrates wide detection range (5～1000 ng mL-1), high accuracy (recovery 85%～95%) and low detection limit (5 ng mL-1) due to elimination of the noise background produced in the HPLC system. In addition, the conditions of derivatization and clean up were optimized. The method was applied and evaluated in the determination of PFCAs from the real environmental samples.
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