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Analysis of persistent organic pollutants(POPs),especially the emerging POPs,remains challenge.Direct detection of perfluorooctane sulfonyl fluoride(PFOSF)by chromatography and mass spectrometry,for example,has not yet reported due to its special chemical and physical properties(2).PFOSF)is a main precursor of environmentally ubiquitous perfluorooctanesulfonate(PFOS)and the quantity released to the environment is substantial.While GC or GC-MS is no amendable for the direct analysis of highly polar PFOSF and PFOS,indirect analysis with various derivatization procedures was not successful.Furthermore,determination of PFOSF presents significant challenges for HPLC and LC/MS analysis due to the lack of chromophore and ionizable functional group,respectively.In this study,a new method was developed by reacting PFOSF with benzylamine to allow rapid quantitative analysis by using LC/MS(3).The developed method demonstrated good linearity in the range from 2 to 80 ng mL-1 for the reaction product in organic solvent,while the absolute instrument detection limit was 2.5 pg.Liquid-liquid and liquid-solid extraction procedures were established for analysis of water and soil samples,and recoveries were in the range of 51-128%.In addition,the reaction was selective for PFOSF,whereas PFOS did not nearly react.The developed simple analytical method with good reproducibility might not only be applied for analysis of PFOSF in the environment but also be applicable for supporting investigations on environmental fate of PFOSF,particularly its environmental and bio-transformation to PFOS.