In this work, a method was developed and optimized for the analysis of polyfluoroalkyl and/or perfluoroalkyl substances(PFASs) content in surface water and sediment samples with high instrumental response and good separation. Surface water and sediment samples were collected from the Yangtze River Delta(YRD) to analyze the distribution characteristics of perfluoroalkyl carboxylic acids(PFCAs), perfluoroalkane sulfonic acids(PFSAs), perfluoroalkyl phosphonic acids(PFPAs), perfluoroalkyl phosphinic acids(PFPiAs), and polyfluoroalkyl phosphoric acid diesters(di PAPs). The results showed that the total concentrations of PFCAs and PFSAs in YRD varied from 31 to 902 ng/L. PFCAs(≥ 11 carbons) and PFSAs(≥ 10 carbons atoms) were not detected in any surface water samples. The mean concentrations of all PFCAs and PFSAs in surface water from the sampling areas decreased in the following order:Yangtze river(191 ng/L) ≈ Taihu lake(189 ng/L) > Huangpu river(122 ng/L) ≈ Qiantang river(120 ng/L) > Jiaxing urban river(100 ng/L). Strong significant(p < 0.05) correlations between the concentrations of many of the compounds were found in the sampling areas, suggesting a common source for these compounds. Only perfluorooctanoic acid(PFOA) was observed in all sediment samples, at concentrations varying from 0.02 to 1.35 ng/g. Finally, detection rates of two di PAPs were only 8% and 10%, respectively and the concentration of di PAPs was two to three times lower compared to PFCAs and PFSAs. In this work, a method was developed and optimized for the analysis of polyfluoroalkyl and / or perfluoroalkyl substances (PFASs) content in surface water and sediment samples with high instrumental response and good separation. Surface water and sediment samples were collected from the Yangtze River Delta (YRD) to analyze the distribution characteristics of perfluoroalkyl carboxylic acids (PFCAs), perfluoroalkane sulfonic acids (PFSAs), perfluoroalkyl phosphonic acids (PFPAs), perfluoroalkyl phosphinic acids (PFPiAs), and polyfluoroalkyl phosphoric acid diesters that the total concentrations of PFCAs and PFSAs in YRD varied from 31 to 902 ng / L. PFCAs (≥ 11 carbons) and PFSAs (≥ 10 carbons atoms) were not detected in any surface water samples. The mean concentrations of all PFCAs and PFSAs in surface water from the sampling areas decreased in the following order: Yangtze river (191 ng / L) ≈ Taihu lake (189 ng / L)> Huangpu river (122 ng / L) ≈ Qiantang river )> Jiaxing urban river (100 ng / L). Strong significant (p <0.05) correlations between the concentrations of many of the compounds were found in the sampling areas, suggesting a common source for these compounds. Only perfluorooctanoic acid (PFOA) was Observed in all sediment samples, the concentration changes from 0.02 to 1.35 ng / g. Finally, detection rates of two di PAPs were only 8% and 10%, respectively and the concentration of di PAPs were two to three times lower compared to PFCAs and PFSAs.