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Perfluorinated compounds (PFCs) have been determined in various matrices within China including water bodies, precipitations, biota and non-occupationally PFCs-exposed populations in recent years, yet little attention has been focused on the distributions of PFCs in urban river sediments from Chinese major metropolises such as Guangzhou and Shanghai so far. In this study, sediment samples of 0–2cm were collected from 13 sites in the Zhujiang River across Guangzhou and nine sites in the Huangpu River across Shanghai. PFCs analysis on these sediments via high performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) system was implemented targeting eight analytes involving perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHxS), perfluorooctane sulfonate (PFOS), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA …