AbstractThe multi-matrices samples from snow (n = 4), lake water (n = 4), surface runoff water (SRW) (n = 1) and coastal seawater (n = 10) were collected to investigate the spatial distribution and the composition profiles of per- and polyfluoroalkyl substances (PFASs) in Fildes Peninsula, King George Island, Antarctica in 2011. All samples were prepared by solid-phase extraction and analyzed by using high performance liquid chromatography/negative electrospray ionization-tandem mass spectrometry (HPLC/(−)ESI-MS/MS). 14 PFASs in snow, 12 PFASs in lake water, 9 PFASs in SRW and 13 PFASs in coastal seawater were quantified, including C4, C7, C8, C10 PFSAs, C4–C9, C11–C14, C16 PFCAs, and FOSA. PFOA was detected in all samples with the highest concentration (15,096 pg/L) in coastal seawater indicating a possible influence of local sewage effluent. High concentration and mostly frequency of PFBA occurred in snow (up to 1112 pg/L), lake water (up to 2670 pg/L) and SRW (1431 pg/L) while detected in the range of method detection limited (MDL) in the coastal seawaters indicate that PFBA is mainly originated from atmospheric dust contamination and also affected by the degradation of their precursors. No geographical differences in PFOS concentrations (n = 8, 18 ± 3 pg/L) were measured in all snow and lake water samples also suggests that PFOS could be originated from the degradation of their precursors which can transported by long-range atmospheric route, but in a very low level.