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Perfluorooctane sulfonate (PFOS) and other perfluoroalkyl compounds (PFCs) were measured in liver samples from 29 marine tucuxi dolphins from Rio de Janeiro state (RJ), Brazil. PFC measurement combined liquid chromatography and mass spectrometry, using a CapLC system connected to a Quadrupole-LIT mass spectrometer. PFOS was the only PFC detected and it was so in all samples. PFOS concentrations (ng x g(-1) dw) of dolphins (n=23) from the highly contaminated Guanabara Bay (in RJ) varied between 43 and 2431 as well as between 76 and 427 from areas of RJ other than the quoted bay (n=6). Concentrations of three fetuses and one neonate varied between 664 and 1590. Fetus/mother ratios were calculated in two situations (2.75 and 2.62). It seems that mother-to-calf transference plays important role for relationships between PFOS and age. When a one-year-old male calf presenting 2431 ng x g(-1) dw was excluded from the test, significant correlations were observed between PFOS concentrations and both age and total length. Despite the placental transference, PFOS concentrations were not significantly lower in females than in males. PFOS levels in marine tucuxi dolphins from Guanabara Bay are among the highest detected to date in cetaceans, and this may represent a threat to the small population concerned.