A method for the simultaneous determination of six perfluoroalkyl compounds (perfluorooctanesulfonic acid (PFOS) and five perfluoroalkyl carboxylic acids), five phenolic compounds (nonylphenol (NP), bisphenol A (BPA), and methyl-, ethyl- and propylparabens), and the brominated flame retardant hexabromocyclododecane (HBCDD) in surface water and effluent wastewater has been developed. The selected pollutants include eight of the industrial pollutants (PFOS and derivatives, NP, and HBCDD) that could be regulated in surface water according to an European Union Directive proposal and four compounds of great concern because their estrogenicity (BPA and parabens). The method is based on solid-phase extraction and determination by high-performance liquid chromatography-triple quadrupole mass spectrometry in negative electrospray ionization mode. Method quantitation limits of NP, PFOS and derivatives, and HBCDD allow its application for routinely control of surface water according to the EU proposal of directive.