In freshwater systems, organic micropollutants are bound to natural organic matter (NOM), which is responsible for a decrease in their recoveries by solid-phase extraction (SPE). This "negative effect" has been investigated for the SPE of polycyclic aromatic hydrocarbons (PAHs), oxygenated PAHs, nitrated PAHs and n-alkanes from salt water using Aldrich humic acid as a model of NOM. The effect has been partially obviated by the addition of isopropanol as a surfactant. The SPE protocol, developed with isopropanol, has been applied to the water-extract of a highly contaminated sediment. The water-extract has been size fractionated by cross-flow ultrafiltration into particulate (PM), colloidal (CM) and truly dissolved matter (tDM). Organic extracts from SPE experiments have been analyzed by gas chromatography-mass spectrometry. The major classes of molecules are heteroaromatic PAHs and PAHs. Those molecules are mainly bound to the tDM, which highlights: (1) the competition between organic micropollutants and natural organic molecules for available sorption sites and (2) the toxicological hazard linked to the mobilization of sediments highly contaminated by both industrial and urban activities.