Enrichment techniques have become an important feature in the trace analysis of oestrogen mimicking chemicals in the environment. Recent developments such as accelerated solvent extraction (ASE) have improved extraction recoveries in a wide variety of solid matrices including sediments, sludges and leachate soils. Such samples taken from the Irish Midlands Shannon Catchment region during the winter of 2004/5 and suspected to contain certain xenooestrogens or hormonally active agents were extracted using this technique, which was then coupled with high performance liquid chromatography (HPLC) for quantification purposes. ASE was thus employed to both isolate and pre-concentrate targeted analytes using the minimum amount of solvent hence making extractions more conservational. Two simple, yet extremely sensitive liquid chromatographic methods were developed based on UV detection; one for phthalates and one for alkylphenols, with recoveries reaching up to 92.0%. Acid digestion was used for the extraction of the tin and organotin compounds with analysis by polarography. In river sediment, levels of up to 24.4 mg kg(-1) phthalate, 1.14 mg kg(-1) 4-nonylphenol and 118 mg kg(-1) tin were found. In leachate sediments, values up to 49.8 mg kg(-1) phthalate, 1.57 mg kg(-1) 4-nonylphenol, and 36.0 mg kg(-1) tin were determined. In sludge, values up to 174 mg kg(-1) phthalate and 22.8 mg kg(-1) 4-nonylphenol were quantified. The highest value of tin (118 mg kg(-1)) was found present in an area of high leisure craft activity. Typical sediment levels of tin at other river locations ranged between 1.20 and 37.5 mg kg(-1).