In this study a number of analytical procedures are described to determine pharmaceuticals and personal care products (PPCPs) and their metabolites during sewage treatment. The work shows that PPCPs occur in sewage influent and are removed by various wastewater treatment processes. PPCPs include a wide range of chemicals such as prescription drugs as well as diagnostic agents, fragrances, sun-screen agents, and various other compounds commonly present in household items (e.g. detergents, cleaners, toothpastes etc.). During this study a number of PPCPs including painkillers (aspirin, ibuprofen), cholesterol control medication (clofibric acid), antibacterial agents (triclosan), musks (including galaxolide and tonalide), X-ray contrast media (diatrizoate), cancer treatment drugs (cyclophosphamide) and anti-depressant drugs (fluvoxamine) were investigated. Analysis was carried out using a number of techniques. Samples were extracted using solid phase extraction or liquid-liquid extraction and the extracts analysed using capillary gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring or liquid chromatography mass spectrometry (LC-MS) or LC-MS-MS. The results obtained show that aspirin, clofibric acid, diatrozate, fluvoxamine and cyclophosphamide were not detected in any of the crude sewage or sewage effluent samples above the limit of detection of the applied methods. Ibuprofen was detected in all crude sewage samples as well as in all effluent samples with one exception. Removal of ibuprofen by the different STWs was generally between 80–100%, with the exception of one STW where removal was poor (14.4 to 44%). Triclosan was also detected in all crude sewage samples and in all sewage effluent samples. The highest concentration of triclosan detected was 3100 ng l⁻¹. A high removal efficiency was observed in effluent samples taken on two occasions (average removal 95.6%). The concentrations of musks detected in the crude sewage were generally low except for galaxolide and tonalide. The results from STW effluent samples showed significant removal of galaxolide (70–83% removal) except at one STW (STW 1) where removal was low (57% and 39%). Similar removal efficiencies for tonalide were achieved at these STWs (73–96%) except at STW 1 where removal was poor (53%).