The extraction of organic contaminants from water and sediment samples is the critical and time consuming step in the analysis as they are present in trace amounts. In this study, efficient, selective, and rapid analytical methods in determining organic contaminants in water and sediment samples were developed. Since these compounds are of wide range polarity, a tandem-cartridges solid phase extraction (SPE) using C18 and LiChrolut EN was found to be efficient with the advantage of minimising sample volume and reducing analysis time. Sediment samples were extracted using pressurized liquid extraction (PLE) with simultaneous clean-up by incorporating silica in the extraction cell. The developed methods were applied to water and sediment samples from point and non-point pollution sources. The data sets obtained were subjected to chemometric analysis (CA, DA and PCA). Sterols was found to be strongly correlated to sewage and chicken farm samples while PAHs and pesticides were correlated to samples from agricultural activities.