This chapter gives a survey of recent literature on the analysis of organophosphorus flame retardants (OPs) and plasticizers in water. The main literature sources are reviewed from the last eight years, taking into account research articles reporting new analytical developments. Only few new techniques, such as solid-phase microextraction, solid-phase extraction or microporous membrane liquid liquid extraction, have been investigated for their ability of combining the extraction and clean-up steps. Commonest analytical procedures used for the identification of OPs are based on gas chromatography coupled with nitrogen-phosphorus detector or mass spectrometry; as an alternative, liquid chromatography followed by (tandem) mass spectrometry detection is employed.