The determination of organotin compounds (OTCs) in environmental matrices has been subject to great scientific attention during last years, as the accuracy and sensitivity of analytical methods need to be improved in order to be able to detect the compounds of interest in a complex matrix such as sediment. The European Union Water Framework Directive (2013/39/EU) sets very restrictive environmental quality standards for 45 priority substances and other pollutants, including OTCs. Therefore, it is necessary to develop analytical methods in compliance with the environmental quality standard (EQSs) proposed to protect the aquatic environment and human beings. So far various analytical procedures have been used, including gas chromatographic analyses. Most of these methods comprise different steps such as extraction, derivatisation, clean up and the use of several sophisticated instrumentations, as well. Among them the conversion of tributyltin into Sn to allow its determination by Atomic Absorption Spectrometry or Anodic Stripping Voltammetry (AVS) has also been attempted. A great number of studies have been performed on OTCs analysis in marine sediment. However, the only review available in literature discussing the upgrades of analytical methods is dated back to 1997. We reviewed the analytical procedures and discussed them comparatively in order to identify the current state-of-the-art in OTCs detection. Finally, environmental concerns about OTCs were discussed.