There have been many methods available for the determination of butyltin compounds in sediment. The variations of these methods are not in the methods of determination but rather in the extraction of these compounds from the complex matrices. All of these methods have not been critically compared or evaluated, mainly because of the lack of a suitable reference sediment for butyltin compounds. Recently, the National Research Council of Canada has introduced a reference sediment (PACS‐1) which contains certified values of butyltin compounds. The present study compares the recoveries of ten extraction techniques for butyltin species using ethylation derivatization and GC AA as the method of determination. Of these ten methods, only four were found satisfactory for extraction of the dibutyltin and tributyltin species. None of the methods evaluated, however, could quantitatively extract monobutyltin from sediment.