Butyl‐, cyclohexyl‐ and phenyltin compounds were extracted from enzymically‐hydrolysed wine and beer samples with 0.05% tropolone in pentane. Methyl derivatives were made by Grignard reaction for determination by gas chromatography‐atomic absorption spectrometry. Wine and beer samples contained <0.1 to 160 nl/ml of butyltins from an undetermined source of contamination. GC‐MS confirmation of butyltins also detected phenyltin, and di‐ and tricyclohexyltin compounds at levels less than the GC‐AAS based method detection limits of 0.05–0.13 ng Sn/mL.