Abstract: Organotins in oyster samples were determined by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) after microwave-assisted extraction. Oyster samples were extracted under the conditions of microwave power 60 W for 20 min， while 1.0 mol/L acetic acid and 0.5 mol/L sodium acetate in methanol severed as extraction solvent. After filtration, samples were determined by HPLC-ICP-MS. Under the optimized conditions, the recoveries of dibutyltin, tributyltin and triphenyltin are 104%, 99.3% and 113%, and the detection limits are 0.33, 0.22 and 0.48 ng/g, respectively. The results are consistent with the certified value of CE 477 mussel tissue reference material.