The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was applied to the simultaneous determination of five organotin compounds in the shellfish samples. The Agilent TC-C 18 column was used for the separation, the mobile phase of the HPLC was CH 3 CN:H 2 O:CH 3 COOH = 65:23:12 (v/v/v), 0.05% TEA, pH 3.0, at a flow rate of 0.4 ml min −1 . A mix standard solution of five mixed organotin compounds from 100 µg l −1 to 0.5 µg l −1 was used for the method assessment. The experimental results indicate that the correlation coefficient of calibration curves (R 2 ) for each organotin compound was over 0.998. The shellfish samples were treated by supersonic extraction with the same mobile phase for 30 min. The four organotin compounds including dibutyltin (DBT), tributyltin (TBT), diphenyltin (DPHT), and triphenyltin (TPHT) in the shellfish samples were detected by this method. It was found that the domain compounds in the samples were TBT and TPHT. The recovery tests from the standard addition for TMT, TBT, and TPHT were over 80%. However, the recoveries of DPHT and DBT were relatively low, 37.3% and 75.2%, respectively. The reason might be attributed to the decomposition of those compounds during the extraction procedure.