Two pretreatment methods were used to detect chloramphenicol residues in aquatic products combining the super high performance liquid chromatography tandem mass spectrometry. The samples were extracted by 1% formic acid-acetonitrile solution and purified by PRi ME HLB solid-phase extraction column. The correlation coefficient was greater than 0.99 in the range of 5-100μg/L. Under the 3μg/kg and 5μg/kg two levels of average standard addition recovery were 100.0%-109.3% and 86.0%-102.8%（conventional methods were 83.24%-102.24%and 70.8%-97.2%）, relative standard deviation were 3.9 and 6.8（conventional methods were 9.5 and 12.3）. The new method had higher sensitivity, accuracy, precision, simple and quick operation, suitable for bulk sample testing at the same time compared with the conventional method.