An ultra-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the analysis of three triphenylmethane bactericides in sediment by accelerated solvent extraction(ASE).The analytes were extracted from the dispersed samples with neutral alumina by ASE using acetonitrile-McIlvaine buffer(10∶2，by volume) as solution.The extract were analyzed by UPLC-MS/MS in multiple-reaction monitoring(MRM) mode,quantified by the internal standardization.The calibration curves of three triphenylmethane dyes were linear in the range of 0.5-50.0 μg/L with correlation coefficients more than 0998.Under the optimal extraction conditions of 60 ℃ temperature and 1 500 psi pressure,the recoveries of three compounds ranged from 65.8% to 112%,with RSDs(n=6) of 5.1%-14.4%.The limits of detection and quantitation were in the range of 0.006-0.007 μg/kg and 0.024-0.028 μg/kg,respectively.The method was successfully used to detect the sediment samples from Gehu Lake.