A rapid and reliable analytical method,based on large-volume injection and gas chromatography-mass spectrometry(PTV/GC-MS) was developed for the determination of 12 benzotriazoles and benzothiazoles in aquatic matrixes.1.0 L water samples were acidified to pH 3.0 using 3 mol/L HCl.The samples were then passed through an Oasis HLB cartridge.The analytes were eluted with 6 mL methanol-acetonitrile(1∶1).The solution was evaporated to dryness under a gentle stream of nitrogen,and redissolved in acetone,internal standard and silylation reagent.The sealed vials were incubated at 38 ℃ for 1 h before instrument analysis.The separation of target compounds was achieved in a DB-5MS fused-silica capillary column.The analytes were detected in selected ion monitoring(SIM) that operated in electron impact(EI) mode.The calibration curves of 12 target compounds were linear in the range of 0.1-100 ng/L with correlation coefficients not less than 0.992.Spiked recoveries of the target analytes were in the ranges of 46%-116% for tap water,and 43%-117% for river water,with RSDs of 1.0%-16% and 1.0%-15%,respectively.The method detection limits for tap water and river water were in the ranges of 0.050-1.3 ng/L and 0.057-1.8 ng/L,respectively.The method was simple and sensitive,and was successfully employed in the detection of corrosion inhibitors in river water collected from the city section of the Pearl River.