Records of the environmental occurrence of organothiophosphate esters (OTPEs), which are used as flame retardants and food and industrial additives, are unavailable. In this study, we discovered three OTPEs, namely ,,-tris(2,4-di--butylphenyl) phosphorothioate (AO168═S), -butyl -(butyl-methylphenyl) -(di-butylphenyl) phosphorothioate (BBMDBPt)/,-bis(dibutylphenyl) -methyl phosphorothioate (BDBPMPt), and -butyl -ethyl -hydrogen phosphorothioate (BEHPt), in the surface water of the Yangtze River Basin by applying a characteristic phosphorothioate fragment-directed high-resolution mass spectrometry method. Among the 17 water samples tested, the detection frequencies of AO168═S and BEHPt were 100% and that of BBMDBPt/BDBPMPt was 29%. The mean concentration of AO168═S was 56.9 ng/L (30.5-148 ng/L), and semi-quantitative analysis revealed that the mean concentrations of BEHPt and BBMDBPt/BDBPMPt were 17.2 ng/L (5.5-65.4 ng/L) and 0.8 ng/L (
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