Abstract:A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was established for the simultaneous determination of 3-chloropropanol ester (3-MCPDE), 2-chloropropanol ester (2-MCPDE) and gycidyl ester (GE) in various fatty foods in this study. The 3-MCPDE, 2-MCPDE and GE in vegetable oils, bakery foods, fried- puffed foods and milk powder were determined by GC-MS/MS after the optimization of extraction, transesterification and derivatization of samples and conditions of GC-MS/MS. The limits of quantitation (LOQs) of the four types of food products were 10, 20, 50 and 100 μg/kg, respectively, and the total mean recoveries were in the range of 68.9% ~116.5% with the relative standard deviation (RSD n=6) of 2.11%~13.90%. The results showed that the samples had good linear correlation within a wide linear range, and the correlation coefficients (R) were higher than 0.99. The proposed method had the advantages of high extraction efficiency, good purification effect, high detection sensitivity and accuracy, which could be used for qualitative and quantitative determination of 3-MCPDE, 2-MCPDE and GE in vegetable oils, milk powder, fried- puffed foods and bakery foods.