Abstract: A suitable GC-MS/MS method was established for the determination of 22 phthalate esters (PAEs) in milk powder. The milk powder samples were dissolved in water, extracted by acetonitrile, salted out by NaCl, then quantitated by GC-MS/MS in multiple reaction monitoring mode (MRM). As a result, 22 PAEs possessed an excellent linear relation by using matrix-matched standard curve under 5~500 ng/mL, the correlation coefficients were all greater than 0.99, LODwas 1.0~5.0 μg/kg, LOQ was 3.0~15.0 μg/kg. The recoveries were 82.4%~111.4% at three spiked level with relative standard deviation (n=6) of 2.4%~9.5%. This analytical method is simple, quick, sensitive and stable, which can be used for a monitoring and screening analysis of 22 PAEs in milk powder.