Abstract: A method of GC-MS for the determination of 16 phthalates (PAE′s) in food was proposed. The pretreatment methods for different matrixes of samples were described in detail, and the high-fatty food was purified by gel permeation chromatography (GPC). HP-5MS quartz capillary column was used for separation, and EI source was used for determination in MS. Linearity ranges of the 16 PAE′s were kept in the same range of 0.50-20.0 mg·L-1, with detection limits (3S/N) ranged from 6.03 to 826 μg·kg-1. Tests for recovery were made at the concentration levels of 1 and 10 mg·kg-1 of the mixed phthalate standards, values of recovery found were in the ranges of 79.2%-101% for pure oil and fat and 77.8%-97.4% for high-fatty food. Values of RSD′s (n=3) found were in the ranges of 3.4%-6.9% and 4.1%-6.0% respectively.