According to the different samples using different extraction methods, fat-free food samples were extracted by n-hexane, oil samples by ethyl acetate: cyclohexane (V/V=1), fat- containing samples by petroleum ether, ethyl acetate and cyclohexane jointly. Each extract was concentrated to 2mL, determined by gas chromatography-mass spectrometer. The result showed that the recovery rate of rapid determination of phthalates plasticizer was 85.9%~110.2%, RSD was 1.87%~5.89%.