The methods for the determination of dioxin (PCDD/Fs), polychlorinated biphenyls(PCBs, both indicator and coplanar) and chloropropanols in food with stable isotope dilution technique and gas chromatography- mass spectrometry were established based on the method EPA1613A and 1668A of US EPA, EPS1/RM/31 of Enviroment Canada and AOAC 2000.01 respectively. The international intercalibration collaborative study and Food Analysis Performance Accreditation System (FAPAS) were participated by China CDC, and get satisfactory result with z score. The method were used for determination of dioxin and PCBs in fish collected from different area of China and dioxin-like compounds in the samples of major animal origin food from Chinese total diet study in 2000, which indicate is wide appilction.