Abstract: GC-MS/MS was applied to the determination of melamine in poultry eggs with dispersive solid phase extraction with syringe. The poultry egg sample was extracted with acetonitrile, and then anhydrous magnesium sulfate and sodium chloride were added. After centrifugation, fat in the supernatant was removed with n-hexane. Dispersive solid phase extraction with syringe was adopted with PSA and GCB as dispersive solid phase adsorbent. After filtration, the filtrate was dried by nitrogen blowing and then derivatized. The DB-5MS quartz capillary chromatographic column was used for GC separation and the timed-selected reaction monitoring mode was adopted in MS determination. Linear relationship between values of peak area and mass concentration of melamine was kept in the range of 5.0-200.0 μg·L^-1, with lower limits of determination (10S/N) in the range of 2.4-3.5 μg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 80.3%-103%, with RSDs (n=6) in the range of 0.60%-8.9%.