Abstract: GC-MS was applied to the determination of 16 phthalates in liquor. The sample was extracted with ethyl acetate. The extracts were separated on DB-5MS UI column, and determined under full scan and selected ion monitoring shared mode in MS. Linear relationships between values of peak area and mass concentration of 16 phthalates were kept in the same range of 0.5-10.0 mg·L-1, with detection limits (3S/N) in the range of 0.01-0.10 mg·L-1. Values of inter-day recovery found by standard addition method were in the range of 83.7%-114%, with inter-day RSD′s (n=6) in the range of 3.4%-9.8%;values of within-day recovery found by standard addition method were in the range of 81.9%-113%, with within-day RSD′s (n=6) in the range of 1.5%-6.7%.