Abstract: GC-MS was applied to the determination of 17 volatile organic solvents in nail polish. The sample was extracted with methanol, and the extract was filtered with organic needle filter of 0.22 μm. DB-624 capillary column was used as the stationary phase in GC separation, and full-scanning mode as well as selected ion monitoring mode were adopted in MS determination. Linear relationship between values of peak area and mass fraction of 17 volatile solvents were obtained in the same range of 3.2-400 g·kg-1, with detection limits (3S/N) in the range of 0.14-1.60 g·kg-1. Tests for recovery was made by standard addition method, and values of recovery found were in the range of 89.7%-106% with RSD′s (n=6) in the range of 0.96%-6.6%.