Abstract: Headspace-GC-MS/MS was applied to the determination of anisole in water. 3 g of NaCl and 10 mL of water sample were placed into head-space flask, and the mixture was equilibrated at 70 ℃ for 15 min while stirred, at a rate of 95 r·min-1. Rxi-5Sil capillary column was used for separation in GC. EI and MRM were adopted in MS. The linearity range of anisole was between 0.005-0.1 μg·L-1 with detection limit (3S/N) of 0.001 μg·L-1. Values of recovery obtained by standard addition method were in the range of 73.7%-92.2% and RSDs (n=6) were in the range of 3.7%-8.2%.