Abstract: The stir bar was placed in 20 mL of a headspace bottle, and 18 mL of water sample and 2 mL of methanol were added into the headspace bottle. After closed the lip, the solution was stirred for 20 min at 20℃ with the speed of 800 r·min^-1. The stir bar was taken out and placed into the thermal desorption glass tube. Desorption solution was separated by GC using DB-5MS chromatographic column as stationary phase. SIM was adopted in MS analysis. Linear relationships between values of peak area and mass concentration of 23 OPPs were found in the range of 0.05-5.00 mg·L^-1, with detection limits (3S/N) in the range of 0.3-25 μg·L^-1. Test for recovery was made by standard addition at 3 concentration levels, giving results in the range of 70.9%-97.1%, with RSDs (n=6) all less than 5.5%.