Abstract: The sample (0.100 0 g) was dissolved ultrasonically with 5.0 mL of water, and the solution was introduced into the headspace sampling apparatus, and equilibrated at 80 ℃ for 30 min. After the headspace extraction gaseous of methanol from the solution, HP-INNOWAX capillary column was used as stationary phase for gas chromatography separation. The mode of SIM was adopted in MS, and external standard method was adopted for quantification. Linear relationship between values of peak area and mass concentration of methanol was found in the range of 0.50-100 mg·L^-1, with detection limits (3S/N) of 0.002 5%. Test for recovery was made by standard addition method, giving results in the range of 90.0%-100%, with RSDs (n=6) less than 2.2%.