Abstract: The mashed cork sample (0.500 0 g) was extracted ultrasonically with water for 30 min, and 9 mL of the extract was taken and 1.8 g of Na₂SO₄ were added into the extraction bottle. After solid-phase microextraction at 55℃ for 35 min, the solution was desorbted for 7 min at the injection port of the gas chromatography, and guaiacol was determined by GC-MS. As shown by the results, linear relationship between values of peak area and mass concentration of guaiacol was found in the range of 25.00-2 000 μg·L^-1, with detection limit (3S/N) of 0.022 μg·L^-1. Test for recovery was made by standard addition method, giving results in the range of 69.8%-115%, and RSDs (n=6) ranged from 6.3% to 13%.