Abstract: The sample of bitter almond (0.1 g) was hydrolyzed with 4 mol·L-1 H2SO4 in a 25 mL head-space bottle heated in a boiling-water bath for 15 min, and then extracted by SPME with the PDMS/DVB extractor for 20 min. The extractor was desorbed for 1 min at the inlet of the gas chromatograph, and separation of amygdalin was carried out on the HP-5MS chromatographic column with programmed temperature elevation. Helium with flow-rate of 1.0 mL·min-1 was used as carrier gas. Electron bombardment ionization (230 ℃, 70 eV) and whole scanning in the mass range of 40-600 amu were adopted in MS analysis. Linearity was obtained in the range within 100 μg·g-1. A sample of bitter almond was analyzed by this method, value of amygdalin content of 60.43 μg·g-1 was found, which is in consistency with the value determined by spectrophotometry. Value of RSD (n=5) found by analyzing the same sample was 1.8%. Values of recovery over 90% were obtained in the recovery tests at 2 concentration levels of 60 μg·g-1 and 20 μg·g-1.