Abstract: The sample (0.100 0 g) was placed into the microwave extraction tube, and 15 mL of acetonitrile was added. The mixture was oscillated whirling for 2 min and extracted by microwave for 20 min. Cooling to room temperature, the supernatant was collected. 10 mL of acetonitrile was added and the mixture was oscillated whirling for 2 min. The above supernatants were combined and concentrated to dryness nearby, and then dried by N₂-blowing. The residue was diluted with 10 mL of acetone. Tris(2-chloroethyl) phosphate, tris(1,3-dicloropropyl) phosphate, tris(2-chloroisopropyl) phosphate, triphenyl phosphate, tri-p-cresyl phosphate, tri-m-cresyl phosphate and tri-o-cresyl phcsphate in the above solution were determined by gas chromatography mass spectrometry (GC-MS) using DB-5MS column as the stationary phase.SIM mode was adopted in MS analysis. Linearity ranges of the 7 organophosphate ester flame retardants were all 1.00-100 mg·L^-1, with lower limits of determination (10S/N) of 0.28-1.00 mg·L^-1.Test for recovery was made by standard addition method, giving results in the range of 85.9%-95.2%, with RSDs (n=9) all less than 8.0%.