Abstract: The matrix solid phase dispersion（MSPD）and solid phase extraction（SPE）coupled with gas chromatography-mass spectrometry（GC-MS） methods have been established for the determination of diethylstilbestrol（DES）in aquatic products. DES was extracted with ethyl acetate and cleaned up by the dispersive method with Florisil, whereas, ultrasonic extraction with ethyl acetate and Florisil SPE column purification were employed in the SPE analytical procedure. DES in the extracts were then quantified by GC-MS. Good linear range (r2=0.9985) between 1~300μg/L was obtained under the optimized chromatographic conditions. Comparing the recovery(>80%) and LOD(0.5 μg /kg) with SPE method, MSPD has a higher recovery(>90%) and a lower LOD(0.3 μg /kg). Both these methods fulfill the requirements of the analysis of residues. Through the comparison of analytical procedure and results, it is confirmed that the MSPD method is quicker and simpler than the SPE method.