Abstract: Gas chromatography-mass spectrometry (GC-MS) coupled with solid-phase extraction was developed for determination of 4-hexylresorcinol residue in crustacean. The 4-HR was extracted with ethyl acetate, purified by silicagel column and eluted with ethyl acetate, the eluent was concentrated and dissolved in ethyl acetate-n-hexane(1:1，v/v), then analyzed by gas chromatography-mass spectrometry. The results showed that the linear range was 0.05 ~10 μg/mL and its correlation coefficient was 0.9 997.When spiked within 0.05~1 mg/kg, the average recoveries of intraday and intraday were 76.8%~102%, and their relative standard deviations were 2.43%~7.65%.The limits of detection and limits of quantitation were 0.01 mg/kg and 0.05 mg/kg, respectively. This method can be applied to determine the 4-HR residues in crustacea with the advantages of high extraction efficiency, high purification effect and less solvent consumption.