Through the optimization and improvement of GB/T5009.17-2003,a method of hydride generation-atomic fluorescence spectrometry(HG-AFS)coupled with acidic sulfhydryl cotton extraction was developed for the determination of methyl-mercury in seafood.Hydrochloric acid containing Cu2+ was added to the sample and grounded evenly to extract methyl-mercury.After centrifugation,filtration,adsorption,the sample was eluted with the sulfhydryl cotton and detected by AFS and quantified by external standard.Under the optimized conditions,there was a good linear relationship between the fluorescence intensity and the concentration of methyl-mercury quality when the methyl-mercury was in the concentration ranged of 0 ~ 8.0μg/L.The average recoveries were between 97.0%~116.5%,the RSD were between 1.5%~3.0% and the detection limit of method was 0.1mg/kg.The method was quick,easy,less interference,low detection limit and suitable for the determination of methyl-mercury in seafood.