对国标方法 GB/T 5009.17-2003进行优化和改进,建立酸提取巯基棉-氢化物发生原子荧光法(hy-dride generation-atomic fluorescence spectrometry,HG-AFS)测定海产品中甲基汞的方法。样品研磨均匀后,加入含有Cu2+的盐酸萃取样品中的甲基汞,经离心、过滤后用巯基棉吸附,洗脱后用原子荧光仪检测,外标法定量。结果表明:甲基汞在0～8.0μg/L内,荧光强度与甲基汞质量浓度之间线性关系良好(相关系数为1),以2.0、5.0μg/L 2个添加量在样品中添加甲基汞,平均回收率在97.0%～116.5%,相对标准偏差为1.5%～3.0%,方法的检出限为0.1 mg/kg。该方法简便快速,机体干扰小,检出限低,精密度、准确性均能满足海产品中甲基汞的测定要求。

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.