Marine animals sample was extracted with 30%nitric acid solution , and then adjusted the pH with 2 mol/L sodium acetate-acetic acid buffer solution. The eluate obtained was determined and identified by purge and trap gas chromatography-cold vapor atomic fluorescence spectrometry (P&T-GC-CVAFS). The propylation derivatization converted Methyl mercury (MeHg) to the more volatile methyl propyl mercury (MeHgPr), Ethyl mercury(EtHg) to the more volatile ethyl propyl mercury(EtHgPr), which could be concentrated through purge and trap system with a further clean-up of matrix. Tests for recovery were made by addition of standard MeHg and EtHg solutions at 3 different concentration levels to blank marine animals sample matrixes, values of MeHg recovery found were in the range from 80.5%to 103.2%, with RSDs (n=6) in the range from 1.7%to 6.9%;values of EtHg recovery found were in the range from 84.2%to 103.7%, with RSDs(n=6) in the range from 2.3%to 7.0%.%海产动物样品经过30%硝酸溶液提取，用2 mol/L醋酸钠-醋酸缓冲溶液调节pH后，用吹扫捕集-气相色谱-冷原子荧光光谱仪联用系统测定其中的甲基汞和乙基汞的含量。使用衍生试剂，将甲基汞转化为甲基丙基汞，乙基汞转化为乙基丙基汞，吹扫捕集进行富集并进一步消除基体干扰。以空白样品为基体，添加3种浓度水平的甲基汞和乙基汞标准溶液，测得甲基汞的回收率为80.5%~103.2%，相对标准偏差（n=6）为1.7%~6.9%；乙基汞的回收率在84.2%~103.7%，相对标准偏差（n=6）为2.3%~7.0%。
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