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作 者:易华娟 苏雍伦 何洁玲 张树权 陈锦杭 YI Huajuan;SU Yonglun;HE Jieling;ZHANG Shuquan;CHEN Jinhang(Dongguan Institutes for Food And Drug Control,Dongguan,Guangdong 523808,China;Guangdong Medical University,Dongguan,Guangdong 523808,China;Zhongshan Customs Technology Center,Zhongshan,Guangdong 528403,China)
机构地区:[1]东莞市食品药品检验所,广东东莞523808 [2]广东医科大学,广东东莞523808 [3]中山海关技术中心,广东中山528403
出 处:《农产品加工》2022年第23期49-53,58,共6页Farm Products Processing
基 金:东莞市社会发展科技项目(20221800902042)。
摘 要:建立气相色谱-冷蒸气原子荧光光谱法(Gas chromatography-cold vapour atomic fluorescence,GC-CVAFS)检测鱼及鱼饲料中甲基汞(MeHg)的方法。对仪器的参数和前处理条件进行优化,在此基础上采用碱法消解鱼样和酸法消解鱼饲料以提取甲基汞,而后进行乙基化反应,最后通过全自动烷基汞测定仪分析测定MeHg含量。在10~1000 pg内,MeHg的标准曲线方程为Y=365.68X-1900.2,线性关系强(R^(2)=0.9998);加质量浓度为10,20,100μg/kg时,碱法消解鱼样的加标回收率为95.7%~102.8%,相对平均偏差(Relative standard deviation,RSD)为1.21%~3.62%;酸法消解鱼饲料的加标回收率为102.9%~109.8%,RSD为2.16%~3.90%;碱法和酸法消解的检出限分别为3.1μg/kg和2.9μg/kg,定量限均为10μg/kg。该方法精密度良好、灵敏度高,能够快速、准确、高效地检测鱼及鱼饲料中的MeHg含量。This study established a determination method of methlymercury(MeHg)in fish and fish feedstuffs by gas chromatography-cold vapour atomic fluorescence(GC-CVAFS).On the basis of optimizing Instrument parameter and pretreatment condition,alkaline digestion was developed to extract the MeHg in fish while fish feedstuffs were digested by acid.The extracted MeHg samples were then determined by the automated alkylmercury analytical system after ethylation reation.The results showed that the calibration curva of MeHg(Y=365.68X-1900.2)was in good linearity with a correlation of 0.9998 in the rage of 10~1000 pg.When the concentration of standard addition were 10,20,100μg/kg,the recovery of adding methylmercury and relative standard deviation(RSD)of alkaline digestion in fish were 95.7%~102.8%and 1.21%~3.62%,and of acid digestion in fish feedstuffs were 102.9%~109.8%and 2.16%~3.90%.The detection limit,quantification limit of alkaline digestion and acid digestion were 3.1μg/kg and 2.9μg/kg,both 10μg/kg.The method was high precision and sensitivity,which was suitable for the determination of MeHg in fish and fishe feedstuffs with speed,accuracy and efficiency.
关 键 词:鱼及鱼饲料 酸法消解 碱法消解 甲基汞 气相色谱-冷蒸气原子荧光光谱法
分 类 号:TS254.7[轻工技术与工程—水产品加工及贮藏工程]
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