水产品中甲基汞测定方法的优化  

Method optimization for methylmercury determination in aquatic products

作　　者：刘奇[1] 柯常亮[1] 陈洁文[1] 林颂雄[1] 蔡楠[1] 黄珂[1] 纪晓敏 李刘冬[1] 

机构地区：[1]中国水产科学研究院南海水产研究所农业部水产品加工重点实验室农业部水产品贮藏保鲜质量安全风险评估实验室(广州),广东广州510300 [2]汕尾市海洋与渔业环境监测站,广东汕尾516611

出　　处：《食品工业科技》2016年第3期299-302,共4页Science and Technology of Food Industry

基　　金：国家农产品质量安全风险评估重大专项(GJFP2014009);中央级公益性科研院所基本科研业务费专项(中国水产科学研究院南海水产研究所;2014TS10);农业部水产品加工重点实验室开放基金项目(NYJG201306)

摘　　要：本研究对标准方法进行了优化,建立了水产品中甲基汞残留的快速测定方法。本方法采用硫酸和溴化钾超声辅助提取样品中甲基汞,经甲苯反萃,气相色谱测定。结果显示,在25.0～1000μg/L浓度范围内,甲基汞标准曲线方程为y=21.49x-660.9,线性良好（r=0.9995）;方法检测限和定量限分别为7.58、25.0μg/kg;加标量为50.0、100、500、1000μg/kg时,回收率范围为80.8%～108%,相对标准偏差范围为1.56%～8.10%,表明该方法满足水产品中甲基汞残留测定的要求。方法优化后步骤减半,耗时缩短三分之二,样品分析效率大幅提高,适合批量测定水产品中甲基汞残留。A method was developed for methylmercury（ MMC） fast determination in aquatic products through standard method optimizing.Samples were extracted by sulfuric acid and potassium bromide in assist of ultrasound,back-extracted by toluene,detected by gas chromatography（ GC）.As shown,calibration curve（ y = 21.49x-660.9）was in good linearity with a correlation coefficient of 0.9995 in the range of 25.0 ～ 1000 μg / L. The limit of detection（ LOD） and the limit of quantitation（ LOQ） were 7.58 and 25.0 μg /kg,respectively.While spiked at 50.0,100,500 and1000 μg / kg,the recoveries of MMC ranged from 80.8% to 108% with relative standard deviation（ RSD） of 1.56% ～8.10%. It indicated that the method was qualified to detect MMC residue in aquatic products. After optimization,efficiency of sample analysis was greatly improved because of the reduction of half procedures and two thirds time saving,which made the method suitable for quantitation of MMC in batch samples.

关 键 词：甲基汞 水产品 气相色谱法 快速测定 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]