摘要
建立稻米中无机汞（Hg（Ⅱ））和甲基汞（MeHg）的液相色谱一电感耦合等离子体质谱检测方法。样品中的Hg（Ⅱ）和MeHg经提取液（0．1％L-半胱氨酸＋5％甲醇）超声提取、0．22μm水系滤膜过滤净化，以0．1％L-半胱氨酸＋0．06mol／乙酸铵＋5％甲醇为流动相，用Venusil@MPC18色谱柱分离，以电感耦合等离子体质谱进行测定。结果显示，Hg（1I）和MeHg能有效分离，且在0．10～5．00μg／L范围内线性关系良好。当称样量为0．5g时，方法的检出限（LOD）为0．001mg／kg，定量限（LOQ）为0．003mg／kg，Hg（11）的加标回收率为94．5％～96．3％，MeHg的加标回收率为99．1％一106．7％。本方法准确、快速、便捷，可应用于稻米中Hg（Ⅱ）、MeHg的同时测定。
To establish a method for the determination of mercury and methylmercury in rice by high performance liquid chroma- tography coupled with inductively coupled plasma mass spectrometry （HPLC-ICP-MS） .Mercury and methylmercury in sample were ultrasonic extracted by 0. 1% L-eysteine ＋5% methanol, purified by 0. 22 μm water filtration, separated by Venusil, MP C 18 column, with 0. 1% L-eysteine ＋5% methanol ＋0.06 mol/L ammonium acetate as the mobile phase, and determinated by in- ductively coupled plasma mass spectrometry.Hg（ I1 ） and MeHg could be well separated, and it showed good linearity in the range of 0. 10-5.00 μg/L.When the sample weight is 0. 5 g,the limit of detection was 0. 001 mg/kg,the limit of quantification was 0. 003 mg/kg,and the average recoveries of Hg（ II ） and MeHg were 94.5% -96.3% and 99.1% - 106.7%.The method was ac- curate,rapid,simple,and can be used for simultaneous determination of mercury（ I1 ） and methylmercury in rice.
出处
《化学试剂》
CAS
北大核心
2018年第3期257-260,共4页
Chemical Reagents
基金
粮食公益性行业科研专项资助项目(201513006-03)
