液相色谱-电感耦合等离子体质谱法测定水产品中的4种形态汞

Determination of 4 forms of mercury in aquatic products by liquid chromatography-inductively coupled plasma mass spectrometry

中文关键词:  液相色谱-电感耦合等离子体质谱法  汞  形态分析

英文关键词:liquid chromatography-inductively coupled plasma mass spectrometry  mercury  speciation analysis

中文摘要:

      目的 建立一种微波萃取-高效液相色谱分离-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma mass spectrometry, HPLC-ICP/MS)测定水产品中无机汞(inorganic mercury, IMC)、甲基汞(methyl mercury, MMC)、乙基汞(ethyl mercury, EMC)和苯基汞(phenyl mercury, PMC)的方法。方法 样品经25%四甲基氢氧化胺微波萃取后, 用流动相定容, 0.45 μm微孔滤膜过滤后备用。样品经反相色谱柱分离, ICP/MS检测。结果 4种形态的汞在质量浓度0.5～20 ng/mL的范围内呈线性关系, 虾仁样品在0.01、0.02、0.2 mg/kg添加水平下的回收率为61.3%~113.7%; 鳕鱼在0.01、0.02、0.5 mg/kg添加水平下回收率为60.8%~109.8%; 金枪鱼在0.01、0.02、1.0 mg/kg添加水平下回收率为75.5%~115.9%, 日内相对标准偏差小于8%, 日间相对标准偏差小于10%; 4种形态汞的检出限均为4 μg/kg。结论 该方法快速、准确、灵敏, 适合用于水产品中4种汞形态分析检测。

英文摘要:

      Objective To establish a method for the determination of inorganic mercury (IMC), methyl mercury (MMC), ethyl mercury (EMC), and phenyl mercury (PMC) in aquatic products by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP/MS). Methods After microwave extraction with 25% tetramethyl hydroxide, the samples were filtered by a 0.45 μm microporous membrane using a mobile phase constant volume. The samples were separated by reversed-phase chromatographic column and detected by ICP/MS. Results The 4 forms of mercury showed linear relationships in the mass concentration range of 0.5? 20 ng/mL. The recoveries of shrimp samples at the addition levels of 0.01, 0.02, and 0.2 mg/kg were 61.3%?113.7%, the recoveries of cod at the addition levels of 0.01, 0.02, and 0.5 mg/kg were 60.8%?109.8%; and the recoveries of tuna at the addition level of 0.01, 0.02 and 1.0 mg/kg were 75.5%?115.9%. The intraday relative standard deviations were less than 8%, and the intraday relative standard deviations were less than 10%. The limits of detection of 4 forms of mercury were all 4 μg/kg. Conclusion The method is rapid, accurate and sensitive, which is suitable for the analysis and detection of four kinds of mercury in aquatic products.