液相色谱-原子荧光光谱法检测水产品中汞形态

摘要

A method of high performance liquid chromatography–atom fluorescence spectrometric (HPLC–AFS) was established for the determination of inorganic mercury [Hg(Ⅱ)] and methyl-mercury (MeHg) in aquatic products. The experimental factors affecting the determination results, such as the composition of mobile phase, carrying current, oxidant agent, reducing agent, carrier gas and auxiliary gas were studied and optimized, and the evaluation of method was researched. Good linear range of Hg(Ⅱ) and MeHg was obtained ranging from 1 ng/mL to 20 ng/mL, and the correlation coefficients were 0.999 4and 0.999 1. The detection limits of Hg(Ⅱ) and MeHg were 0.19 ng/mL and 0.17 ng/mL, respectively; the relative standard deviations of chromatographic peak areas were 3.16% and 2.16% (n=7), respectively; and the spiked recoveries were 74%–100% and 71%–91%, respectively. This method can be used for the determination of different mercury deformations in aquatic products.%建立了液相色谱–原子荧光光谱联用测定水产品中无机汞和甲基汞含量的方法。对影响测定结果的分析条件，如流动相组成、载流、还原剂、氧化剂、载气和屏蔽气进行了研究和优化，同时考察了该方法的有效性。结果表明：无机汞和甲基汞在质量浓度1～20 ng／mL范围内线性关系良好，相关系数分别为0.9994，0.9991；检出限分别为0.19，0.17 ng／mL；色谱峰面积的相对标准偏差分别为3.16%，2.16%（n=7）；加标回收率分别为74%～100%，71%～91%。该方法可用于水产品中汞元素的形态分析。