液相色谱-原子荧光光谱法测定海产动物干制品中三种形态汞含量的方法研究

Determination of Three Forms of Mercury in Marine Dry Products by Liquid Chromatography-Atomic Fluorescence Spectrometry

目的:建立液相色谱-原子荧光光谱法测定海产动物干制品中三种形态汞含量的方法。方法:样品通过水浴超声振荡提取,冷冻离心机离心分离样液,取上清液用氢氧化钠溶液调节pH值,过膜后经过形态分析仪预处理,由高效液相色谱分离,最后用原子荧光光度计检测。结果:三种形态汞的线性范围0～10μg/L,二价汞的线性方程S=3753.6C-6783.7,相关系数0.9984,检出限0.50μg/L;甲基汞的线性方程S=4492.8C-5798.7,相关系数0.9995,检出限0.50μg/L;乙基汞的线性方程S=3199.4C-79.6,相关系数0.9989,检出限0.52μg/L。方法的加标回收率:甲基汞100.0%～104.0%;乙基汞98.0%～100.0%;二价汞101.0%～102.0%,方法的精密度:甲基汞2.83%～8.98%,乙基汞3.41%～9.39%,二价汞2.42%～8.21%。结论:采用液相色谱仪和原子荧光光谱仪联合测定海产动物干制品中三种形态汞含量,方法的精密度、准确度及线性关系均比较满意,适合用于海产品中三种形态汞含量的测定。

Objective: To establish a method for the determination of mercury in dried marine animal products by liquid Chromatography-Atomic fluorescence spectrometry. Methods: The sample was extracted by ultrasonic vibration in a water bath, and then the sample liquid was centrifuged and separated by a centrifuge. The supernatant was adjusted by sodium hydroxide solution. After passing through the membrane, it was pretreated by morphological analyzer, separated by high performance liquid chromatography, and finally detected by atomic fluorescence spectrometer. Results: The linear range of three forms of mercury was 0~10μg/L, the linear equation of divalent mercury S=3753.6C-6783.7, the correlation coefficient was 0.9984, the detection limit was 0.50μg/L, the linear equation of methyl mercury S=4492.8C-5798.7, the correlation coefficient 0.9995, the detection limit 0.50μg/L, ethyl mercury linear equation S=3199.4C-79.6, the correlation coefficient 0.9989, the detection limit 0.52μg/L. The method standard addition recovery rate was: A Base mercury 100%~104%;ethyl mercury 98.0%~100%;divalent mercury 101%~102%;the precision of the method was 2.83~8.98% for methyl mercury;3.41~9.39% for ethyl mercury;2.42%~8.21% for divalent mercury. Conclusion: The method was suitable for the determination of three forms of mercury in marine animal dry products. The precision, accuracy and linearity were satisfactory. It was suitable for the determination of three forms of mercury in seafood.