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建立了超声酸提取-高效液相-原子荧光联用测定温州海产品中无机汞[Hg(Ⅱ)]、甲基汞(MeHg)和乙基汞(EtHg)含量的方法,并优化了实验条件。实验采用5mol/L盐酸溶液,超声3.0h提取汞化合物,硫代硫酸钠络合,最后经C18柱(4.6mm×150mm)分离,流动相为5%乙腈-0.06mol/L乙酸铵-0.12%L-半胱氨酸。在最佳条件下,3种汞化合物在0—20μg/L范围内线性良好,相关系数(r)均优于0.9990,检出限分别为1.04、1.09和1.29μg/L,相对标准偏差(RSDs)均小于5%(n=10),温州海产品的汞加标回收率达到90.1%—107.3%。该方法操作简便,精密度高,干扰少,适用于各地海产品中汞化合物的形态分析测定。
A method for the determination of inorganic mercury [Hg (Ⅱ)], methylmercury (MeHg) and ethylmercury (Hg (Hg)) in Wenzhou seafood was established by using ultrasonic acid extraction-high performance liquid chromatography-atomic fluorescence spectrometry . The experiment used 5mol / L hydrochloric acid solution, 3.0h extraction of mercury compounds, sodium thiosulfate complexation, and finally by C18 column (4.6mm × 150mm) separation, the mobile phase was 5% acetonitrile -0.06mol / L ammonium acetate -0.12% L-cysteine. Under the best conditions, the linearity of the three mercury compounds in the range of 0-20μg / L was good with correlation coefficients (r) better than 0.9990, and the detection limits were 1.04, 1.09 and 1.29μg / L, respectively. The relative standard deviations (RSDs ) Were less than 5% (n = 10). The recovery rate of mercury in Wenzhou seafood reached 90.1% -107.3%. The method is simple and convenient to operate, has high precision and less interference, and is suitable for the determination of the mercury compounds in marine products in various places.