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目的建立高效液相色谱与原子荧光光谱联用测定水产品中甲基汞及其他形态汞的检测方法。方法样品经盐酸超声提取后离心过滤,以5%乙腈-4.62 g/L乙酸铵-1.2 g/L半胱氨酸溶液作流动相,经反相C18色谱柱分离后无需氧化和紫外消解,直接由原子荧光光谱仪检测,外标法定量。结果甲基汞、乙基汞和无机汞的最佳线性范围为0~50μg/L,r>0.999 0,检出限为0.5~1.5μg/L,精密度RSD<6%,加标回收率为78%~120%,鱼肉标准物质中甲基汞测定值在参考值范围内。结论该法操作简便灵敏,结果准确可靠,适合于水产品中汞形态的测定。
Objective To establish a method for the determination of methylmercury and other forms of mercury in aquatic products by high performance liquid chromatography coupled with atomic fluorescence spectrometry. Methods The samples were sonicated with hydrochloric acid and centrifuged. The samples were separated by centrifugation with 5% acetonitrile-4.62 g / L ammonium acetate-1.2 g / L cysteine solution and separated by reversed phase C18 column without oxidation and UV digestion. By atomic fluorescence spectrometry, external standard method. Results The optimum linear range of methylmercury, ethylmercury and inorganic mercury was 0 ~ 50μg / L, r> 0.999 0, the detection limit was 0.5 ~ 1.5μg / L, RSD <6% Is 78% ~ 120%, the standard value of methylmercury fish in the reference value within the measured value. Conclusion The method is simple, sensitive and accurate. The method is suitable for the determination of mercury speciation in aquatic products.