高效液相色谱-原子荧光联用法快速测定海产品中汞形态

Rapid determination of mercury in seafood with liquid chromatography/atomic fluorescence

目的建立海产品中快速测定汞形态的方法。方法对海产品中甲基汞的液相色谱-原子荧光光谱联用测定方法进行了优化,避免使用C18小柱对样品的前处理进行净化,同时对流动相组成进行进一步的优化,使汞形态化合物的分离时间缩短至6 min以内。结果在优化条件下,3种汞形态的质量浓度为2μg/L^10μg/L时,标准曲线的浓度与其峰面积呈良好的线性关系,相关系数(r)均>0.999。无机汞、甲基汞、乙基汞的检出限(S/N=3)分别为0.073μg/L、0.131μg/L、0.135μg/L;平均回收率分别为95.8%、97.5%、94.1%,相对偏差均<10%。不同海产品的甲基汞加标回收率为83.7%~122.8%。结论该检测方法准确、快速、易操作,可满足海产品中甲基汞的检测。

Objective To establish a method for the rapid determination of mercury forms in seafood. Methods Liquid chromatography- atomic fluorescence spectrum determination method in seafood methyl mercury was optimized,avoid using C18 column purification of sample pretreatment,and to further optimize the mobile phase composition at the same time,making the mercury forms compounds separated within a shorter time to 6 min. Results Under optimized conditions,standard curve and peak area were in good linearity,when the three different forms of mercury among 2 μg / L- 10 μg / L,with the correlation coefficient（ r） all 〉0. 999. The detection limits of inorganic mercury,methyl mercury,ethyl mercury（ S / N = 3）,were respectively 0. 073 μg / L,0. 131 μg / L,0. 135 μg / L; the average recoveriey were 95. 8%,97. 5%,94. 1% respectively,and the relative deviation was less than 10%. The standard addition recoveries of methylmercury in different seafood were among 83. 7%-122. 8%. Conclusion The method is accurate,fast,easy to operate,which can meet the detection of methyl mercury in seafood.