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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 rapid method for determination of mercury speciation in seafood. Methods The determination of methylmercury in seafood by liquid chromatography-atomic fluorescence spectrometry was optimized to avoid the pretreatment of the sample with C18 column, and the mobile phase composition was further optimized to make the mercury form The compound separation time is shortened to 6 min. Results Under the optimum conditions, the concentration of standard curve was linear with the peak area when the concentration of 3 mercury species was 2μg / L ~ 10μg / L, the correlation coefficient (r) was> 0.999. The detection limits (S / N = 3) of inorganic mercury, methylmercury and ethylmercury were 0.073μg / L, 0.131μg / L and 0.135μg / L, respectively.The average recoveries were 95.8%, 97.5%, 94.1 %, Relative deviation <10%. Different marine products methylmercury spiked recoveries of 83.7% ~ 122.8%. Conclusion The detection method is accurate, rapid and easy to operate, which can meet the detection of methylmercury in seafood.