湿法消解-原子荧光光谱法同时检测海产品中的总砷与总汞

Simultaneous determination of total arsenic and total mercury in seafood by wet digestion-atomic fluorescence spectrometry

目的建立湿法消解-原子荧光光谱法同时测定海产品中总砷、总汞含量的分析方法。方法采取硝酸、高氯酸和硫酸混合体系的冷消解及热消解结合的方法,并采用电炉高温短时间加热的优化条件进行消解样品,利用氢化物原子荧光光谱法同时进行总砷、总汞的测定。结果砷在0～40μg/L浓度范围内呈良好线性关系,汞在0～12μg/L浓度范围内呈良好线性关系,相关系数均大于0.999。砷的检出限为0.037μg/L,回收率为94.36%～96.62%,精密度为0.86%～1.36%,汞的检出限为0.048μg/L,回收率为93.33%～95.28%,精密度为0.88%～2.62%。通过对能力验证HMRL1601海鱼粉中总汞、总砷的检测,检测结果总汞为0.30 mg/kg,总砷为2.06 mg/kg,均为满意结果,黄鱼、紫菜质控样的检测值均在参考值允许范围内。结论该方法操作简便、准确灵敏,适用于每一个实验室开展海产品中总砷总汞的同时测定。

Objective To establish a method for the simultaneous determination of total arsenic and total mercury in seafood by wet digestion-atomic fluorescence spectrometry. Methods Samples were digested by combination of cold digestion and heat digestion with mixed acid（nitric acid, perchloric acid and sulfuric acid）, and adopting the improved condition of short time heating with high temperature. Total arsenic and total mercury were simultaneously determined by hydride generation atomic fluorescence spectrometry. Results There were good linear relationships of arsenic and mercury within the concentration ranges of 0～40 μg/L and 0～12 μg/L, respectively, and correlation coefficients were greater than 0.999. The limits of detection of arsenic and mercury were 0.037 μg/L and 0.048 μg/L, the recovery rates were 94.36%～96.62% and 93.33%～95.28%, and the precisions were 0.86%～1.36% and 0.88%～2.62%, respectively. According to the proficiency test of total mercury and total arsenic of HMRL1601 sea fish powder, the detection results of total mercury and total arsenic were 0.30 mg/kg and 2.06 mg/kg, which were both satisfied, and the detection values of yellow croaker and laver quality control samples were within the reference ranges. Conclusion The established method is simple, accurate and sensitive, which is suitable for each laboratory to carry out the simultaneous determination of total arsenic and total mercury in seafood.