湿法消解-原子荧光光谱法同时测定油脂样品中砷和汞.doc

湿法消解-原子荧光光谱法同时测定油脂样品中砷和汞 杜洪凤 沈月华 张坤 （四川省疾病预防控制中心，四川 成都 610031） 摘要：目的 建立原子荧光光谱同时测定油脂样品中砷和汞的方法。方法 硝高酸消解油脂样品，在最佳仪器、反应条件下同时测定其中的砷和汞。结果 检出限：As0.087ng/mL、Hg0.0065ng/mL。线性范围：As0ng/mL~20 ng/mL，相关系数0.9999；Hg0ng/mL~4ng/mL，相关系数0.9996。精密度：测定10ng/mL As、2ng/mLHg混合标准试液得到的标准精密度（RSD），砷1.6%、汞2.7%。样品加标回收率：As 95.5%~101.4%、Hg92.5%~102.0%之间。结论 该方法具有较高的灵敏度、准确度、精密度和较低的检出限，满足了油脂样品中砷和汞的同时测定要求，同时也适合于食品、生物材料等样品的测定。 关键词 湿法消解；原子荧光光谱；同时测定；油脂 ；砷；汞 Synchronizing Determination of Arsenic and Mercury in Fat by Atomic Fluorescence Spectrometry Using Wet Digestion Du Hongfeng, Shen Yue-hua, Zhang Kun. (Sichuan Provincial Center for Disease Control and Prevention, Chengdu 610031, China) [Abstract] Objective]: To establish a method for the synchronizing determination of arsenic and mercury in fat by Atomic Fluorescence Spectrometry using wet digestion. Methods:Under the proposed conditions, determine arsenic and mercury in fat using wet digestion with HNO3 –HClO4. Result:The detection limits are 0.087ng/mL for arsenic and 0.0065ng/mL for mercury. The linear calibration curve for arsenic is within the range of 0~20ng/mL of which correlative coefficient is 0.9999, and for mercury is within the range of 0~4ng/mL of which correlative coefficient is 0.9996. The RSDs for arsenic at 10ng/mL and mercury at 2ng/mL are 1.6% and 2.7%, respectively. The recovery rates of spiking standards for arsenic and mercury are in the range of 95.5%~101.4% and 92.5%~102.0%, respectively. Conclusion:The determination of arsenic and mercury in fat by Atomic Fluorescence Spectrometry using wet digestion are developed with satisfactory sensitivity, accurate, precision and low detection limits. And it suits the purpose of the simultaneous determination for arsenic and mercury in food, organism materials, etc. [Key words] Wet digestion; AFS; Synchronizing determination; Fat, Arsenic; Mercury 砷、汞都是重要的卫生监测指标，其检测的方法很多。对于砷、汞测定，油脂类样品比较复杂，前处理难度大。本文就湿法消解油脂样品中，利用原子荧光光谱法同时测定砷、汞方法学指标及实际应用进行了试验研究。 1 材料与方法 1.1 仪器与试剂 1.1.1 仪器及器材 A