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目的:建立Mg(OH)2共沉淀和同位素稀释电感耦合等离子体质谱(ID-ICP-MS)法测定酱油样品中的微量铅。方法:考察并优化pH值和Mg(NO3)2添加量对Pb共沉淀的影响。结果:结果表明,采用Mg(OH)2共沉淀法可有效去除酱油中大量的可溶性盐。用ID-ICP-MS测定酱油中微量Pb的平均加标回收率为93.0%,RSD≤0.4%。结论:利用建立的方法测定13种市售酱油中的微量铅,铅含量在0.01~0.21mg/L之间,均未超过相关的国家标准(GB2717-2003)限量(≤1.0mg/L)。
Objective: To establish a method for determination of trace lead in soy sauce samples by Mg (OH) 2 co-precipitation and isotope dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS). Methods: The effects of pH value and Mg (NO3) 2 addition on Pb coprecipitation were investigated and optimized. Results: The results showed that Mg (OH) 2 coprecipitation method can effectively remove a large amount of soluble salt in soy sauce. The average spiked recoveries of trace Pb in soy sauce by ID-ICP-MS were 93.0% and RSD≤0.4%. Conclusion: The trace amounts of lead and lead in thirteen commercially available soy sauce were determined by the established method. The contents of lead and lead were all within the range of 0.01-0.21 mg / L, all of which did not exceed the limit of the relevant national standard (GB2717-2003) (≤1.0 mg / L).