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目的建立石墨消解-微波消解法测定乳粉中的总砷、总汞、铅和镉含量的分析方法。方法样品经石墨加热预消解,采用微波消解法前处理,并采用电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定乳粉中的总砷、总汞、铅和镉含量。结果总砷、总汞、铅和镉的平均加标回收率为94.4%?108.3%,精密度的相对标准差(relative standard deviation,RSD)为1.1%?4.6%,方法检出限分别为4.4、4.8、4.9、0.6?g/kg。乳粉质控样和考核样中总砷、总汞、铅和镉的测定结果均在参考值范围内,结果均为满意。结论该方法操作简便,重现性良好,测定结果准确、可靠,适用于乳粉中总砷、总汞、铅和镉的含量测定。
Objective To establish a method for the determination of total arsenic, total mercury, lead and cadmium in milk powder by graphite digestion - microwave digestion. Methods The samples were pre-digested by graphite heating and pre-treated by microwave digestion. Total arsenic, total mercury, lead and cadmium in milk powder were determined by inductively coupled plasma mass spectrometry (ICP-MS). Results The average recoveries of total arsenic, total mercury, lead and cadmium were 94.4% -108.3%, and the relative standard deviations (RSDs) were 1.1% -4.6%. The detection limits were 4.4 , 4.8, 4.9, 0.6 μg / kg. Determination of total arsenic, total mercury, lead and cadmium in milk powder quality control and assessment samples were within the reference range, the results are satisfactory. Conclusion The method is simple, reproducible and accurate. The method is accurate and reliable and is suitable for the determination of total arsenic, total mercury, lead and cadmium in milk powder.