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目的建立微波消解-电感耦合等离子体质谱法(ICP-MS)准确测定各类食品中痕量汞、镉、铅、砷的分析方法。方法采用微波消解法处理样品,ICP-MS测定以72Ge、103Rh、185Re作为内标消除非质谱干扰,八极杆碰撞池(ORS3)消除质谱干扰。结果采用本方法测定汞、镉、铅、砷的定量限分别为0.05、0.05、0.40、0.40μg/L;在定量限附近测定的回收率和相对标准偏差分别为:100.0%、90.0%、96.0%、112.0%和7.6%、8.0%、11.8%、6.2%。结论采用ICP-MS法准确测定食品中痕量有害元素的关键点及控制措施,适用于食品安全风险监测大批量样品的分析。
Objective To establish a method for the accurate determination of trace mercury, cadmium, lead and arsenic in various foods by microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS). Methods The samples were treated by microwave digestion. The mass spectrometry interferences were eliminated by ICP-MS using 72Ge, 103Rh and 185Re as internal standards and the interference of octopole collision cell (ORS3). Results The limit of quantification of mercury, cadmium, lead and arsenic were 0.05,0.05,0.40 and 0.40μg / L, respectively. The recoveries and relative standard deviations (RSDs) of the method were 100.0%, 90.0% and 96.0 %, 112.0% and 7.6%, 8.0%, 11.8%, 6.2%. Conclusion The key points and control measures for the determination of trace harmful elements in food by ICP-MS are suitable for the analysis of large quantities of food safety risk monitoring samples.