微波消解ICP-MS与快速消解ICP-MS法测定大米粉质控样、盲样中铅、镉、总砷的对比研究  

A Comparative Study on Determining Lead, Cadmium and Total Arsenic in Controlled Samples and Blind Samples of Rice Flour by Microwave Digestion ICP-MS and Rapid Digestion ICP-MS

作　　者：张慧 张惠珠 牛红霞 张翠霞[1] 祝艳蕊 ZHANG Hui;ZHANG Huizhu;NIU Hongxia;ZHANG Cuixia;ZHU Yanrui(Heze Center for Disease Control and Prevention,Heze 274000,China;Heze Testing Institute for Food and Drug Control,Heze 274000,China)

机构地区：[1]菏泽市疾病预防控制中心,山东菏泽274000 [2]菏泽市食品药品检验检测研究院,山东菏泽274000

出　　处：《现代食品》2022年第18期150-153,162,共5页Modern Food

摘　　要：目的:对比微波消解和快速消解处理方法的效果,探讨两种方法的适用性和可靠性,建立快速、高效测定突发食品重金属中毒、质控考核中铅、镉、砷的方法。方法:采用微波消解和快速消解分别进行样品前处理,ICP-MS法测定,从检出限、准确度、精密度以及加标回收率等方面进行对比分析。结果:两种测定方法的检出限无显著差异,标准物质的测定值均在认定值范围之内,RSD <10%,加标回收率在88.9%~109.8%,盲样中两方法测定铅、镉、总砷的结果差异无统计学意义(Pb t=-2.423,P>0.05;Cd t=1.275,P>0.05;As t=-2.200,P>0.05),反馈的盲样考核结果为满意(Pb 0.150 mg·kg^(-1),Z=0.34;Cd 1.02 mg·kg^(-1),Z=-0.56;As 0.104 mg·kg^(-1),Z=0.57)。结论:快速消解试剂用量少、耗时短、操作简单,在突发应急检测、盲样考核中可代替微波消解进行各元素的测定。Objective: This research makes a comparative study on the effects of microwave digestion and rapid digestion, and probes into the applicability and reliability of the two methods, so as to settle on a rapid and efficient method for determining lead, cadmium and arsenic in emergent food heavy metal poisoning and quality control assessment. Method:Microwave digestion and rapid digestion are adopted to pretreat the samples, and ICP-MS is used to measure, whereby comparative analysis is made in terms of detection limit, accuracy, precision, and recovery rate. Result: Microwave digestion and rapid digestion yield to detection limit with no significant difference, and the measured values of standard substances are all within the range of certified values, RSD<10%, and the recovery of standard addition is between 88.9%~109.8%.In blind samples, the measurements of lead, cadmium and total arsenic in the two methods present no significant differences and no statistical significance(Pb t=-2.423,P>0.05;Cd t=1.275,P>0.05;As t=-2.200,P>0.05) and the feedback blind sample assessment result is satisfactory(Pb 0.150 mg·kg^(-1), Z=0.34;Cd 1.02 mg·kg^(-1), Z=-0.56;As 0.104 mg·kg^(-1), Z=0.57).Conclusion: The rapid digestion features less reagent dosage, shorter time and simpler operation, hence it can replace the microwave digestion in emergent situations and blind sample assessments to determine the elements.

关 键 词：微波消解 快速消解 ICP-MS 大米粉 

分 类 号：O657.63[理学—分析化学]