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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
【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。
【Abstract】 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.
【Key words】 microwave digestion; rapid digestion; ICP-MS; rice flour;
- 【文献出处】 现代食品 ,Modern Food , 编辑部邮箱 ,2022年18期
- 【分类号】O657.63;TS210.7
- 【下载频次】83