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食品研究与开发:2022,43(13):141-146
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两种消解方法对ICP-MS检测小麦粉中Pb、As、Cd、Cr的影响
(1.浙江大学中原研究院,河南 郑州 450001;2.河南三方元泰检测技术有限公司,河南 郑州 450001)
Effects of Two Digestion Methods on the Detection of Pb,As,Cd and Cr in Wheat Flour by ICP-MS
(1.Zhejiang University Zhongyuan Institute,Zhengzhou 450001,Henan,China;2.Henan Sanfang Yuantai Testing Technology Co.,Ltd.,Zhengzhou 450001,Henan,China)
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投稿时间:2021-05-27    
中文摘要: 为比较微波消解法和湿法消解法两种前处理方法对电感耦合等离子体质谱(inductively coupled plasma-mass spectrometry,ICP-MS)测定小麦粉中铅(Pb)、砷(As)、镉(Cd)、铬(Cr)4种元素含量的影响,称取样品适量,分 3个浓度梯度加标,同时做6组平行试验,加标后分别用微波消解法和湿法消解法处理,消解完全后用去离子水定容,使用ICP-MS同时测定 Pb、As、Cd、Cr,以外标法定量,同时用内标元素铟(In)在线校正,以能动甄别(kinetic energy discrimination,KED)模式消除质谱干扰,最后以标准样品验证,同时分析比较两种前处理方法的消解时间和试剂消耗量。结果表明,Pb、As、Cd、Cr在 0~100 μg/L 具有良好的线性关系,相关系数均超过 0.999 5,检出限为0.010 μg/L~0.117 μg/L,加标回收率为80.3%~104.4%,精密度(n=6)为1.71%~8.65%;微波消解法消解平均用硝酸5 mL、过氧化氢2 mL,用时2.55 h;湿法消解法消解平均用硝酸20.5 mL、高氯酸2 mL,用时7.03 h。
Abstract:This article aimed to compare the effects of microwave digestion and wet digestion on the determination of lead(Pb),arsenic(As),cadmium(Cd),and chromium(Cr)in wheat flour by inductively coupled plasma-mass spectrometry(ICP-MS).Appropriate amount of sample was made into in three concentration gradients with six parallels for each gradient.Then,samples were treated by microwave digestion and wet digestion,respectively,and diluted to the scale with deionized water.The content of Pb,As,Cd and Cr in samples was determined by ICP-MS with external standard method,and the internal standard indium (In)was used for on-line calibration.The interferences in MS were eliminated by kinetic energy discrimination(KED)and finally standard sample was used for verification.The digestion time and reagent consumption of the two preprocessing methods were compared.The analysis indicated that the four elements showed good linearity in the range of 0-100 μg/L.The correlation coefficients were all over 0.999 5 and the detection limits were 0.010 μg/L-0.117 μg/L.The recoveries were 80.3%-104.4% and relative standard deviation (n=6)were 1.71%-8.65%.Microwave digestion took 2.55 h with 5 mL nitric acid and 2 mL hydrogen peroxide,and wet digestion cost about 7.03 h with 20.5 mL nitric acid and 2 mL perchloric acid.
文章编号:202213021     中图分类号:    文献标志码:
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