微波消解-电感耦合等离子体质谱法同时测定粮食中6种元素含量
目的 建立微波消解-电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)同时测定粮食中铅、砷、铬、镉、汞、铝6种元素的含量, 了解粮食中重金属污染状况。方法 针对汞元素易挥发和易在仪器管路残留的问题, 优化赶酸温度、金溶液浓度、内标元素等主要影响因素。采用硝酸-过氧化氢作为消解体系, 加入金溶液, 微波消解后70 ℃赶酸, 采用ICP-MS法检测粮食加工品中6种元素的含量。结果 200个样品中6种元素含量的测定结果为: 铅0.083~0.10 mg/kg; 砷0.017~0.10 mg/kg; 铬0.059~0.19 mg/kg; 镉0.0025~0.038 mg/kg; 汞0.0054~0.015 mg/kg; 铝4.9~29 mg/kg。除铝元素目前缺失限量标准外, 铅、砷、铬、镉、汞含量的合格率为100%。方法检出限为0.0004~0.5 ng/mL, 加标回收率为88.0%~106.0%, 相对标准偏差为0.6%~2.5%, 相关系数r为0.9992~0.9999。结论 该方法简便快捷、汞残留少、准确度和精密度高, 满足粮食及相关产品中铅、砷、铬、镉、汞、铝等多元素的同时测定, 能够有效监测粮食中重金属污染状况。
Objective To establish a method for the simultaneous determination of 6 kinds of elements in grain including Pb, As, Cr, Cd, Hg and Al by inductively coupled plasma mass spectrometry (ICP-MS) combining with microwave digestion method, and understand the heavy metal pollution in grain. Methods Considering the problems of the easy volatilization and residual of Hg in instrument piping, the main factors such as temperature of acid-removing, concentrations of Au and internal elements were optimized. The sample that added Au solution was digested by nitricacid-H2O2 under microwave, and then the acid was removed at 70 ℃. Finally, the content of Pb, As, Cr, Cd, Hg and Al were determined by ICP-MS. Results The determination results of 6 kinds of elements in 200 samples were as follows: Pb 0.083~0.10 mg/kg; As 0.017~0.10 mg/kg; Cr 0.059~0.19 mg/kg; Cd 0.0025~ 0.038 mg/kg; Hg 0.0054~0.015 mg/kg; and Al 4.9~29 mg/kg. The qualified rates of Pb, As, Cr, Cd, and Hg were 100% except for Al because of a lack of limit standards. The limits of detection ranged from 0.0004 ng/mL to 0.5 ng/mL. The average recoveries ranged from 88.0% to 106.0% and the precision ranged from 0.6% to 2.5%. The calibration curve correlation coefficients ranged from 0.9992 to 0.9999. Conclusion This method is simple and fast, with low-residual of Hg, good accuracy and reproducibility, which can be used for simultaneous determination of Pb, As, Cr, Cd, Hg and Al in grain and similar samples, and can effectively monitor the heavy metal pollution in grain.
标题：微波消解-电感耦合等离子体质谱法同时测定粮食中6种元素含量
英文标题：Simultaneous determination of 6 kinds of elements in grain by inductively coupled plasma mass spectrometry combined with microwave digestion method
作者：
吴云静 河南省口岸食品检验检测所
黄姗 河南省口岸食品检验检测所
中文关键词:粮食,电感耦合等离子体质谱法,元素,
英文关键词:grain,inductively coupled plasma mass spectrometry,element,
发表日期：2018-01-04
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