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分步消解法ICP-MS测量大米中砷及不确定度评价

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为提高食品中重金属测定方法的准确性与可重复性、保障人民食品安全,采用石墨-微波分步消解法,使用电感耦合等离子质谱(ICP-MS)对大米中重金属砷含量进行检测,并根据试验过程对检测结果进行不确定度评定,分析测量过程中的样品称量、样品消解、标准溶液的配制、标准曲线的拟合和测量重复性等因素造成的不确定度,计算各不确定度分量,分析不确定度和扩展不确定度判断检测结果的可靠性.所测大米样品中的砷含量为0.110 mg/kg,扩展不确定度为0.011 mg/kg,k=2.通过对测量过程中不确定度的评定,试验发现该检测过程中的不确定度主要来源于样品消解和测量重复性,并与其他方法测试所得不确定度进行对比分析,结果较好.
Uncertainty Evaluation and Determination of Arsenic in Rice by ICP-MS with Stepwise Digestion Method
It was to improve the accuracy and repeatability of the determination method of heavy metals in food and to ensure people's food safety.The content of heavy metal arsenic in rice was detected by ICP-MS with graphite-microwave stepwise digestion method.The uncertainty of the detection results was evaluated according to the experimental process.The uncertainty caused by sample weighing,sample digestion,preparation of standard solution,fitting of standard curve,measurement repeatability and other factors in the measurement process was analyzed.The component of uncertainty was quantified,and the reliability of detection results was evaluated by the results of synthetic uncertainty and extended uncertainty.The content of arsenic in rice samples was 0.110 mg/kg.The extended uncertainty was 0.011 2 mg/kg(k=2).On the basis of the evaluation of the uncertainty in the measurement process,it was found that the uncertainty in the measurement process mainly came from sample digestion and repeatability.The result was well by comparing and analyzing with the other methods.

stepwise digestionricearsenicuncertainty

卢鑫、刘聪、陈燕敏、刘冰、侯金妹

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郑州师范学院化学化工学院(郑州 450044)

安徽泽众安全科技有限公司(合肥 232000)

清华大学合肥公共安全研究院(合肥 230601)

分步消解 大米 不确定度

安徽省重大科技专项

202203a07020034

2024

食品工业
上海市食品工业研究所

食品工业

影响因子:0.47
ISSN:1004-471X
年,卷(期):2024.45(1)
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