不同液相色谱-串联质谱法检测标准测量不确定度的评定  

Evaluation of Measurement Uncertainty for Different Detection Standards of Liquid Chromatography-Tandem Mass Spectrometry

作　　者：韩帅兵 张耀中[1] 于淼 薛雯 李向阳[1] 吴亚玉[1] 周力[1] Han Shuaibing;Zhang Yaozhong;Yu Miao;Xue Wen;Li Xiangyang;Wu Yayu;Zhou Li(Shandong Institute of the Control of Agrochemicals,Jinan Shandong 250100,China)

机构地区：[1]山东省农药检定所,山东济南250100

出　　处：《农药科学与管理》2021年第6期41-48,共8页Pesticide Science and Administration

摘　　要：分别依据标准方法GB/T 20769-2008《水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法》和GB 23200.121-2021《食品安全国家标准植物源性食品中331种农药及其代谢物残留量的测定液相色谱-质谱联用法》,对大白菜中吡虫啉的残留量测定进行了不确定度评定。通过对两种方法测定步骤的具体分析并建立相应的数学模型,详细评定了包括标准溶液、样品称量、前处理过程、标准溶液峰面积、样品峰面积及方法精密度在内的不确定度分量,并计算出两种方法各自的合成相对标准不确定度及相对扩展不确定度。结果显示,在相同实验室条件下,在95%的置信限(k=2)内,方法GB 23200.121-2021的测量相对扩展不确定度为4.0%,小于GB/T 20769-2008的测量相对扩展不确定度5.6%;决定方法GB 23200.121-2021不确定度大小的关键因素为标准溶液(占比64.3%);决定方法GB/T 20769-2008不确定度大小的关键因素为标准溶液(占比33.1%)和方法精密度(占比51.7%)。The uncertainties of the method to determine imidacloprid residues in Chinese cabbage were evaluated,according to“GB 23200.121-2021 National food safety standard Determination of 331 pesticides and metabolites Residues in foods of plant origin Liquid chromatography-tandem mass spectrometry method”and“GB/T 20769-2008 determination of 450 pesticides and related chemicals residues in fruits and vegetables LC-MS-MS method”.The uncertainty components including standard solution,sample weighing,pretreatment process,peak area of standard solution,peak area of sample and method precision were evaluated in detail by analyzing the determination steps of the two methods and establishing corresponding mathematical models.The combined relative standard uncertainty and relative expanded uncertainty of each method were calculated.The results showed that under the same laboratory conditions,within the 95%confidence limit(k=2),the relative expanded uncertainty of GB 23200.121-2021 is 4.0%,which is less than 5.6%of GB/T 20769-2008.The key factors affecting the uncertainty of method GB 23200.121-2021 were standard solution(accounting for 64.3%),and those of method GB/T 20769-2008 were standard solution(33.1%)and method precision(51.7%).

关 键 词：不确定度 液相色谱-串联质谱 检测 残留量 

分 类 号：S482[农业科学—农药学] O657.72[农业科学—植物保护]