气相色谱-串联质谱法测定果汁中4种六六六残留量的不确定度评定  

Uncertainty evaluation in determination of 4 kinds of benzene hexachloride residues in juice by gas chromatography-tandem mass spectrometry

作　　者：张君丽[1] 张迪雅 迟恒[1] 葛驰宇[1] ZHANG Junli;ZHANG Diya;CHI Heng;GE Chiyu(Food and Pharmaceutical Research Institute,Jiangsu Food and Pharmaceutical Science College,Huai’an 223005,China)

机构地区：[1]江苏食品药品职业技术学院食品药品研究院,江苏淮安223005

出　　处：《食品与发酵工业》2023年第21期264-269,共6页Food and Fermentation Industries

基　　金：2021年江苏省“青蓝工程”中青年学术带头人资助基金。

摘　　要：为评定气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定果汁中α-六六六、β-六六六、γ-六六六、δ-六六六残留量的不确定度。采用GB 23200.113—2018《食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定气相色谱-质谱联用法》测定果汁中六六六的残留量,建立不确定度数学模型,分析测定过程中各种因素(包括样品溶液、分析仪器、方法回收率、标准系列工作溶液和标准曲线拟合)引入的不确定度。该法测定α-六六六、β-六六六、γ-六六六、δ-六六六的扩展不确定度分别为0.0086、0.0088、0.0090、0.0100 mg/kg。标准曲线拟合和标准系列工作溶液的配制是影响GC-MS/MS法测定果汁中六六六残留量不确定度的主要因素。拟合标准曲线时调整标准曲线的权重可以提高低浓度点的定量准确性。配制标准溶液时,应该选择合适的稀释方法,规范使用各类量具。This study aimed to evaluate the uncertainty for the determination ofα-benzene hexachloride(BHC),β-BHC,γ-BHC,andδ-BHC in juice by gas chromatography-tandem mass spectrometry(GC-MS/MS).GB 23200.113—2018 was used to determine the content of BHC in juice.The mathematical model of uncertainty was established to analyze the uncertainty caused by various factors in the determination process,including sample solution,analytical instrument,method recovery,standard series working solutions,and standard curve fitting.The expanded uncertainties forα-BHC,β-BHC,γ-BHC,andδ-BHC were 0.0086,0.0088,0.0090,and 0.0100 mg/kg respectively.The fitting of the standard curve and the preparation of the standard series working solutions were the main factors which affected the determination of BHC in fruit juice by GC-MS/MS.Adjusting the weight of the standard curve can improve the quantitative accuracy of the low-concentration points.During the preparation of standard solutions,an appropriate dilution method should be selected and various measuring tools should be used standardly.

关 键 词：气相色谱-串联质谱法 果汁 六六六 不确定度 标准曲线拟合 标准系列工作溶液 

分 类 号：O657.63[理学—分析化学] TS255.44[理学—化学]