气相色谱法测定茶鲜叶中4种有机磷农药残留量的不确定度分析  

Evaluation of Uncertainty in Determination of Four Organophosphorus Pesticide Residues in Fresh Tea Leaves by Gas Chromatography

作　　者：刘腾飞[1] 张丽[2] 杨代凤[1] 朱松[3] 周锋杰 LIU Tengfei;ZHANG Li;YANG Daifeng;ZHU Song;ZHOU Fengjie(Jiangsu Taihu Area Institute of Agricultural Sciences,Suzhou 215105,China;Center for Food Safety and Nutrition,Suzhou Vocational University,Suzhou 215104,China;State Key Laboratory of Food Science and Technology,Jiangnan University,Wuxi 214122,China;Suzhou Agricultural Products Safety and Quality Inspection Center,Suzhou 215128,China)

机构地区：[1]江苏太湖地区农业科学研究所,江苏苏州215105 [2]苏州市职业大学食品安全与营养研究中心,江苏苏州215104 [3]江南大学食品科学与技术国家重点实验室,江苏无锡214122 [4]苏州市农产品质量安全监测中心,江苏苏州215128

出　　处：《食品工业科技》2023年第1期323-331,共9页Science and Technology of Food Industry

基　　金：江苏省农业科技自主创新资金项目[CX(21)3055];浙江省农药残留检测与控制研究重点实验室开放课题(2021PRG007)。

摘　　要：采用气相色谱外标法对茶鲜叶中敌敌畏、乐果、马拉硫磷和杀螟硫磷4种农药残留量进行测定,依据不确定度评定的相关标准及规范,建立不确定度评定的数学模型,对整个检测过程中不确定度进行系统性评价,包括样品测定重复性、标准曲线拟合、添加回收率3个A类评定分量,以及标准溶液配制、样品称量和前处理、仪器测定4个B类评定分量。结果显示:当茶鲜叶中敌敌畏、乐果、马拉硫磷、杀螟硫磷的残留量分别为0.096、0.39、0.19、0.19 mg/kg时,其扩展不确定度分别为0.021、0.073、0.036、0.023 mg/kg(k=2,置信概率P=95%)。标准溶液配制及标准曲线拟合是引入不确定度的主要因素,在今后的检测过程中应加以重点关注。该评定结果为客观评价茶鲜叶中4种有机磷农药残留检测结果的准确性提供了参考。Aim to evaluate the uncertain factors which may influence the accuracy of detection of pesticide residues in fresh tea leaves,a case study of dichlorvos,dimethoate,malathion and fenitrothion residues in fresh tea leaves was carried out using gas chromatography with external standard method.According to the relevant standard and protocol,a mathematical model has been studied.The uncertainties created by the entire experimental process were evaluated systematically.Three A-type evaluation components,including reproducibility of determination,fitness of standard curve and recovery rate,and four B-type evaluation components,including preparation of standard solution,sample weighing and pretreatment,and the measurement of instrument were investigated.The results revealed that the expanded uncertainty of measured values of dichlorvos,dimethoate,malathion and fenitrothion in the spiked tea leaves were 0.021,0.073,0.036 and 0.023 mg/kg(k=2,confidence interval P=95%),while the theoretical content were 0.096,0.39,0.19 and 0.19 mg/kg,respectively.Preparation of standard solution and fitness of standard curve contributed to the major effect on uncertainty,which should be paid more attention for future determination.Our study provides a reference for the accuracy assessment of method in detection of four organophosphorus pesticide residues in fresh tea leaves.

关 键 词：气相色谱法 茶鲜叶 有机磷农药 不确定度 

分 类 号：S481.8[农业科学—农药学]