园林土壤中氯氰菊酯残留量测定的不确定度评定分析  

Uncertainty evaluation for the determination of cypermethrin residue in landscape soil

作　　者：罗红雨 陆皓茜[2] 施林林[2] 周锋杰 Luo Hongyu;Lu Haoqian;Shi Linlin;Zhou Fengjie(Suzhou Liuyuan Management Office,Suzhou 215006,China;Jiangsu Taihu Area Institute of Agricultural Sciences,Suzhou 215106,China;Suzhou Agricultural Products Safety and Quality Inspection Center,Suzhou 215128,China)

机构地区：[1]苏州市留园管理处,江苏苏州215006 [2]江苏太湖地区农业科学研究所,江苏苏州215106 [3]苏州市农产品质量安全监测中心,江苏苏州215128

出　　处：《江苏林业科技》2024年第1期11-16,共6页Journal of Jiangsu Forestry Science & Technology

基　　金：江苏省农业科技自主创新资金项目“有机物料驱动太湖地区农田土壤质量及碳库演变的长期定位观测研究”[CX(22)3005];苏州市科技计划项目“生态敏感区HDPE沼液稻田消纳适宜承载量及关键技术研究”(SNG221015)。

摘　　要：不确定度评定分析对于检测方法的改进和定量评价检测结果的质量具有重要意义。采用分散固相萃取-气相色谱法测定园林土壤中氯氰菊酯的残留量,对测定过程中产生不确定度的主要来源进行分析,包括样品重复测量、标准溶液配制、标准曲线拟合、样品称量和前处理、回收率和气相色谱仪测定,并对各分量进行量化、合成与扩展。结果显示,氯氰菊酯农药在0.10 mg/kg添加水平下,各分量的相对标准不确定度分别为7.03×10^(-3),3.00×10^(-2),1.63×10^(-2),8.17×10^(-3),1.12×10^(-2),1.32×10^(-2)和8.66×10^(-3);相对合成标准不确定度为9.72×10^(-3),扩展不确定度为0.0018 mg/kg;当置信水平为95%(k=2)时,测定结果可表示为(0.090±0.0018)mg/kg。通过评定发现,不确定度的主要影响因素是标准溶液的配制、标准曲线的拟合和回收率,提示在样品检测过程中需严格控制这几个环节。该研究为分散固相萃取-气相色谱技术测定园林土壤中氯氰菊酯残留量检测方法的改进和检测结果的评价提供了参考。The evaluationof uncertainty is of great importance for improving detection methods and quantitatively characterizing the quality of determination results.In this study,a method based on dispersive solid phase extraction(d-SPE)and gas chromatography(GC)was utilized to quantify cypermethrin residue in landscape soil.The key sources of uncertainty in the measurement process were evaluated,including repeated determination of samples,standard solution preparation,fitness of standard curve,sample weighing and pretreatment,recovery rate,and the measurement of GC.Each uncertainty component was quantified and subsequently combined and expanded following the law of propagation of uncertainty.The results showed that when landscape soil was spiked with cypermethrin at a concentration level of 0.10 mg/kg,the relative standard uncertainty of each component were 7.03×10^(-3),3.00×10^(-2),1.63×10^(-2),8.17×10^(-3),1.12×10^(-2),1.32×10^(-2) and 8.66×10^(-3),respectively.The relative combined standard uncertainty was calculated to be 9.72×10^(-3),and the expanded uncertainty was determined to be 0.0018 mg/kg.The determination results of cypermethrin in landscape soil in 95% confidence interval could be expressed as(0.090±0.0018)mg/kg(k=2).Based on uncertainty evaluation,the main sources of uncertainty came from standard solution preparation,standard curve fitting and recovery rate,indicating that these aspects should be controlled strictly in the following sample analysis.The findings could provide a valuable reference for improving and assessing the accuracy of the d-SPE-GC method for the determination of cypermethrin residue in landscape soil.

关 键 词：气相色谱法 园林土壤 氯氰菊酯 不确定度 分析 

分 类 号：S481.8[农业科学—农药学]