首页|园林土壤中氯氰菊酯残留量测定的不确定度评定分析

园林土壤中氯氰菊酯残留量测定的不确定度评定分析

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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 0.001 8 mg/kg;当置信水平为 95%(k=2)时,测定结果可表示为(0.090±0.001 8)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.
Uncertainty evaluation for the determination of cypermethrin residue in landscape soil
The evaluationof uncertainty is of great importance for improving detection methods and quantitatively characteri-zing 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 uncer-tainty of each component were 7.03×10-3,3.00×10-2,1.63×10-2,8.17×10-3,1.12×10-2,1.32×10-2and 8.66×10-3,re-spectively.The relative combined standard uncertainty was calculated to be 9.72×10-3,and the expanded uncertainty was determined to be 0.001 8 mg/kg.The determination results of cypermethrin in landscape soil in 95%confidence interval could be expressed as(0.090±0.001 8)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 assess-ing the accuracy of the d-SPE-GC method for the determination of cypermethrin residue in landscape soil.

Gas chromatographyLandscape soilCypermethrinUncertaintyAnalysis

罗红雨、陆皓茜、施林林、周锋杰

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苏州市留园管理处,江苏 苏州 215006

江苏太湖地区农业科学研究所,江苏 苏州 215106

苏州市农产品质量安全监测中心,江苏 苏州 215128

气相色谱法 园林土壤 氯氰菊酯 不确定度 分析

江苏省农业科技自主创新资金项目苏州市科技计划项目

CX223005SNG221015

2024

江苏林业科技
江苏省林业科学研究院 江苏省林业科技情报中心

江苏林业科技

影响因子:0.461
ISSN:1001-7380
年,卷(期):2024.51(1)
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