气相色谱法测定韭菜中腐霉利含量的不确定度评估
Uncertainty evaluation of determination of procymidone in Chinese chive by gas chromatography
纪卫红 1王欣 1郭文丽1
作者信息
- 1. 天津市食品安全检测技术研究院仪器分析部 天津 300308
- 折叠
摘要
本实验采用QuEChERS前处理,气相色谱法(QuEChERS-GC-ECD)检测韭菜中的腐霉利含量,并做出不确定度评估.以JJF 1059.1-2012《测量不确定度评定与表示》和CNAS-GL006《化学分析中不确定度的评估指南》为指导,通过分析梳理各个检测环节,找出可能影响检测结果准确性的多个不确定因素,并对其做出系统分析、科学评估和量化处理.结果显示,引入本法不确定度的环节包括:标准溶液配置(标准物质及定容过程)、样品前处理(样品称量及试剂移取过程)、样品的重复性测定过程及仪器本身性能引入的不确定度.得到了韭菜中腐霉利含量测定的合成相对标准不确定度为 0.335 mg/kg,扩展不确定度为 0.670 mg/kg,本实验测得的腐霉利含量结果可表示为(8.24±0.670)mg/kg,k=2.建立了该分析方法的数学模型,为提高该法测定结果的准确性、科学性、稳定性提供了技术支撑.
Abstract
In this experiment,QuEChERS pretreatment and Gas Chromatography(QuEChERS-GC-ECD)were used to detect the content of procymidone in Chinese chive,and the uncertainty was evaluated.The method was based on JJF 1059.1-2012 Evaluation and Expression of Measurement Uncertainty and CNAS-GL006 Guide for Evaluation of Uncertainty in Chemical Analysis.Through the analysis and sorting of the whole testing process,multiple uncertain factors that may affect the accuracy of testing results were found.After making systematic analysis,scientific evaluation and quantitative treatment of these uncertainty components,it is finally found that the uncertainty sources of this method mainly include the standard material configuration(reference material and constant volume process),sample pretreatment(sample weighing and reagent transfer process),sample repeatability determination process and the uncertainty introduced by the instrument.The synthetic relative standard uncertainty was 0.335 mg/kg,and extended uncertainty was 0.670 mg/kg.The content of procymidone obtained in this experiment can be expressed as(8.24±0.670)mg/kg,k=2.The mathematical model of the analysis method was established,which provided technical support for improving the accuracy,scientificity and stability of the determination results of the method.
关键词
气相色谱/韭菜/腐霉利/不确定度Key words
Gas chromatography/Chinese chive/Procymidone/Uncertainty引用本文复制引用
出版年
2024
NETL
NSTL
万方数据