背景:新烟碱(NEO)用于薄荷的植物检疫处理。L作物,这种做法要求在非常低的浓度下精确控制这些有害物质。
目的:本研究的目的是应用一种基于总误差方法学的同时验证和评估测量不确定度的方法。为了准确量化MenthaSpicata中两个近地天体的存在。我用一个快速的,Easy,便宜,有效,Rugged,和安全(QuEChERS)-LC-MS/MS方法。
方法:采用QuEChERS提取方法对吡虫啉和啶虫脒进行定量,与LC-MS/MS相结合,确保分析方法的准确性,并管理与其常规使用相关的风险。基于β含量的完整而详尽的验证方法,γ-置信公差区间用于不确定度评估,利用广义枢轴量(GPQ)概念和蒙特卡罗模拟,这避免了对额外数据的需要,同时在预定可接受的限度内实现每个浓度水平的中间精度。
结果:验证程序基于两个近地天体的二次模型的选择,允许在工作浓度范围内通过LC-MS/MS测定法验证啶虫脒和吡虫啉。通过β含量值(66.7、80和90%)和风险值(10和5%)的变化证明了不确定性分布区间的灵活性,保持在20%的可接受性范围内,相对扩展不确定度不超过15%和11%。
结论:用于分析两个近地天体的QuEChERS-LC-MS/MS方法已使用不确定度曲线策略成功地得到了充分验证。
结论:实施总体验证策略,其中包括验证和不确定性评估,称为不确定性曲线,用于对MenthaSpicata的两个重要近地天体进行量化。L使用QuEChERS-LC-MS/MS这种定性方法是通过在每个浓度水平的中间精度条件下利用分析验证的数据来计算方法的测量不确定性而进行的,而无需额外的努力。之后,我们证明了该策略用于啶虫脒和吡虫啉的LC-MS/MS定量的灵活性,使用能够选择和修改β含量和γ置信度值的决策工具。
BACKGROUND: Neonicotinoids (NEOs) are used for the phytosanitary treatment of Mentha Spicata.L crops, and this practice requires precise control of these harmful substances at very low concentrations.
OBJECTIVE: The objective of this study is to apply an approach allowing simultaneously validation and evaluation of measurement uncertainty based on total error methodology, in order to accurately quantify the presence of two NEOs in Mentha Spicata.L utilizing a Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS)-LC-MS/MS methodology.
METHODS: The quantification of imidacloprid and acetamiprid employing a QuEChERS extraction method, coupled with LC-MS/MS, ensuring the accuracy of the analytical method and managing the risks associated with its routine use. A complete and exhaustive validation approach based on the \"β-content, γ-confidence\" tolerance interval was used for the uncertainty assessment, using the generalized pivot quantity (GPQ) concept and Monte Carlo simulation, which avoids the need for additional data while achieving intermediate precision for each concentration level within predetermined acceptable limits.
RESULTS: The validation procedure is based on the choice of a quadratic model for the two NEOs, allowing the validation of acetamiprid and imidacloprid by LC-MS/MS assay within the range of working concentration. The flexibility of the uncertainty profile intervals was demonstrated with a variation in β-content values (66.7, 80, and 90%) and risk values (10 and 5%), which remained within the acceptability limits of 20%, and the relative expanded uncertainty did not exceed 15 and 11%.
CONCLUSIONS: A QuEChERS-LC-MS/MS method for the analysis of two NEOs has been successfully fully validated using the uncertainty profile strategy.
CONCLUSIONS: Implementation of an overall validation strategy, which involves both the validation and uncertainty assessment known as the uncertainty profile, for the quantification of two important NEOs in Mentha Spicata.L using QuEChERS-LC-MS/MS. This qualimetric approach has been conducted by computing the measurement uncertainty of the method utilizing data from analytical validation under conditions of intermediate precision at each level of concentration without additional effort. After that we have demonstrated the flexibility of this strategy for the LC-MS/MS quantification of acetamiprid and imidacloprid, using a decision tool that enables the choice and modification of β-content and γ-confidence values.