Background Triple quadrupole (MS/MS) and high-resolution mass spectrometry (HRMS), coupled with ultra-high performance (UHP) liquid chromatography (LC) or gas chromatography (GC), are technologies used to analyze pesticide residues in fruits and vegetables. LC-MS/MS has been the gold standard for analysis of pesticides, offering reliable performance and sensitivity, while LC-HRMS is expanding in application to serve as another benchmark. Method development and testing scope expansion are constantly required with new generation mass spectrometers. Objective This article discusses the development and validation of a quantitative and confirmatory method that can analyze over 400 pesticide residues using a state-of-the-art UHPLC/electrospray ionization (ESI)-MS/MS system. Methods Homogenized fruit and vegetable samples were fortified with pesticides and were extracted using a modified quick, easy, cheap, effective, rugged, and safe method. Samples were injected onto a UHPLC/ESI-MS/MS system, and data were acquired in multiple reaction monitoring (MRM) mode. The method was validated using a nested experimental design, and was able to quantify and confirm 416 pesticides in fruits and vegetables. It was also complimentary to the UHPLC/ESI Q-Orbitrap quantitative and screening methods previously developed in the authors’ laboratory. Results The method demonstrated good performance. In all matrixes, 92% of pesticides yielded recoveries between 81–110%, more than 95% of pesticides yielded intermediate precision ≤20%, about 65% of pesticides yielded measurement uncertainties ≤20%, and 96% of pesticides yielded measurement uncertainties ≤50%. Conclusion This method shows great potential to be a standalone method or as part of a laboratory workflow for quantitative and confirmatory analysis of pesticide residues in fruits and vegetables. Highlights This method was developed using the same mobile phases, analytical columns, and extraction procedure, as UHPLC/ESI Q-Orbitrap methods. Extracts can be run on either system, streamlining monitoring programs and offering high sample throughput.

中文翻译：

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基于 UPHLC/ESI-MS/MS 分析水果和蔬菜中 416 种农药的 UHPLC/ESI Q-Orbitrap 筛选的补充、定量和确证方法

背景 三重四极杆 (MS/MS) 和高分辨率质谱 (HRMS) 以及超高效 (UHP) 液相色谱 (LC) 或气相色谱 (GC) 是用于分析水果和蔬菜中农药残留的技术. LC-MS/MS 一直是农药分析的黄金标准，具有可靠的性能和灵敏度，而 LC-HRMS 正在扩大应用范围以作为另一个基准。新一代质谱仪不断需要方法开发和测试范围的扩展。目的 本文讨论了使用最先进的 UHPLC/电喷雾电离 (ESI)-MS/MS 系统分析 400 多种农药残留的定量和确证方法的开发和验证。方法 均质的水果和蔬菜样品用农药强化，并使用改进的快速、简单、便宜、有效、耐用和安全的方法进行提取。将样品注入 UHPLC/ESI-MS/MS 系统，并以多反应监测 (MRM) 模式获取数据。该方法使用嵌套实验设计进行了验证，能够量化和确认水果和蔬菜中的 416 种农药。它还补充了作者实验室之前开发的 UHPLC/ESI Q-Orbitrap 定量和筛选方法。结果该方法表现出良好的性能。在所有基质中，92% 的农药的回收率在 81-110% 之间，超过 95% 的农药的中间精密度≤20%，约 65% 的农药的测量不确定度≤20%，96% 的农药的测量不确定度≤50%。结论 该方法显示出作为独立方法或作为实验室工作流程的一部分对水果和蔬菜中农药残留进行定量和确证分析的巨大潜力。亮点 该方法是使用与 UHPLC/ESI Q-Orbitrap 方法相同的流动相、分析柱和萃取程序开发的。提取物可以在任一系统上运行，从而简化监测程序并提供高样品通量。作为 UHPLC/ESI Q-Orbitrap 方法。提取物可以在任一系统上运行，从而简化监测程序并提供高样品通量。作为 UHPLC/ESI Q-Orbitrap 方法。提取物可以在任一系统上运行，从而简化监测程序并提供高样品通量。