Advancements in multiresidue pesticide analysis in fruits and vegetables using micro-flow liquid chromatography coupled to tandem mass spectrometry

IF 5.7 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta Pub Date : 2025-04-21 DOI:10.1016/j.aca.2025.344100

Florencia Jesús , Víctor Cutillas , Ana M. Aguilera del Real , Amadeo Rodríguez Fernández-Alba

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Abstract

Background

A reliable analysis of pesticide residues in fruits and vegetables is crucial for food safety and regulatory compliance. Traditionally, analytical-flow liquid chromatography coupled to mass spectrometry (LC-MS/MS) has been the gold standard but, shifting to low-flow LC-MS/MS presents an improved alternative that enhances sensitivity, reduces the injected amount of sample and aligns with the principles of green analytical chemistry. Operating at micro-flow rates significantly reduces solvent consumption and organic waste, which is particularly important for routine control laboratories. This approach maintains high sensitivity, robustness, and performance, addressing the critical need for greener, efficient, and reliable methodologies for multiresidue pesticide analysis.

Results

This study assessed the performance of a micro-flow LC system operating at a flow rate of 50 μL min⁻¹, coupled to a triple quadrupole mass spectrometer, for the multiresidue analysis of 257 pesticides in tomato and orange matrices, in compliance with the ISO 17025. The method showed excellent retention time stability, with deviations under 2.1 s across 50 injections. Peak area repeatability was robust, with relative standard deviations of 3.4 % for tomato and 2.9 % for orange. The instrumental limits of quantification demonstrated high sensitivity, with 89 % of pesticides identified at very low concentrations (0.001–0.002 mg kg⁻¹), outperforming the traditional analytical-flow LC-MS/MS method, which identified 75–81 % of compounds. Matrix effects were minimal, with less than 20 % signal suppression or enhancement for most compounds. The method was successfully tested through the analysis of proficiency tests samples, and the analysis of 39 real samples proved its applicability for routine food monitoring.

Significance

This work establishes micro-flow LC-MS/MS as an innovative method for multiresidue pesticide analysis in fruits and vegetables, combining high analytical performance with significant sustainability advantages, reducing solvent consumption by over fivefold compared to the conventional analytical-flow method. These benefits underscore micro-flow LC-MS/MS as a promising, efficient, and environmentally friendly option for multiresidue pesticide analysis, positioning it as a valuable tool for broader adoption in food safety analysis.

Abstract Image

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微流液相色谱-串联质谱法在果蔬多残留农药分析中的应用进展

背景果蔬中农药残留的可靠分析对于食品安全和监管合规至关重要。传统上，分析流液相色谱-质谱联用仪（LC-MS/MS）一直是黄金标准，但改用低流量 LC-MS/MS 后，灵敏度提高了，进样量减少了，而且符合绿色分析化学的原则。以微流速运行可大大减少溶剂消耗和有机废物，这对常规控制实验室尤为重要。该方法保持了较高的灵敏度、稳健性和性能，满足了多残留农药分析对绿色、高效和可靠方法的迫切需求。结果本研究评估了微流液相色谱系统的性能，该系统的流速为 50 μL min-1，与三重四极杆质谱仪联用，用于番茄和橙子基质中 257 种农药的多残留分析，符合 ISO 17025 标准。该方法的保留时间稳定性极佳，50 次进样的偏差小于 2.1 秒。峰面积重复性良好，番茄和橙子的相对标准偏差分别为 3.4% 和 2.9%。仪器的定量限显示了很高的灵敏度，在极低浓度（0.001-0.002 mg kg-1）下就能鉴定出 89% 的农药，优于传统的分析流 LC-MS/MS，后者只能鉴定出 75-81% 的化合物。基质效应极小，大多数化合物的信号抑制或增强小于 20%。该方法通过对能力验证样品的分析进行了成功的测试，对 39 个真实样品的分析证明了它在常规食品监测中的适用性。这项工作将微流 LC-MS/MS 确立为一种创新的方法，用于水果和蔬菜中多残留农药的分析，它将高分析性能与显著的可持续发展优势相结合，与传统的分析流方法相比，溶剂消耗量减少了五倍以上。这些优势表明，微流 LC-MS/MS 是一种前景广阔、高效、环保的多残留农药分析方法，是食品安全分析领域广泛采用的重要工具。

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来源期刊

Analytica Chimica Acta 化学-分析化学

CiteScore

10.40

自引率

6.50%

发文量

1081

审稿时长

38 days

期刊介绍： Analytica Chimica Acta has an open access mirror journal Analytica Chimica Acta: X, sharing the same aims and scope, editorial team, submission system and rigorous peer review. Analytica Chimica Acta provides a forum for the rapid publication of original research, and critical, comprehensive reviews dealing with all aspects of fundamental and applied modern analytical chemistry. The journal welcomes the submission of research papers which report studies concerning the development of new and significant analytical methodologies. In determining the suitability of submitted articles for publication, particular scrutiny will be placed on the degree of novelty and impact of the research and the extent to which it adds to the existing body of knowledge in analytical chemistry.