Jesús Florencia, Cutillas Víctor, Aguilera Del Real Ana M, Fernández-Alba Amadeo Rodríguez
European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, University of Almeria, Agrifood Campus of International Excellence (ceiA3), Ctra. Sacramento s/n, La Cañada de San Urbano, 04120, Almería, Spain.
Pesticide Residue Research Group, Department of Chemistry and Physics, University of Almería, Agrifood Campus of International Excellence (ceiA3), Ctra Sacramento s/n La Cañada de San Urbano, 04120, Almería, Spain.
Anal Chim Acta. 2025 Jul 8;1358:344100. doi: 10.1016/j.aca.2025.344100. Epub 2025 Apr 21.
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.
This study assessed the performance of a micro-flow LC system operating at a flow rate of 50 μL min, 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), 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.
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.
对水果和蔬菜中的农药残留进行可靠分析对于食品安全和法规合规至关重要。传统上，分析型液相色谱-质谱联用（LC-MS/MS）一直是金标准，但转向低流量LC-MS/MS提供了一种改进的替代方案，可提高灵敏度、减少样品进样量并符合绿色分析化学的原则。以微流量运行可显著减少溶剂消耗和有机废物，这对常规控制实验室尤为重要。这种方法保持了高灵敏度、稳健性和性能，满足了对更绿色、高效和可靠的多残留农药分析方法的迫切需求。
本研究评估了一个流速为50 μL/min的微流量液相色谱系统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的性能，该方法符合ISO 17025标准。该方法显示出出色的保留时间稳定性，在50次进样中偏差低于2.1秒。峰面积重复性良好，番茄的相对标准偏差为3.4%，橙子为2.9%。仪器定量限显示出高灵敏度，89%的农药在极低浓度（0.001 - 0.002 mg/kg）下被鉴定出来，优于传统的分析型液相色谱-质谱联用方法，后者鉴定出75 - 81%的化合物。基质效应最小，大多数化合物的信号抑制或增强小于20%。该方法通过能力验证样品分析成功进行了测试，对39个实际样品的分析证明了其在常规食品监测中的适用性。
本工作确立了微流量LC-MS/MS作为水果和蔬菜中多残留农药分析的创新方法，将高分析性能与显著的可持续性优势相结合，与传统分析型方法相比，溶剂消耗减少了五倍以上。这些优势突出了微流量LC-MS/MS作为多残留农药分析的一种有前途、高效且环保的选择，使其成为食品安全分析中更广泛采用的有价值工具。
