Verdini Emanuela, Pacini Tommaso, Orsini Serenella, Sdogati Stefano, Pecorelli Ivan
Chemistry Department, Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche "Togo Rosati", 06126 Perugia, Italy.
Foods. 2024 Sep 30;13(19):3131. doi: 10.3390/foods13193131.
The detection and quantification of polar pesticides in liquid chromatography coupled with mass spectrometry present significant analytical challenges. This study compares the performance of three LC columns (Hypercarb™, Raptor Polar X™, and Anionic Polar Pesticide™) in separating and quantifying eleven polar pesticides in chicken eggs using a score-based methodology. Analytes include glyphosate, its metabolites, and other high-polarity pesticides like Ethephon, Glufosinate, and Fosetyl aluminum, included in the EU's official control plan. Polar pesticides, characterized by high polarity and hydrophilicity, lead to analytical issues such as poor retention and unconventional peak shapes with traditional reversed-phase methods. Their weak interaction with hydrophobic stationary phases complicates separation, necessitating specific stationary phases to enhance retention and selectivity. This study evaluates these columns' efficacy in complex matrices like chicken eggs and other food samples. Chromatographic separation was performed using a UPLC system coupled with a Q-TOF mass spectrometer; extraction and purification involved freeze-out, centrifugation, and filtration steps. The study highlights the critical role of column selection in achieving accurate and reliable separation and quantification of highly polar analytes in matrices of animal origin, offering in the meantime an easy-to-apply methodology of selection for the right determination of the best chromatographic column for different purposes.
液相色谱-质谱联用技术中极性农药的检测和定量分析面临重大挑战。本研究采用基于评分的方法,比较了三种液相色谱柱(Hypercarb™、Raptor Polar X™和Anionic Polar Pesticide™)在分离和定量鸡蛋中11种极性农药方面的性能。分析物包括草甘膦及其代谢物,以及欧盟官方控制计划中包含的其他高极性农药,如乙烯利、草铵膦和 fosetyl铝。极性农药具有高极性和亲水性,采用传统反相方法时会导致分析问题,如保留性差和峰形异常。它们与疏水固定相的相互作用较弱,使分离变得复杂,因此需要特定的固定相来提高保留性和选择性。本研究评估了这些色谱柱在鸡蛋等复杂基质以及其他食品样品中的功效。使用超高效液相色谱系统与Q-TOF质谱仪进行色谱分离;提取和纯化包括冷冻、离心和过滤步骤。该研究强调了柱选择在动物源基质中实现高极性分析物准确可靠分离和定量方面的关键作用,同时提供了一种易于应用的选择方法,以便为不同目的正确确定最佳色谱柱。