Granados-Povedano Mireya, Domínguez Irene, Egea-González Francisco, Garrido Frenich Antonia, Arrebola Francisco Javier
Department of Chemistry and Physics (Analytical Chemistry Area), Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), Agrifood Campus of International Excellence ceiA3, University of Almeria, E-04120 Almeria, Spain.
Foods. 2023 Feb 8;12(4):739. doi: 10.3390/foods12040739.
A new polyvalent wide-scope analytical method, valid for both raw and processed (juices) fruits, combining target and non-target strategies, has been developed and validated to determine low concentrations of 260 pesticides, as well as many potential non-target substances and metabolites. The target approach has been validated according to SANTE Guide requirements. Trueness, precision, linearity, and robustness values were validated in raw fruit (apple) and juice (apple juice) as representative solid and liquid food commodities. Recoveries were between 70-120% and two ranges of linearity were observed: 0.5-20 μg kg (0.5-20 μg L apple juice) and 20-100 μg kg (20-100 μg L apple juice). The limits of quantification (LOQs) reached were lower than 0.2 μg kg in apple (0.2 μg L apple juice) in most cases. The developed method, based on QuEChERS extraction followed by gas chromatography-high resolution mass spectrometry (GC-HRMS), achieves part-per-trillions lower limits, which allowed the detection of 18 pesticides in commercial samples. The non-target approach is based on a retrospective analysis of suspect compounds, which has been optimized to detect up to 25 additional compounds, increasing the scope of the method. This made it possible to confirm the presence of two pesticide metabolites which were not considered in the target screening, phtamlimide and tetrahydrophthalimide.
一种新的多价广谱分析方法已被开发并验证，该方法适用于生果和加工（果汁）水果，结合了靶向和非靶向策略，用于测定260种农药的低浓度，以及许多潜在的非靶向物质和代谢物。靶向方法已根据SANTE指南要求进行验证。在作为代表性固体和液体食品商品的生果（苹果）和果汁（苹果汁）中验证了准确性、精密度、线性和稳健性值。回收率在70%-120%之间，观察到两个线性范围：0.5-20μg/kg（0.5-20μg/L苹果汁）和20-100μg/kg（20-100μg/L苹果汁）。在大多数情况下，苹果（苹果汁）中的定量限（LOQ）低于0.2μg/kg（0.2μg/L苹果汁）。所开发的方法基于QuEChERS萃取，随后进行气相色谱-高分辨率质谱（GC-HRMS），实现了万亿分之一的下限，这使得能够检测商业样品中的18种农药。非靶向方法基于对可疑化合物的回顾性分析，该分析已进行优化，以检测多达25种额外的化合物，扩大了该方法的范围。这使得能够确认两种在靶向筛查中未考虑的农药代谢物邻苯二甲酰亚胺和四氢邻苯二甲酰亚胺的存在。
