Canadian Food Inspection Agency, Calgary Laboratory, 3650-36th Street N.W, Calgary, AB T2L 2L1, Canada.
US Food and Drug Administration, Center for Food Safety and Applied Nutrition, 5001 Campus Drive, College Park, MD 20740, USA.
J AOAC Int. 2020 Nov 1;103(6):1547-1559. doi: 10.1093/jaoacint/qsaa065.
Effective and expansive methods for multiresidue pesticide analysis are desired for routine monitoring programs. These methods are complex, especially when several hundred pesticides are involved.
Two approaches to sort data and identify isomers and isobaric ions in pesticide mixtures were evaluated to determine whether they could be differentiated by mass resolving power and/or chromatographic resolution.
This study presents an application of ultra-high performance liquid chromatography electrospray Q-Orbitrap mass spectrometry (UHPLC/ESI Q-Orbitrap) along with QuEChERS for the quantitation of 655 pesticide residues in fruits and vegetables.
From the developed method, 94.7% of the 655 pesticides in fruits and 93.9% of those in vegetables had recoveries between 81% and 110%; 98.3% in both fruits and vegetables had an intermediate precision of ≤20%; and 97.7% in fruits or 97.4% in vegetables showed measurement uncertainty of ≤50%. When the retention time difference (ΔtR) of two isomers was ≥0.12 min, they were chromatographically resolved. Twenty five out of 35 pairs or groups of isomers were chromatographically separated (ΔtR ≥ 0.12 min), but 14 pairs were not resolved (ΔtR < 0.12 min). There were 493 pairs of pesticides with a mass-to-charge difference of <1 Da. Only one pair of isobaric ions could not be separated by mass and chromatographic resolution.
UHPLC/ESI Q-Orbitrap along with QuEChERS sample preparation offers a practical quantitative companion method to a non-target data acquisition for target analysis workflow for pesticide residue analysis in routine monitoring programs for food safety.
对于常规监测计划，需要有效且广泛的多残留农药分析方法。这些方法很复杂，尤其是涉及数百种农药时更是如此。
评估了两种用于对农药混合物中的异构体和同量异位离子进行分类和识别的数据处理方法，以确定它们是否可以通过质量分辨率和/或色谱分辨率来区分。
本研究应用超高效液相色谱电喷雾 Q-Orbitrap 质谱（UHPLC/ESI Q-Orbitrap）和 QuEChERS 对水果和蔬菜中的 655 种农药残留进行定量分析。
在所开发的方法中，94.7%的水果中 655 种农药和 93.9%的蔬菜中 655 种农药的回收率在 81%至 110%之间；水果和蔬菜的中间精密度均≤20%；97.7%的水果或 97.4%的蔬菜的测量不确定度≤50%。当两种异构体的保留时间差（ΔtR）≥0.12min 时，它们在色谱上得到分离。35 对或组异构体中有 25 对（ΔtR≥0.12min）在色谱上得到分离，但有 14 对没有得到分离（ΔtR<0.12min）。有 493 对质量电荷比差值<1Da 的农药。只有一对同量异位离子不能通过质量和色谱分辨率分离。
UHPLC/ESI Q-Orbitrap 结合 QuEChERS 样品制备为农药残留分析的常规监测计划中的目标分析工作流程提供了一种实用的定量伴随方法，用于非靶向数据采集。
