Institute of Quality Standard and Testing Technology for Agro-products of Sichuan Academy of Agricultural Sciences, Chengdu 610066, China.
Laboratory of Quality and Safety Risk Assessment for Agro-products (Chengdu), Ministry of Agriculture, Chengdu, 610066, China.
Anal Methods. 2024 Sep 12;16(35):5990-5998. doi: 10.1039/d4ay00563e.
A general strategy for qualitative screening and quantitative analysis of 403 pesticides in various fruits and vegetables was developed using ultrahigh-performance liquid chromatography (UHPLC) in conjunction with a Thermo Q Exactive Focus high-resolution mass spectrometer, relying on an executable compound database comprised of the exacted mass of precursor ions, retention times, and fragment ions. Taking advantage of the powerful separation capacity of UHPLC, an Orbitrap analyzer with high sensitivity in full scan mode and elevated mass resolution of product ions in the MS/MS mode, eight pairs of isomers and fifty-seven groups of isobaric compounds were selectively identified. The method was then systematically assessed and validated for eight fruits and vegetables, in terms of screening detection limit (SDL), matrix effects, recovery, and precision over 400 pesticides. The results showed that the SDLs of 68.0-84.4% for the pesticides were less than or equal to 10 μg kg in the representative matrices, recoveries in the range of 60-120% accounting for 48.6-84.4% of all the targets at three lower fortified levels of 5, 20, and 50 μg kg with a precision of less than 20% while the range of overall average recoveries for the majority of the pesticides were from 82.4% to 105.1% in the as-selected matrices with RSDs between 3.9% and 7.7%. Using this method, screening data from a survey of pesticide residues in 68 practical samples across 32 different matrix types provides scientific data for the inspection and supervision of pesticide residue safety of fruits and vegetables.
建立了一种超高效液相色谱（UHPLC）结合 Thermo Q Exactive Focus 高分辨率质谱仪，利用可执行的化合物数据库（包括前体离子的精确质量、保留时间和碎片离子），对各种水果和蔬菜中的 403 种农药进行定性筛选和定量分析的通用策略。利用 UHPLC 的强大分离能力，在全扫描模式下具有高灵敏度的 Orbitrap 分析仪和在 MS/MS 模式下具有高分辨的产物离子，选择性地鉴定了 8 对异构体和 57 组同量异位体化合物。然后，系统地评估和验证了该方法在 8 种水果和蔬菜中的筛查检测限（SDL）、基质效应、回收率和精密度，共 400 多种农药。结果表明，68.0-84.4%的农药在代表性基质中的 SDL 小于或等于 10μgkg，回收率在 60-120%范围内，占所有目标物的 48.6-84.4%，在 5、20 和 50μgkg 三个较低加标水平下的精密度小于 20%，而大多数农药的总体平均回收率范围在 82.4%-105.1%之间，相对标准偏差（RSD）在 3.9%-7.7%之间。使用该方法，对 32 种不同基质类型的 68 个实际样品中农药残留的调查结果进行了筛选，为水果和蔬菜中农药残留安全的检验和监督提供了科学数据。
