In this study, multi-residue analysis methods for 32 pyrethroids in fruit and vegetable samples were established in both GC–MS/MS and UHPLC-MS/MS. The parameters that affecting the ionization efficiencies of pyrethroids in UHPLC-ESI-MS/MS, including ion source temperature, in-source fragmentation, and mobile phase conditions were thoroughly investigated to guarantee better performance. These two techniques were comprehensively compared in terms of recovery, LOQ, linearity, and matrix effects. In general, UHPLC-MS/MS was found suitable for more pesticides than GC–MS/MS. Lower LOQs were obtained for most of the selected pyrethroids in UHPLC-MS/MS. Similar results were obtained in terms of recoveries and RSDs for the validated pesticides in fortification experiments. A total of 136 real samples were analyzed by both techniques, obtaining similar results. The results suggest that UHPLC-MS/MS offers a suitable alternative to GC–MS/MS in the routine analysis of pyrethroids in fruits and vegetables.

本研究在 GC-MS/MS 和 UHPLC-MS/MS 中建立了水果和蔬菜样品中 32 种拟除虫菊酯的多残留分析方法。对影响 UHPLC-ESI-MS/MS 中拟除虫菊酯电离效率的参数（包括离子源温度、源内碎裂和流动相条件）进行了彻底研究，以确保更好的性能。这两种技术在回收率、LOQ、线性和基质效应方面进行了全面比较。一般而言，发现 UHPLC-MS/MS 比 GC-MS/MS 适用于更多的农药。在 UHPLC-MS/MS 中，大多数选定的拟除虫菊酯获得了较低的 LOQ。在强化实验中验证的农药的回收率和 RSD 方面也获得了类似的结果。这两种技术共分析了 136 个真实样品，得到相似的结果。结果表明，在水果和蔬菜中拟除虫菊酯的常规分析中，UHPLC-MS/MS 可以替代 GC-MS/MS。