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Simultaneous determination of thiacloprid and its five metabolites in vegetables and flowers using QuEChERS combined with HPLC-MS/MS

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journal contribution
posted on 2023-05-26, 05:20 authored by Shaodong Pan, Xianpeng Song, Dan Wang, Yajie Ma, Xiangliang Ren, Hongyan Hu, Yongpan Shan, Xiaoyan Ma, Junyu Luo, Changcai Wu, Yan Ma, Jinjie Cui

Neonicotinoids have recently been banned in the European Union due to concerns about their environmental safety. Thiacloprid is a neonicotinoid, and is frequently used in agricultural pest control. However, the lack of quantitative methods for assessing its multiple metabolites has made it difficult to perform a comprehensive safety assessment. Therefore, we established an analytical method for effectively determining thiacloprid and its five metabolites in vegetables and flowers using QuEChERS-HPLC-MS/MS. The samples were extracted with acidified acetonitrile (containing 0.5% acetic acid) and were cleaned with graphitised carbon black (GCB) and octadecylsilane (C18) before the residue analysis. This method provided linearity ranging from 2–2000 μg kg−1, and its linear regression coefficients exceeded 0.995. Limits of Quantitation (LOQs) are achieved at 2 μg kg−1, and Limits of Detection (LODs) ranged from 0.09–0.80 μg kg−1. The method was validated on seven matrices spiked at 2, 200, and 2000 μg kg−1. Average recoveries ranged from 77–119%, with an intra-day Relative Standard Deviation (RSDr) of 1.5–13.4% and an inter-day Relative Standard Deviation (RSDR) of 0.9–14.4%. This method was used on cucumbers sprayed with thiacloprid and 19 types of flower samples collected from the field, after which thiacloprid and several of its metabolites were detected.


The work was supported by the Agricultural Science and Technology Innovation Program of Chinese Academy of Agricultural Sciences China Agriculture Research System .