Development and validation of a combined QuEChERS and HPLC-MS/MS method for trace analysis of ten diamide insecticides in agricultural products†

IF 2.7 3区 化学 Q2 CHEMISTRY, ANALYTICAL
Fajun Tian, Zhenzhen Zhou, Junfeng Lu, Chengkui Qiao, Caixia Wang, Tao Pang, Linlin Guo, Jun Li, Rongli Pang and Hanzhong Xie
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引用次数: 0

Abstract

Diamide insecticides are being widely registered worldwide, yet most of them lack established maximum residue limits (MRLs) in agricultural products. In this study, we combined a QuEChERS (quick, easy, cheap, efficient, rugged, and safe) extraction method with high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) analysis to simultaneously identify and quantify ten diamide insecticides in seven matrices for the first time. The method was validated in accordance with SANTE/11312/2021 guidelines, including sensitivity, linearity, trueness, and precision. Excellent linearity (R2 > 0.99) was obtained for all diamide insecticides within the concentration range of 5–1000 µg kg−1. The limit of detection (LOD) and limit of quantification (LOQ) were 0.01–1 µg kg−1 and 5 µg kg−1, respectively. The recoveries of the ten diamide insecticides at three levels (5, 100, and 1000 µg kg−1) ranged from 76.6% to 108.2% with good intra-day relative standard deviation (RSDr) (1.0–13.4%) and inter-day relative standard deviation (RSDR) (2.3–15.7%). The proposed method was applied to analyze 70 real agricultural product samples, and only six samples contained diamide insecticides. The results demonstrated that the method was both convenient and reliable for detecting diamide insecticides in agricultural products. The method was then applied to analyze agricultural product samples collected in a field trial to estimate the MRLs for the next step.

Abstract Image

QuEChERS - HPLC-MS/MS联合分析农产品中10种二胺类杀虫剂的方法建立及验证
二胺类杀虫剂在世界范围内广泛注册,但大多数杀虫剂在农产品中缺乏确定的最大残留限量。本研究首次将QuEChERS(快速、简便、廉价、高效、坚固、安全)提取方法与高效液相色谱-串联质谱(HPLC-MS/MS)分析相结合,对7种基质中的10种二胺类杀虫剂进行了同时鉴定和定量。该方法按照SANTE/11312/2021指南进行验证,包括灵敏度、线性度、真实度和精密度。在5 ~ 1000µg kg-1的浓度范围内,所有二胺类杀虫剂均具有良好的线性关系(R2 > 0.99)。检测限和定量限分别为0.01-1µg kg-1和5µg kg-1。10种二胺类杀虫剂在5、100、1000µg kg-1 3个水平上的回收率为76.6% ~ 108.2%,日内相对标准偏差(RSDr)为1.0 ~ 13.4%,日内相对标准偏差(RSDr)为2.3 ~ 15.7%。应用该方法对70份实际农产品样品进行了分析,结果显示含二胺类杀虫剂的样品只有6份。结果表明,该方法简便、可靠,可用于农产品中二胺类杀虫剂的检测。然后将该方法应用于田间试验中收集的农产品样品的分析,以估计下一步的MRLs。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
Analytical Methods
Analytical Methods CHEMISTRY, ANALYTICAL-FOOD SCIENCE & TECHNOLOGY
CiteScore
5.10
自引率
3.20%
发文量
569
审稿时长
1.8 months
期刊介绍: Early applied demonstrations of new analytical methods with clear societal impact
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