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
{"title":"Development and validation of a combined QuEChERS and HPLC-MS/MS method for trace analysis of ten diamide insecticides in agricultural products†","authors":"Fajun Tian, Zhenzhen Zhou, Junfeng Lu, Chengkui Qiao, Caixia Wang, Tao Pang, Linlin Guo, Jun Li, Rongli Pang and Hanzhong Xie","doi":"10.1039/D4AY02117G","DOIUrl":null,"url":null,"abstract":"<p >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 (<em>R</em><small><sup>2</sup></small> &gt; 0.99) was obtained for all diamide insecticides within the concentration range of 5–1000 µg kg<small><sup>−1</sup></small>. The limit of detection (LOD) and limit of quantification (LOQ) were 0.01–1 µg kg<small><sup>−1</sup></small> and 5 µg kg<small><sup>−1</sup></small>, respectively. The recoveries of the ten diamide insecticides at three levels (5, 100, and 1000 µg kg<small><sup>−1</sup></small>) ranged from 76.6% to 108.2% with good intra-day relative standard deviation (RSD<small><sub>r</sub></small>) (1.0–13.4%) and inter-day relative standard deviation (RSD<small><sub>R</sub></small>) (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.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 10","pages":" 2282-2294"},"PeriodicalIF":2.7000,"publicationDate":"2025-02-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ay/d4ay02117g?page=search","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Analytical Methods","FirstCategoryId":"92","ListUrlMain":"https://pubs.rsc.org/en/content/articlelanding/2025/ay/d4ay02117g","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
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

求助全文
约1分钟内获得全文 求助全文
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
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术官方微信