Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

IF 1.7 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL
Keisuke Nakamura, Takamitsu Otake, Nobuyasu Hanari
{"title":"Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Keisuke Nakamura,&nbsp;Takamitsu Otake,&nbsp;Nobuyasu Hanari","doi":"10.1093/jaoacint/qsad080","DOIUrl":null,"url":null,"abstract":"<p><strong>Background: </strong>Supercritical fluid extraction (SFE) is a fast, versatile, and solvent-efficient automatic extraction method. Despite its advantages, the results of our proficiency tests imply that the applicability assessments of SFE for pesticide residues were insufficient.</p><p><strong>Objective: </strong>In this study, as analytical method using SFE was optimized and validated by testing the incurred and fortified brown rice samples with organophosphorus (OP), pyrethroid (PYR), and dithiolane (DIT) pesticides.</p><p><strong>Method: </strong>A validation study using the incurred sample with etofenprox, fenitrothion, and isoprothiolane was performed by comparing the analytical results obtained using the SFE and solid-liquid extraction with homogenization (SLE), which is a well-validated official multi-residue extraction method. The tests on the fortified samples were also performed for seven pesticide residues, chlorpyrifos, diazinon, O-ethyl O-4-nitrophenyl phenylphosphonothioate (EPN), etofenprox, fenitrothion, isoxathion, and isoprothiolane, at three fortification levels, 0.001, 0.01, and 0.1 mg/kg.</p><p><strong>Results: </strong>In the test on the incurred samples, optimized SFE-to-SLE analytical values (CSFE/CSLE) were 99.2-100.1%, with RSD lower than 3%. In contrast, the analytical-to-spiked concentrations in the tests on the fortified samples were 96.4-105.0%, with RSD lower than 8.8%.</p><p><strong>Conclusions: </strong>These results indicate that the proposed SFE method, which is well validated with the incurred brown rice sample, is useful for determining OP, PYR, and DIT pesticide residues in brown rice.</p><p><strong>Highlights: </strong>The proposed SFE method satisfies EU and Japanese maximum residue limits (MRLs). The consumption of solvent can be reduced to one-fourth of that of SLE using the proposed SFE method.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.7000,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of AOAC International","FirstCategoryId":"97","ListUrlMain":"https://doi.org/10.1093/jaoacint/qsad080","RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0

Abstract

Background: Supercritical fluid extraction (SFE) is a fast, versatile, and solvent-efficient automatic extraction method. Despite its advantages, the results of our proficiency tests imply that the applicability assessments of SFE for pesticide residues were insufficient.

Objective: In this study, as analytical method using SFE was optimized and validated by testing the incurred and fortified brown rice samples with organophosphorus (OP), pyrethroid (PYR), and dithiolane (DIT) pesticides.

Method: A validation study using the incurred sample with etofenprox, fenitrothion, and isoprothiolane was performed by comparing the analytical results obtained using the SFE and solid-liquid extraction with homogenization (SLE), which is a well-validated official multi-residue extraction method. The tests on the fortified samples were also performed for seven pesticide residues, chlorpyrifos, diazinon, O-ethyl O-4-nitrophenyl phenylphosphonothioate (EPN), etofenprox, fenitrothion, isoxathion, and isoprothiolane, at three fortification levels, 0.001, 0.01, and 0.1 mg/kg.

Results: In the test on the incurred samples, optimized SFE-to-SLE analytical values (CSFE/CSLE) were 99.2-100.1%, with RSD lower than 3%. In contrast, the analytical-to-spiked concentrations in the tests on the fortified samples were 96.4-105.0%, with RSD lower than 8.8%.

Conclusions: These results indicate that the proposed SFE method, which is well validated with the incurred brown rice sample, is useful for determining OP, PYR, and DIT pesticide residues in brown rice.

Highlights: The proposed SFE method satisfies EU and Japanese maximum residue limits (MRLs). The consumption of solvent can be reduced to one-fourth of that of SLE using the proposed SFE method.

超临界萃取-液相色谱-串联质谱法定量测定糙米中有机磷、拟除虫菊酯和二硫代烷农药残留。
背景:超临界流体萃取是一种快速、通用、溶剂高效的自动萃取方法。尽管SFE具有优势,但我们的能力测试结果表明,SFE对农药残留的适用性评估不足。目的:本研究通过对含有有机磷(OP)、拟除虫菊酯类(PYR)和二硫杂环戊烯(DIT)农药的糙米样品进行检测,优化并验证了SFE的分析方法。方法:通过比较SFE和固液提取均化法(SLE)获得的分析结果,使用埃托芬prox、杀硝基苯和异硫平产生的样品进行验证研究,这是一种经过充分验证的官方多残留提取方法。在三个强化水平(0.001、0.01和0.1)下,还对强化样品进行了7种农药残留的测试,即毒死蜱、二嗪农、O-乙基-4-硝基苯基硫代膦酸酯(EPN mg/kg。结果:在对所产生样品的测试中,SFE对SLE的最佳分析值(CSFE/CSLE)为99.2-100.1%,RSD低于3%。与此相反,强化样品的分析加标浓度为96.4-105.0%,RSD低于8.8%。结论:该方法可用于糙米中OP、PYR和DIT农药残留的测定。亮点:拟议的SFE方法符合欧盟和日本的最大残留限量。使用所提出的SFE方法,溶剂的消耗可以减少到SLE的四分之一。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
求助全文
约1分钟内获得全文 求助全文
来源期刊
Journal of AOAC International
Journal of AOAC International 医学-分析化学
CiteScore
3.10
自引率
12.50%
发文量
144
审稿时长
2.7 months
期刊介绍: The Journal of AOAC INTERNATIONAL publishes the latest in basic and applied research in analytical sciences related to foods, drugs, agriculture, the environment, and more. The Journal is the method researchers'' forum for exchanging information and keeping informed of new technology and techniques pertinent to regulatory agencies and regulated industries.
×
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