农药2024,Vol.63Issue(4) :268-273.DOI:10.16820/j.nyzz.2024.0406

超高效液相色谱-串联质谱法测定稻田水体中8种常用稻田除草剂的残留

Simultaneous determination of residues of 8 frenquently-used herbicide in rice field water by UPLC-MS/MS

石莹 徐漫 康艺瑾 闫新利 朱椿元 王赛尔 王玲玲
农药2024,Vol.63Issue(4) :268-273.DOI:10.16820/j.nyzz.2024.0406

超高效液相色谱-串联质谱法测定稻田水体中8种常用稻田除草剂的残留

Simultaneous determination of residues of 8 frenquently-used herbicide in rice field water by UPLC-MS/MS

石莹 1徐漫 1康艺瑾 1闫新利 1朱椿元 1王赛尔 1王玲玲1
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作者信息

  • 1. 生态环境部南京环境科学研究所国家环境保护农药环境评价与污染控制重点实验室,南京 210042
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摘要

[目的]基于固相萃取技术,结合超高效液相色谱串联质谱(UPLC-MS/MS)法建立了稻田水中8种常用稻田除草剂(苯噻酰草胺、丙草胺、丁草胺、二氯喹啉酸、苄嘧磺隆、吡嘧磺隆、五氟磺草胺、二甲戊灵)残留的检测方法.[方法]稻田水样品经滤纸过滤,经过C18固相萃取小柱富集浓缩后,以0.1%甲酸水-乙腈为流动相进行梯度洗脱,采用UPLC-MS/MS测定,基质外标法定量.[结果]8种除草剂在所建立的方法下线性关系良好,相关系数(r)大于0.99,方法检出限(LOD)为0.0012~0.025 μg/L.在稻田水基质平均加标回收率为80.33%~90.10%,相对标准偏差(RSD)为2.66%~8.21%,该方法适用于稻田水体中8种除草剂的残留量测定.[结论]该方法条件下8种除草剂均表现为基质增强效应,在实际检测稻田水体残留时采用固相萃取技术进行实际样品净化浓缩处理,前处理步骤简单,灵敏可靠,适用于稻田水体中常用稻田除草剂的快速残留检测.

Abstract

[Aims]Based on solid-phase extraction(SPE)technique combined with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),determination method of 8 frenquently-used rice field herbicides(mefenacet,pretilachlor,butachlor,quinclorac,bensulfuron-methyl,pyrazosulfuron-ethyl,penoxsulam and pendimethalin)in paddy water were established.[Methods]The paddy water samples were filtered through filter paper,enriched and concentrated by a C18 solid phase extraction cartridge,and then subjected to gradient elution with 0.1%formic acid water-acetonitrile as the mobile phase,determined by UPLC-MS/MS and quantified by matrix external standard method.[Results]The linearity of the method was good with the correlation coefficients(r)greater than 0.99.The limits of detection(LODs)of the method were in the range of 0.0012-0.025 pg/L.The average spiked recoveries were in the range of 80.33%-90.10%in paddy water matrix with the relative standard deviations(RSDs)in the range of 2.66%-8.21%,which made the method suitable for the determination of the eight herbicide residues in rice water.[Conclusions]All the eight herbicides showed matrix-enhanced effects under the conditions of the method,and the solid phase extraction(SPE)technique was used for clean-up and concentration treatment during the actual residue detection in paddy water.The method with simple pre-processing step,is sensitive,reliable,and suitable for the rapid residue detection of frenquently-used paddy herbicides in paddy water.

关键词

稻田水/超高效液相色谱-串联质谱/除草剂/残留分析

Key words

paddy water/UPLC-MS/MS/herbicide/residue analysis

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基金项目

国家市场监督管理总局科技项目(2020MK114)

出版年

2024
农药
沈阳化工研究院有限公司

农药

CSTPCD北大核心
影响因子:0.665
ISSN:1006-0413
参考文献量21
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