海水中酰胺类除草剂及其代谢物的测定
作者:
作者单位:

1.山东省海洋资源与环境研究院,山东省海洋生态修复重点实验室,烟台市海珍品质量安全控制与精深 加工重点实验室 山东 烟台 264006 ;2.东营市垦利区市场监管管理局 山东 东营 257500

作者简介:

丁玉竹(1990—),工程师,研究方向为海洋环境监测,E-mail:714717084@qq.com

基金项目:

山东省现代农业产业技术体系(SDAIT-26-05;SDAIT-14-08);山东省自然科学基金面上项目(ZR2023MD121);烟台市科技计划项目(2023YD089)


Determination of amide herbicides and metabolites in seawater
Author:
Affiliation:

1.Shandong Marine Resource and Environment Research Institute, Shandong Key Laboratory of Marine Ecological Restoration, Yantai Key Laboratory of Quality and Safety Control and Deep Processing of Marine Food, Yantai 264006 , China ; 2.The Market Supervision and Administration Bureau of Kenli District, Dongying 225750 0, China

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    摘要:

    采用气相色谱-质谱法测定海水中酰胺类除草剂及其代谢物。海水样品过滤后使用自动固相萃取仪过HLB柱富集、净化后用3 mL正己烷溶液洗脱,采用气相色谱质谱仪选择离子监测模式(SIM)对洗脱液进行检测,利用外标法对目标物定量。该方法中2-甲基-6-乙基苯胺(MEA)、2,6-二乙基苯胺(DEA)、异丙甲草胺的检出限均为6.0 ng/L,定量限均为15 ng/L;甲草胺、乙草胺、丙草胺、丁草胺的检出限均为12 ng/L,定量限均为30 ng/L。MEA、DEA、异丙甲草胺的线性范围为1.0~25.0 μg/L,甲草胺、乙草胺、丙草胺、丁草胺的线性范围为2.0~50.0 μg/L,方法相对标准偏差为5.3%~9.5%,加标回收率为68.7%~103.0%。该方法分析速度快、灵敏度高,满足药物残留检测的要求,可用于海水中酰胺类除草剂及其代谢物的检测。

    Abstract:

    A method was established for the determination of amide herbicides and their metabolites in seawater by gas chromatography-mass spectrometry (GC-MS). After filtration, the samples were passed through the HLB columns by automatic solid phase extraction, enriched and purified, then eluted with 3 mL n-hexane solution. Ion monitoring mode (SIM) was selected by gas chromatography-mass spectrometry to detect the eluent, and external standard method was used to quantify the target substance. The experimental results showed that good linearities for monoethanolamine (MEA), 2,6-Diethylaniline (DEA), and metolachlor existed in the range of 1.0-25.0 μg/L with their detection limit and quantization limit were 6.0 ng/L and 12 ng/L. Alachlor, acetochlor, pretilachlor, butachlor have good linearities in the range of 2.0-50.0 μg/L with their detection limit and quantization limit were 12 ng/L and 30 ng/L. The relative standard deviations were between 5.3%-9.5%, and the recoveries were 68.7%-103.0%. The method is rapid, sensitive and can be used for the determination of amide herbicides and their metabolites in seawater.

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丁玉竹,孙琰晴,刘小静,等.海水中酰胺类除草剂及其代谢物的测定[J].中国渔业质量与标准,2024,14(5):1-6. DING Yuzhu, SUN Yanqing, LIU Xiaojing, et al. Determination of amide herbicides and metabolites in seawater[J]. Chinese Fishery Quality and Standards,2024,14(5):1-6.

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  • 收稿日期:2024-01-31
  • 录用日期:2024-09-18
  • 在线发布日期: 2025-02-21