引用本文:刘彬,郭丽,邓方,陈冠焱,舒治冲.超高效液相色谱-三重四极杆质谱法测定地表水和地下水中11种三嗪类农药[J].环境监控与预警,2023,15(2):46-51
LIU Bin, GUO Li, DENG Fang, CHEN Guan-yan, SHU Zhi-chong.Determination of 11 Triazine Pesticides in Surface and Ground Water by UPLC-QQQ MSD[J].Environmental Monitoring and Forewarning,2023,15(2):46-51
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超高效液相色谱-三重四极杆质谱法测定地表水和地下水中11种三嗪类农药
刘彬,郭丽,邓方,陈冠焱,舒治冲1,2,3
1.湖北省生态环境监测中心站,湖北 武汉 430072;2.湖北省生态环境厅武汉生态环境监测中心,湖北 武汉 430024;3.湖北省生态环境厅宜昌生态环境监测中心,湖北 宜昌 443005
摘要:
建立了针对地表水和地下水中11种三嗪类农药的超高效液相色谱-三重四极杆质谱分析方法,并对前处理、仪器分析、方法特性指标等因素进行优化探讨。使用SB-C18色谱柱、乙腈-水二元混合液流动相进行化合物分离,设置柱温为40℃、进样量为10 μL,质谱采用正离子模式检测,内标法定量,采用平均相对响应因子法拟合标准曲线。结果表明,11种三嗪类农药的方法检出限为0.003~ 0.01μg/L,对3种质量浓度的基体加标样品分别进行6次平行分析,测定结果的相对标准偏差为2.1%~19%,平均加标回收率为80.0%~108%。采集地表水和地下水样品,经尼龙或聚四氟乙烯滤膜过滤后上机测定,在1种地表水样品中检出了阿特拉津和扑灭津,平均质量浓度分别为0.032 和0.009μg/L。该方法具有准确度高、重复性好、检出限低等优点,能够满足现阶段地表水和地下水的环境管理监测要求。
关键词:  三嗪类  农药  地表水  地下水  液相色谱-三重四极杆质谱
DOI:
分类号:O656;X832
基金项目:北省省级环保科研项目(2021 HB-ZC02);湖北地方标准制修订项目(T-Z-06-2021137)
Determination of 11 Triazine Pesticides in Surface and Ground Water by UPLC-QQQ MSD
LIU Bin, GUO Li, DENG Fang, CHEN Guan-yan, SHU Zhi-chong1,2,3
1. Hubei Ecological Environmental Monitoring Central Station, Wuhan,Hubei 430072, China;2.Wuhan Ecological Environmental Monitoring Center, Department of Ecology and Environment of Hubei Province, Wuhan,Hubei 430024, China;3. Yichang Ecological Environmental Monitoring Center, Department of Ecology and Environment of Hubei Province, Yichang,Hubei 443005, China
Abstract:
A method for determination of 11 triazine pesticides in surface and ground water by UPLC-QQQ MSD was developed, and the parameters of experimental conditions were optimized. SB C18 column and water acetonitrile mobile phase were used. The column temperature was set at 40 ℃, and the injection volume was 10 μL. The MS monitoring mode is MRM ESI+, then the data was analyzed by average RRF method. Under the optimized conditions, the detection limits of target compounds were 0.003~0.01 μg/L. The RSDs(n=6) of three concentration levels were 2.1%~19%, and the average recoveries ranged from 80.0% to 108%. Samples of surface and ground water were collected at random. After filtered by PTFE or Nylon membrane, the filtrate was transferred to UPLC QQQ MSD for detection. Atrazine and propazine were detected in a surface water, the concentrations are 0.032 and 0.009 μg/L respectively. The results showed that this method has the advantages of high accuracy, good repeatability and low detection limit, which is suitable for current environmental management needs.
Key words:  Triazine  Pesticide  Surface water  Ground water  UPLC-QQQ MSD