色谱

色谱 ›› 2020, Vol. 38 ›› Issue (7): 826-832.DOI: 10.3724/SP.J.1123.2019.12022

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法检测环境水体中18种农药残留

杨松1, 邹楠1, 高云2, 许乐园2, 张文文2, 潘灿平3, 慕卫1,2,*()   

  1. 1 山东农业大学植物保护学院农药毒理与应用技术省级重点实验室, 山东 泰安 271018
    2 山东农业大学农药环境毒理研究中心, 山东 泰安 271018
    3 中国农业大学理学院应用化学系, 北京 100193
  • 收稿日期:2019-12-22 出版日期:2020-07-08 发布日期:2020-12-10
  • 通讯作者: 慕卫
  • 作者简介:慕卫.E-mail:muwei@sdau.edu.cn
  • 基金资助:
    山东省自然科学基金(ZR2018BC038);科技部重点研发计划项目(2016YFD0200206)

Determination of 18 pesticide residues in environmental water by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

YANG Song1, ZOU Nan1, GAO Yun2, XU Leyuan2, ZHANG Wenwen2, PAN Canping3, MU Wei1,2,*()   

  1. 1 Key Laboratory of Pesticide Toxicology&Application Technique, College of Plant Protection, Shandong Agricultural University, Tai'an 271018, China
    2 Research Center of Pesticide Environmental Toxicology, Shandong Agricultural University, Tai'an 271018, China
    3 Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China
  • Received:2019-12-22 Online:2020-07-08 Published:2020-12-10
  • Contact: MU Wei
  • Supported by:
    handong Provincial Natural Science Foundation, China(ZR2018BC038);the Key Research and Development Project of the Ministry of Science and Technology(2016YFD0200206)

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摘要：

建立了固相萃取-超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）同时检测环境水体中不同极性范围的18种农药残留的分析方法。样品经大体积固相萃取装置，以2 mL/min的速率通过Cleanrt®-PEP固相萃取柱进行净化和富集，浓缩50倍后结合UPLC-MS/MS检测，外标法定量。研究表明，目标化合物在0.5~50 μg/L范围内线性关系良好，线性相关系数（R2）≥0.995；在10、100和1000 ng/L 3个添加水下，18种农药在3种不同环境水体中的平均回收率为71.3%~105.9%，相对标准偏差（RSD，n=5）为1.3%~9.9%；定量限（LOQ）均为10 ng/L。该方法应用于泰安市区周围水环境的检测，各采集位点均未检出农药残留。该方法具有净化效果好、通用性强、灵敏度高、准确度高和操作简单等优点，适用于环境水体中18种农药的残留检测。

关键词: 超高效液相色谱-串联质谱, 固相萃取, 农药, 环境水体

Abstract:

A method was developed for the simultaneous determination of 18 pesticide residues in environmental water by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The samples were purified and enriched by a large-volume SPE apparatus through a Cleanrt®-PEP SPE column at a rate of 2 mL/min. After being concentrated 50-fold, the samples were detected by UPLC-MS/MS and quantified by the external standard method. The target compounds showed good linearity in the range of 0.5-50 μg/L, with linear correlation coefficients (R2) ≥0.995. At spiked levels of 10, 100 and 1000 ng/L, the average recoveries of the 18 pesticides in the three different environmental water samples were 71.3%-105.9%, and the relative standard deviations (RSDs, n=5) were 1.3%-9.9%. LOQs of the 18 pesticides were 10 ng/L. The method was applied to the detection of the water environment around Tai'an City, and no pesticide residues were detected at any of the collection sites. The method has the advantages of good purification effect, high versatility, sensitivity, and accuracy, and operational simplicity. The method is suitable for the determination of the 18 pesticides in environmental water.

Key words: ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS), solid phase extraction (SPE), pesticide, environmental water