Determination of pendimethalin in water, sediment, and Procambarus clarkii by high performance liquid chromatography-triple quadrupole mass spectrometry

  • Qiuhong YangEmail author
  • Xiaohui AiEmail author
  • Siqi Li
  • Huan Liu
  • Yongtao Liu


We established a high-performance liquid chromatography-triple quadrupole mass spectrometry method for the analysis of pendimethalin residues in water, sediments, and Procambarus clarkii (Louisiana crayfish) tissues. Water samples were concentrated on a HLB solid-phase extraction column and eluted with dichloromethane and acetone (1:1). After drying under a stream of nitrogen gas, the sample volume was adjusted to 1 mL with the mobile phase solvent methanol/water/acetic acid (8:20:0.1). Pendimethalin was extracted with ethyl acetate containing 0.1% acetic acid, after rotary evaporation to dryness at 35 °C, the residue was dissolved in mobile phase solvent, purified by a neutral alumina column and graphitized carbon black powder (0.1 g). The mass characterization was conducted in positive ion mode, and the corresponding ions were detected in multi-reaction monitoring mode. The linear equations were y = 1 × 106x + 14275, at pendimethalin levels of 0.05–20 μg L−1 and y = 691029 × − 414368 for 20–200 μg L−1. The detection limits of pendimethalin in water, sediments, and P. clarkii tissues were 1.0 × 10−4μg L−1 , 5.0 × 10−3μg kg −1 and 5.0 × 10−3 μg kg −1, respectively. The spiked recoveries ranged from 81.6 to 106.3%, and the relative standard deviations ranged from 4.58 to 13.6% (n = 6). The method provided an efficient and low-cost extraction and purification procedure that enabled a sensitive determination of pendimethalin in water as well as complex matrices.


High performance liquid chromatography-triple quadrupole mass spectrometry Pendimethalin Water Sediment Rice-Procambarus clarkii–integrated planting 



The authors sincerely thank the individuals who helped during the research and especially Professor Geng Leng (School of Resources and Environment, University of Electronic Science and Technology of China) for his suggestions.

Conflict of interest

The authors declare that they have no conflict of interest.

Ethical approval

This article does not contain any studies with human subjects. All animal experiments in this study adhered to Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences guidelines and were approved by the Animal Ethics Committee.

Informed consent

Not applicable.

Funding information

This study was funded by the Central Public-interest Scientific Institution Basal Research Fund, the Chinese Academy of Fishery Sciences (Project Number 2018HY-ZD0606), and the Agro-Scientific Research in the Public Interest of China (Project Number 201503108-CC-1).

Compliance with ethical standards

All animal experiments in this study adhered to Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences guidelines and were approved by the Animal Ethics Committee.


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© Springer Nature Switzerland AG 2019

Authors and Affiliations

  1. 1.Yangtze River Fisheries Research InstituteChinese Academy of Fishery SciencesWuhanChina
  2. 2.Chinese Academy of Fishery Sciences, Key Laboratory of Control of Quality and Safety for Aquatic ProductsMinistry of AgricultureBeijingChina
  3. 3.College of FisheriesHuazhong Agricultural UniversityWuhanChina

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