Journal of Analysis and Testing

, Volume 2, Issue 4, pp 322–331 | Cite as

Determination of Triazine Herbicides in Environmental Water Samples by Acetonitrile Inorganic Salt Aqueous Two-Phase Microextraction System

  • Shiqian GaoEmail author
  • Gege Wu
  • Xiaomeng Li
  • Jie Chen
  • Youyi Wu
  • Junxia Wang
  • Zhanen ZhangEmail author
Original Paper


Acetonitrile inorganic salt aqueous two-phase extraction method was established for the determination of triazine herbicides (simeton, cyanazine, desmetryn, terbumeton, terbuthylazine and dimethametryn) in environmental water samples by high-performance liquid chromatography (HPLC). The extraction solvents types and volume of acetonitrile, the inorganic salt types and amount of (NH4)2SO4, extraction time and pH of sample solution were optimized by single-factor experiment and central composite design. Under the optimum extraction conditions, all linear ranges were obtained with coefficients of determination (r) ≥ 0.9993. The limits of detection for this proposed method were in the range of 0.16–0.28 μg/L for six triazine herbicides. The developed method has been successfully applied to the analysis of target triazine herbicides from lake, canal and moat in real-world water samples. The recoveries of target analytes were in the range from 87.0 to 110.9% and the relative standard deviation was lower than 7.3%.


Acetonitrile inorganic salt Aqueous two-phase microextraction Triazine herbicides Environmental water samples High-performance liquid chromatography 



This work was supported by the major project of Natural Science Foundation of Jiangsu Higher Education Institutions of China (no: 15KJA610003), Natural Science Foundation of Jiangsu Province (no. BK20160359) and Natural Science and Technology Program on Water Pollution Control and Treatment (2017ZX07205-2). The authors also acknowledge support from the Preponderant Discipline Construction Project in higher education of Jiangsu Province, China and Jiangsu High Education Collaborative Innovation Center of Water Treatment Technology and Material.

Supplementary material

41664_2018_73_MOESM1_ESM.docx (2.3 mb)
Supplementary material 1 (DOCX 2341 kb)


  1. 1.
    Su Q, Liu B, Hong J, Li AM, He XM, Guo LWH. Determination of 11 triazine herbicides in soil by accelerated solvent extraction high performance liquid chromatography. Environ Chem. 2017;36(3):628–34.Google Scholar
  2. 2.
    Chen S, Huang W. Analysis of triazine herbicides using an up-and-down-shaker-assisted dispersive liquid–liquid microextraction coupled with gas chromatography-mass pectrometry. J Chromatogr B Anal Technol Biomed Life Sci. 2014;955:116–23.CrossRefGoogle Scholar
  3. 3.
    Megersa N, Chimuka L, Solomon Y, Jönsson JÅ. Automated liquid membrane extraction and trace enrichment of triazine herbicides and their metabolites in environmental and biological samples. J Sep Sci. 2015;24(7):567–76.CrossRefGoogle Scholar
  4. 4.
    Liu TT, Cao P, Geng JP, Li JQ, Wang MZ, Wang LM, Li XY, Yin DL. Determination of triazine herbicides in milk by cloud point extraction and high-performance liquid chromatography. Food Chem. 2014;142:358–64.CrossRefGoogle Scholar
  5. 5.
    Wu Q, Feng C, Zhao G, Wang C, Wang Z. Graphene-coated fiber for solid-phase microextraction of triazine herbicides in water samples. J Sep Sci. 2015;35(2):193–9.CrossRefGoogle Scholar
  6. 6.
    Wang X, Liu Q, Yang Y. Determination of 31 triazine herbicides in farmland soils by high performance liquid chromatography-tandem mass spectrometry. Chin J Anal. 2014;42(3):390–6.Google Scholar
  7. 7.
    US EPA. The drinking water standards and health advisories tables [S]. Washington, DC: EPA; 2018.Google Scholar
  8. 8.
    EU. Council directive 98/83/EC on the quality of water intended for human consumption [S]. Brussels: EC; 1998.Google Scholar
  9. 9.
    Fenoll J, Hellín P, Flores P, Martínez CM, Navarro S. Degradation intermediates and reaction pathway of carbofuran in leaching water using TiO2 and ZnO as photocatalyst under natural sunlight. J Photochem Photobiol A. 2013;251(9):33–40.CrossRefGoogle Scholar
  10. 10.
    The Ministry of Health and Standardization Administration of the People's Republic of China. Standards for drinking water quality (GB 5749-2006). Beijing: China Environmental Science Press; 2007.Google Scholar
  11. 11.
    Li P, Yang X, Miao H, Zhao YF, Liu W, Wu YN. Simultaneous determination of 19 triazine pesticides and degradation products in processed cereal samples from Chinese total diet study by isotope dilution–high performance liquid chromatography–linear ion trap mass spectrometry. Anal Chim Acta. 2013;781:63–71.CrossRefGoogle Scholar
  12. 12.
    Rivoira L, De Carlo RM, Cavalli S, Bruzzoniti MC. Simple SPE-HPLC determination of some common drugs and herbicides of environmental concern by pulsed amperometry. Talanta. 2015;131(131):205–12.CrossRefGoogle Scholar
  13. 13.
    Mirzajani R, Ramezani Z, Kardani F. Selective determination of thidiazuron herbicide in fruit and vegetable samples using molecularly imprinted polymer fiber solid phase microextraction with ion mobility spectrometry detection (MIPF-SPME-IMS). Microchem J. 2017;130:93–101.CrossRefGoogle Scholar
  14. 14.
    Zhang LY, Yao D, Li N, Zhang HQ, Yu AM. Ionic liquid homogeneous liquid-liquid microextraction-determination of five triazine herbicides in infant formula by high performance liquid chromatography. Chromatography. 2015;33(7):53–758.Google Scholar
  15. 15.
    Conrad A, Schröter-Kermania C, Hoppe HW, Maria Rüther, Pieper S. Kolossa-Gehring M. Glyphosate in German adults-Time trend (2001 to 2015) of human exposure to a widely used herbicide. Int J Hyg Environ Health. 2016;220(1):8–16.CrossRefGoogle Scholar
  16. 16.
    Dong SY, Huang GQ, Hu Q, Li S, Yao YH, Huang TL. Evaluation of IL-ATPS and IL-MAE for simultaneous determination of herbicides and plant growth regulators in sediment. Chromatographia. 2014;77(13–14):923–31.CrossRefGoogle Scholar
  17. 17.
    Guo Y, Li X, Gao S, Gu HD, Zhang ZE. Magnetic resonance graphene solid Phase extraction/high performance liquid chromatography–tandem mass spectrometry for the determination of 6 triazine herbicides in environmental water samples. Instrum Anal. 2016;35(11):1384–9.Google Scholar
  18. 18.
    Hu J, Li YY, Zhang W, Wang HL, Huang CJ, Zhang MH, Wang XD. Dispersive liquid–liquid microextraction followed by gas chromatography-electron capture detection for determination of polychlorinated biphenyls in fish. J Sep Sci. 2015;32(12):2103–8.CrossRefGoogle Scholar
  19. 19.
    Cardoso GDB, Souza IN, Mouro T, Freire MG, Soares CMF, Lima ÁS. Novel aqueous two-phase systems composed of acetonitrile and polyols: phase diagrams and extractive performance. Sep Purif Technol. 2014;124:54–60.CrossRefGoogle Scholar
  20. 20.
    Kwon YJ, Kaul R, Mattiasson B. Extractive lactic acid fermentation in poly (ethyleneimine)-based aqueous two-phase system. Biotechnol Bioeng. 2015;50(3):280–90.CrossRefGoogle Scholar
  21. 21.
    Wang Y, Zhang D, Wang Y, Liang X, Xu BZ. Optimization of extraction process of yeast metallothionein by aqueous two-Phase system. Food Sci. 2015;18(1):193–201.Google Scholar
  22. 22.
    Chen X, Zhao Y, Liu H. Determination of atrazine and 6 acetamide herbicides residues in corn by gas chromatography. Cereal Feed Ind. 2015;12(2):61–3.Google Scholar
  23. 23.
    Farajzadeh MA, Jozan D, Afshar MR, Mogaddam Norouzi J. Determination of phthalate esters in cow milk samples using dispersive liquid-liquid microextraction coupled with gas chromatography followed by flame ionization and mass spectrometric detection. J Sep Sci. 2015;35(5–6):742–9.Google Scholar
  24. 24.
    Hayriye MA, Taskın M, Kamil B, Serap SB, Melek MT. Ultrasound-assisted surfactant/ionic liquid aqueous two-phase system extraction prior to high performance liquid chromatography for the determination of tetracyclines in milk and honey samples. Turk J Chem. 2017;41:955–66.CrossRefGoogle Scholar
  25. 25.
    Wang K, Jiang J, Kang MQ, Li D, Zang S, Tian SZ, Zhang HQ, Yu AM, Zhang ZW. Magnetical hollow fiber bar collection of extract in homogenous ionic liquid microextraction of triazine herbicides in water samples. Anal Bioanal Chem. 2017;409(10):2569–79.CrossRefGoogle Scholar
  26. 26.
    Megersa N. Hollow fiber-liquid phase microextraction for trace enrichment of the residues of at razine and its major degradation products from environmental water and human urine samples. Anal Methods. 2015;7:9940–8.CrossRefGoogle Scholar

Copyright information

© The Nonferrous Metals Society of China 2018

Authors and Affiliations

  1. 1.School of Environmental Science and EngineeringSuzhou University of Science and TechnologySuzhouPeople’s Republic of China
  2. 2.Jiangsu Key Laboratory of Environmental Science and EngineeringSuzhou University of Science and TechnologySuzhouPeople’s Republic of China
  3. 3.National and Local Joint Engineering Laboratory of Municipal Sewage Resource Utilization TechnologySuzhouPeople’s Republic of China

Personalised recommendations