Springer Nature is making SARS-CoV-2 and COVID-19 research free. View research | View latest news | Sign up for updates

Development of a dispersive liquid-liquid microextraction coupled with magnetic dispersive microsolid phase extraction for determination of triazines in wastewater samples

  • 79 Accesses


The combination of two microextraction techniques (dispersive liquid-liquid microextraction [DLLME] and magnetic dispersive microsolid phase extraction [MDMSPE]) was developed and reported for atrazine and simazine preconcentration from wastewater samples. The proposal methodology involved the use of magnetite supports functionalized with different alkyl or phenyl groups. The magnetic adsorbents were synthesized by the solvothermal method assisted by microwave, characterized, and used in the sample preconcentration of atrazine and simazine. The method validation included parameters such as the wastewater matrix effect, repeatability, and recovery. The analyte separation and quantification were performed by high-performance liquid chromatography with ultraviolet detection (HPLC-DAD). Parameters, such as the polarity and mass of magnetic solids and pH, were evaluated to provide better extraction performance. The highest recoveries (> 95%) were obtained with 50 mg of the phenyl group support (CS2) at pH 5, using 5 mL of the sample and carbon tetrachloride and methanol, as extraction and dispersive solvents, respectively. The lowest limits of detection (LOD) achieved were 13.16 and 13.86 ng L−1, and the limits of quantification (LOQ) were 43.89 and 46.19 ng L−1 for simazine and atrazine, respectively, with repeatability (expressed as %RSD) below 5% in all cases. The developed method is simple, easy, and low cost for the analysis of two herbicides potentially dangerous for environmental and human health.

Graphical abstract

This is a preview of subscription content, log in to check access.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6


  1. 1.

    Environmental Protection Agency. Decision documents for atrazine. Office of the Federal Register. Washington: National Archives and Records Administration; 2006.

  2. 2.

    Jablonowski ND, Schäffer A, Burauel P. Still present after all these years: persistence plus potential toxicity raise questions about the use of atrazine. Environ Sci Pollut Res. 2011;18:328–31.

  3. 3.

    Rodríguez JA, Aguilar-Arteaga K, Díez C, Barrado E. Recent advances in the extraction of triazines from water samples. In: Price A, Kenton J, editors. Herbicides advances in research. London: IntechOpen; 2013. p. 255–76.

  4. 4.

    Salazar-Ledesma M, Prado B, Zamora O, Siebe C. Mobility of atrazine in soils of a wastewater irrigated maize field. Agric Ecosyst Environ. 2018;255:73–83.

  5. 5.

    Prado B, Fuentes M, Verhulst N, Govaerts B, De León F, Zamora O. Fate of atrazine in a soil under different agronomic management practices. J Environ Sci Health B. 2014;49:844–55.

  6. 6.

    Hayes TB, Anderson LL, Beasley VR, de Solla SR, Iguchi T, Ingraham H, et al. Demasculinization and feminization of male gonads by atrazine: consistent effects across vertebrate classes. J Steroid Biochem Mol Biol. 2011;127:64–73.

  7. 7.

    Environmental Protection Agency. Federal Register, 74. Washington, 2009: Office of the Federal Register, National Archives and Records Administration.

  8. 8.

    United States Environmental Protection Agency. National primary drinking water regulations complete table. Washington: Office of the Federal Register, National Archives and Records Administration; 2017.

  9. 9.

    Muhammad M, Shah J, Jan MR, Ara B, Mahabat KM, Jan A. Spectrofluorimetric method for quantification of triazine herbicides in agricultural matrices. Anal Sci. 2016;32:313–6.

  10. 10.

    Mei M, Huang X, Yang X, Luo Q. Effective extraction of triazines from environmental water samples using magnetism-enhanced monolith-based in-tube solid phase microextraction. Anal Chim Acta. 2016;937:69–79.

  11. 11.

    Shah J, Rasul JM, Ara B, Shehzad FU. Quantification of triazine herbicides in soil by microwave-assisted extraction and high-performance liquid chromatography. Environ Monit Assess. 2011;178:111–9.

  12. 12.

    Jiménez-Soto JM, Cárdenas S, Valcárcel M. Dispersive micro solid-phase extraction of triazines from waters using oxidized single-walled carbon nanohorns as sorbent. J Chromatogr A. 2012;1245:17–23.

  13. 13.

    Hernández-Hernández AA, Alvarez-Romero GA, Castañeda-Ovando A, Mendoza-Tolentino Y, Contreras-López E, Galán-Vidal CA, et al. Optimization of microwave-solvothermal synthesis of Fe3O4 nanoparticles. Coating, modification, and characterization. Mater Chem Phys. 2018;205:113–9.

  14. 14.

    Ma WT, Fu KK, Cai Z, Jiang GB. Gas chromatography/mass spectrometry applied for the analysis of Triazine herbicides in environmental waters. Chemosphere. 2003;52:1627–32.

  15. 15.

    Zhou QX, Xie GH, Pag L. Rapid determination of atrazine in environmental water samples by a novel liquid phase microextraction. Chin Chem Lett. 2008;19:89–91.

  16. 16.

    Aguilar-Arteaga K, Rodriguez JA, Barrado E. Magnetic solids in analytical chemistry: a review. Anal Chim Acta. 2010;674:157–65.

  17. 17.

    Hernández-Hernández A, Álvarez-Romero GA, Contreras-López E, Aguilar-Arteaga K, Castañeda-Ovando A. Food analysis by microextraction methods based on the use of magnetic nanoparticles as supports: recent advances. Food Anal Methods. 2017;10:2974–93.

  18. 18.

    González AG, Herrador MA. A practical guide to analytical method validation, including measurement uncertainty and accuracy profiles. Trends Anal Chem. 2007;26:227–38.

  19. 19.

    Katsumata H, Kaneco S, Suzuki T, Ohta K. Determination of atrazine and simazine in water samples by high-performance liquid chromatography after preconcentration with heat-treated diatomaceous earth. Anal Chim Acta. 2006;577:214–9.

  20. 20.

    Zhao RS, Yuan JP, Jiang T, Shi JB, Cheng CG. Application of bamboo charcoal as solid-phase extraction adsorbent for the determination of atrazine and simazine in environmental water samples by high-performance liquid chromatography-ultraviolet detector. Talanta. 2008;76:956–9.

Download references


K. Aguilar-Arteaga, A. Castañeda-Ovando, and A.E. Cruz-Pérez thank Sistema Nacional de Investigadores for the stipend received. All authors gratefully acknowledge the Centro de Investigación en Ciencia y Tecnología Aplicada de Tabasco for the HRTEM analysis and the Consejo Nacional de Ciencia y Tecnologia (Mexico) for the project financing [Project number CB-2013-220163].

Author information

Correspondence to Araceli Castañeda-Ovando.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Additional information

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Aguilar-Arteaga, K., Hernández-Mera, C., Díaz-Batalla, L. et al. Development of a dispersive liquid-liquid microextraction coupled with magnetic dispersive microsolid phase extraction for determination of triazines in wastewater samples. Anal Bioanal Chem 412, 1203–1213 (2020). https://doi.org/10.1007/s00216-019-02354-4

Download citation


  • Coupled microextraction techniques
  • Magnetic adsorbents
  • Triazines
  • Dispersive liquid-liquid microextraction
  • Magnetic dispersive microsolid phase extraction