Food Science and Biotechnology

, Volume 27, Issue 5, pp 1525–1530 | Cite as

Analytical method validation for terbutryn using gas chromatography/ion trap, gas chromatography/mass selective detector, and liquid chromatography/triple quadrupole mass spectrometers

  • Hae Won Jang
  • Jangho Lee
  • Hyunwook Choi
  • Tae Gyu Nam
  • Seung-Hyun Kim
  • Kwang-Geun LeeEmail author


Analytical methods including solvent extraction followed by gas chromatography/ion-trap (GC/IT) with scan and MS/MS mode, a GC/mass selective detector (GC/MSD), and liquid chromatography/triple quadrupole mass spectrometers (LC/MS/MS) were optimized to identify and quantify terbutryn. The spike recovery was 96.5% using GC/IT with scan mode and 103.5% with MS/MS mode, 90.3% by GC/MSD, and 92.5% by LC/MS/MS. The limit of detection (LOD) was 0.0015 mg/kg by GC/IT with scan, 0.026 mg/kg with MS/MS mode, 0.015 mg/kg with GC/MSD, and 0.026 mg/kg by LC/MS/MS. Of the four methods, GC/IT with scan mode was determined to be the most sensitive (with LOD: 0.0015 mg/kg and limit of quantitation (LOQ): 0.0047 mg/kg), rapid (retention time: 9.6 min) and the most precise method (relative standard deviation: 17%) for the quantification of terbutryn. GC/IT with scan mode proved to be the more sensitive analytical method for terbutryn than other methods in this study, showing better accuracy and rapid analysis.


Terbutryn Gas chromatography/mass selective detector Gas chromatography/ion trap Liquid chromatography/triple quadrupole mass spectrometers 



This research was supported by High Value added Food Technology Development Program (Project Nos. 314078-3 and 316050-03) from Ministry of Agriculture, Food, and Rural Affairs (Republic of Korea).

Compliance with ethical standards

Conflict of interest

The authors declare that there are no conflicts of interest.


  1. 1.
    Wang S, Zhao P, Min G, Fang G. Multi-residue determination of pesticides in water using multi-walled carbon nanotubes solid-phase extraction and gas chromatography–mass spectrometry. J. Chromatogr. A. 1165: 166–171 (2007).CrossRefGoogle Scholar
  2. 2.
    Frıas S, Sánchez MJ, Rodrıguez MA. Determination of triazine compounds in ground water samples by micellar electrokinetic capillary chromatography. Anal. Chem. Acta. 503: 271–278 (2004).CrossRefGoogle Scholar
  3. 3.
    Larsen L, Sørensen SR, Aamand J. Mecoprop, isoproturon, and atrazine in and above a sandy aquifer: vertical distribution of mineralization potential. Environ. Sci. Technol. 34: 2426–2430 (2000).CrossRefGoogle Scholar
  4. 4.
    Nilson EL, Unz RF. Antialgal substances for iodine-disinfected swimming pools. Appl. Environ. Microbiol. 34: 815–822 (1977).PubMedPubMedCentralGoogle Scholar
  5. 5.
    Velisek J, Stara A, Kolarova J, Svobodova Z. Biochemical, physiological and morfological responses in common carp (Cyprinus carpio L.) after long-term exposure to terbutryn in real environmental concentration. Pest Biochem. Physiol. 100: 305–313 (2011).CrossRefGoogle Scholar
  6. 6.
    U.S. Environmental Protection Agency. Fact Sheet Number 104: Terbutryn, U.S. EPA, Washington, DC, USA (1986).Google Scholar
  7. 7.
    Villarini M, Scassellati-Sforzolini G, Moretti M, Pasquini R. In vitro genotoxicity of terbutryn evaluated by the alkaline single-cell microgel-electrophoresis” comet” assay. Cell Biol. Toxicol. 16: 285–292 (2000).CrossRefGoogle Scholar
  8. 8.
    NHMRC N. Australian drinking water guidelines paper 6 national water quality management strategy. National Health and Medical Research Council, National Resource Management Ministerial Council, Commonwealth of Australia, Canberra, Australia (2011).Google Scholar
  9. 9.
    Lewis RJ. Sax’s dangerous properties of industrial materials. 10th ed. Vol. 3. Van Nostrand Reinhold, New York, USA (2000).Google Scholar
  10. 10.
    Lehotay SJ. Multiclass, multiresidue analysis of pesticides, strategies for Encyclopedia of Analytical Chemistry. Wiley, Chichester (2000).Google Scholar
  11. 11.
    Quednow K, Püttmann W. Monitoring terbutryn pollution in small rivers of Hesse, Germany. J. Environ. Monitor. 9: 1337–1343 (2007).CrossRefGoogle Scholar
  12. 12.
    Lapworth DJ, Gooddy DC, Stuart ME, Chilton PJ, Cachandt GC, Knapp M, Bishop S. Pesticides in groundwater: some observations on temporal and spatial trends. Water Environ. J. 20: 55–64 (2006).CrossRefGoogle Scholar
  13. 13.
    Djozan D, Ebrahimi B, Mahkam M, Farajzadeh MA. Evaluation of a new method for chemical coating of aluminum wire with molecularly imprinted polymer layer. Application for the fabrication of triazines selective solid-phase microextraction fiber. Anal. Chem. Acta. 674: 40–48 (2010).CrossRefGoogle Scholar
  14. 14.
    Djozan D, Mahkam M, Ebrahimi B. Preparation and binding study of solid-phase microextraction fiber on the basis of ametryn-imprinted polymer: application to the selective extraction of persistent triazine herbicides in tap water, rice, maize and onion. J. Chromatogr. A. 1216: 2211–2219 (2009).CrossRefGoogle Scholar
  15. 15.
    Gao S, You J, Zheng X, Wang Y, Ren R, Zhang R, Bai Y, Zhang H. Determination of phenylurea and triazine herbicides in milk by microwave assisted ionic liquid microextraction high-performance liquid chromatography. Talanta 82: 1371–1377 (2010).CrossRefGoogle Scholar
  16. 16.
    Hernández F, Serrano R, Miralles MC, Font N. Gas and liquid chromatography and enzyme linked immuno sorbent assay in pesticide monitoring of surface water from the western mediterranean (Comunidad Valenciana, Spain). Chromatographia 42: 151–158 (1996).CrossRefGoogle Scholar
  17. 17.
    Maloschik E, Ernst A, Hegedűs G, Darvas B, Székács A. Monitoring water-polluting pesticides in Hungary. Microchem. J. 85: 88–97 (2007).CrossRefGoogle Scholar
  18. 18.
    Adams NH, Levi PE, Hodgson E. In vitro studies of the metabolism of atrazine, simazine, and terbutryn in several vertebrate species. J. Agric. Food. Chem. 38: 1411–1417 (1990).CrossRefGoogle Scholar
  19. 19.
    Carabias-Martínez, R., Rodríguez-Gonzalo E, Herrero-Hernández E, Sánchez-San Román FJ, Flores MG. Determination of herbicides and metabolites by solid-phase extraction and liquid chromatography: Evaluation of pollution due to herbicides in surface and groundwaters. J. Chromatogr. A. 950: 157–166 (2002).Google Scholar
  20. 20.
    Pacáková V, Štulík K, Jiskra J. High-performance separations in the determination of triazine herbicides and their residues. J. Chromatogr. A. 754: 17–31 (1996).CrossRefGoogle Scholar
  21. 21.
    Patsias J, Papadopoulou-Mourkidou E. Rapid method for the analysis of a variety of chemical classes of pesticides in surface and ground waters by off-line solid-phase extraction and gas chromatography-ion trap mass spectrometry. J. Chromatogr. A. 740: 83–98 (1996).CrossRefGoogle Scholar
  22. 22.
    Voyksner RD, Pack T. Investigation of collisional‐activation decomposition process and spectra in the transport regions of an electrospray single‐quadrupole mass spectrometer. Rapid Commun. Mass Spectrom. 5: 263–268 (1991).CrossRefGoogle Scholar
  23. 23.
    Zambonin CG, Palmisano F. Determination of triazines in soil leachates by solid-phase microextraction coupled to gas chromatography–mass spectrometry. J. Chromatogr. A. 874: 247–255 (2000).CrossRefGoogle Scholar
  24. 24.
    Bagheri H, Vreuls JJ, Ghijsen RT, Brinkman UT. Determination of triazine herbicides in surface and drinking waters by off-line combination of liquid chromatography and gas chromatography-mass spectrometry. Chromatographia 34: 5–13 (1992).CrossRefGoogle Scholar
  25. 25.
    Postigo C, de Alda MJ, Barceló D, Ginebreda A, Garrido T, Fraile J. Analysis and occurrence of selected medium to highly polar pesticides in groundwater of Catalonia (NE Spain): An approach based on on-line solid phase extraction–liquid chromatography–electrospray-tandem mass spectrometry detection. J. Hydrol. 383: 83–92 (2010).CrossRefGoogle Scholar
  26. 26.
    Muir DC. Determination of terbutryne and its degradation products in water, sediments, aquatic plants and fish. J. Agric. Food. Chem. 28: 714–719 (1980).CrossRefGoogle Scholar
  27. 27.
    Yang W, Zhang H, Liu Y, Wang J, Zhang YC, Dong AJ, Zhao HT, Sun CH, Cui J. Multiresidue method for determination of 88 pesticides in berry fruits using solid-phase extraction and gas chromatography–mass spectrometry: Determination of 88 pesticides in berries using SPE and GC–MS. Food Chem. 127:855–865 (2011).CrossRefGoogle Scholar

Copyright information

© The Korean Society of Food Science and Technology and Springer Science+Business Media B.V., part of Springer Nature 2018

Authors and Affiliations

  • Hae Won Jang
    • 1
  • Jangho Lee
    • 1
    • 3
  • Hyunwook Choi
    • 1
  • Tae Gyu Nam
    • 1
  • Seung-Hyun Kim
    • 2
  • Kwang-Geun Lee
    • 4
    Email author
  1. 1.Korea Food Research InstituteSeongnamKorea
  2. 2.Department of Applied Bioscience, College of Life and Environmental ScienceKonkuk UniversitySeoulKorea
  3. 3.Food Biotechnology ProgramKorea University of Science and TechnologyDaejeonKorea
  4. 4.Department of Food Science and BiotechnologyDongguk UniversityGoyangKorea

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