Journal of Analytical Chemistry

, Volume 71, Issue 5, pp 508–512 | Cite as

QuEChERS method combined with GC‒MS for pesticide residues determination in water

  • Sherif B. Abdel GhaniEmail author
  • Ahmad H. Hanafi


A miniaturized, QuEChERS based, liquid–liquid extraction method followed by gas chromatography–mass spectrometry was developed and validated for pesticide residues determination in water. Malathion, chlorpyrifos, profenofos, chlorfenapyr, pyriproxyfen, λ-cyhalothrin, coumaphos and α-cypermethrin were selected for this study. The accuracy, precision, specificity, linearity, limit of detection and limit of quantification were evaluated. The recovery ranged from 85.3 to 107% with RSD ranging from 1.8 to 15.4%. The linearity showed reliable range (0.995–0.999). The limit of detection ranged from 0.3 to 4 μg/L. Matrix effect was evaluated. The obtained results meet the European Commission standard legislations, implying that our method can be considered accurate and reproducible. The validated method was used to analyze river and well water samples. No residues of the investigated pesticides were detected in all collected water samples.


QuEChERS water pesticide residues GC‒MS 


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  1. 1.
    Espada, M.C.P., Liebanas, F.J.A., Frenich, A.G., and Vidal, J.L.M., Int. J. Environ. Anal. Chem., 1999, vol. 75, nos. 1-2, p. 165.CrossRefGoogle Scholar
  2. 2.
    Espada, M.C.P., Frenich, A.G., Vidal, J.L.M., and Parilla, P., Anal. Lett., 2001, vol. 34, no. 4, p. 597.CrossRefGoogle Scholar
  3. 3.
    Prestes, O.D., Friggi, C.A., Adaime, M.B., and Zanella, R., Quim. Nova, 2009, vol. 32, no. 6, p. 1620.CrossRefGoogle Scholar
  4. 4.
    Kustera, M., Alda, M.L., and Barcelo, D., J. Chromatogr. A, 2009, vol. 1216, p. 520.CrossRefGoogle Scholar
  5. 5.
    Barceló, D. and Hennion, M.C., Sample handling techniques (extraction and clean-up of samples), in Trace Determination of Pesticides and their Degradation Products in Water, Amsterdam: Elsevier, 1997, p. 249.Google Scholar
  6. 6.
    Frenich, A.G., Vidal, J.L.M., Espada, M.C.P., Garcia, M.D.G., and Arrebola, F.J., Chromatographia, 2000, vol. 52, nos. 9-10, p. 614.CrossRefGoogle Scholar
  7. 7.
    Durand, G. and Barcelo, D., Talanta, 1993, vol. 40, no. 11, p. 1665.CrossRefGoogle Scholar
  8. 8.
    Bruzzoniti, M.C., Sarzanini, C., and Mentasti, E., J. Chromatogr. A, 2000, vol. 902, p. 289.CrossRefGoogle Scholar
  9. 9.
    Tankiewicz, M., Fenik, J., and Biziuk, M., Talanta, 2011, vol. 86, p. 8.CrossRefGoogle Scholar
  10. 10.
    Baez, M.A., Navarro, S., and Solar, A., Bol. Soc. Chil. Quim. (1949–2002), 1999, vol. 44, no. 2, p. 217.Google Scholar
  11. 11.
    Purdesova, A., Hrouzkova, S., Andrascikova, M., Krascsenits, Z., and Matisova, E., Anal. Methods, 2013, vol. 5, no. 13, p. 3403.CrossRefGoogle Scholar
  12. 12.
    Dadfarnia, S. and Shabani, A.M.H., Anal. Chim. Acta, 2010, vol. 658, p. 107.CrossRefGoogle Scholar
  13. 13.
    Jeannot, M.A., Przyjazny, A., and Kokosa, J.M., J. Chromatogr. A, 2010, vol. 1217, no. 16, p. 2326.CrossRefGoogle Scholar
  14. 14.
    Boyd-Boland, A.A., Madgic, S., and Pawliszyn, J.B., Analyst, 1996, vol. 121, no. 7, p. 929.CrossRefGoogle Scholar
  15. 15.
    Pawliszyn, J., Solid-Phase Microextraction: Theory and Practice, New York Wiley, 1997.Google Scholar
  16. 16.
    Anastassiades, M., Lehotay, S.J., Stajnbaher, D., and Schenck, F., J. AOAC Int., 2003, vol. 86, no. 2, p. 412.Google Scholar
  17. 17.
    Lehotay, S.J., Mastovska, K., and Yun, S.J., J. AOAC Int., 2005, vol. 88, no. 2, p. 630.Google Scholar
  18. 18.
    Koesukwiwat, U., Lehotay, S.J., Miao, S., and Leepipatpiboon, N., J. Chromatogr. A, 2010, vol. 1217, no. 43, p. 6692.CrossRefGoogle Scholar
  19. 19.
    Sinha, S.N., Vasudev, K., Vishnu, M., and Rao, V., Food Chem., 2012, vol. 132, no. 3, p. 1574.CrossRefGoogle Scholar
  20. 20.
    Hou, X., Han, M., Dai, X.H., Yang, X.F., and Yi, S., Food Chem., 2013, vol. 138, no. 2, p. 1198.CrossRefGoogle Scholar
  21. 21.
    López, M.G., Fussell, R.J., Stead, S.L., Roberts, D., McCullagh, M., and Rao, R., J. Chromatogr. A, 2014, vol. 1373, p. 40.CrossRefGoogle Scholar
  22. 22.
    Yang, Y., Kong, W., Zhao, L., Xiao, Q., Liu, H., Zhao, X., and Yang, M., J. Chromatogr. B: Anal. Technol. Biomed. Life Sci., 2015, vol. 974, p. 118.CrossRefGoogle Scholar
  23. 23.
    Zeying, H., Wang, L., Peng, Y., Luo, M., Wang, W., and Liu, X., Food Chem., 2015, vol. 169, p. 372.CrossRefGoogle Scholar
  24. 24.
    Brondi, S.H.G., de Macedo, A.N., Vicente, G.H.L., and Nogueira, A.R.A., Bull. Environ. Contam. Toxicol., 2011, vol. 86, p. 18.CrossRefGoogle Scholar
  25. 25.
    Shi, C., Wenjun, G., Jie, C., and Zhu, G., Bull. Environ. Contam. Toxicol., 2010, vol. 84, p. 236.CrossRefGoogle Scholar
  26. 26.
    Wu, X., Xu, J., Liu, X., Dong, F., Wu, Y., Zhang, Y., and Zheng, Y., Bull. Korean Chem. Soc., 2013, vol. 34, no. 3, p. 917.CrossRefGoogle Scholar
  27. 27.
    Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed, European Commission Health & Consumer Protection Directorate-General, SANCO/12571/2013, 2013.Google Scholar
  28. 28.
    Tomlin, C.D.S., The e-Pesticide Manual, Surrey British Crop Prot. Counc., 2000.Google Scholar
  29. 29.
    Mantzos, N., Karakitsou, A., Zioris, I., Leneti, E., and Konstantinou, I., Int. J. Environ. Anal. Chem., 2013, vol. 93, p. 1566.CrossRefGoogle Scholar
  30. 30.
    de Sousa, F.A., Costa, A., de Queiroz, M., Tefilo, R., Neves, A., and de Pinho, G., Food Chem., 2012, vol. 135, p. 179.CrossRefGoogle Scholar
  31. 31.
    MacDougall, D. and Crummett, B.W., Anal. Chem., 1980, vol. 52, no. 14, p. 2242.CrossRefGoogle Scholar
  32. 32.
    Nile, Wikipedia. https://enwikipediaorg/wiki/Nile. Cited June 15, 2015.Google Scholar
  33. 33.
    Malhat, F. and Nasr, I., Am. J. Water. Res., 2013, vol. 1, no. 1, p. 1.Google Scholar
  34. 34.
    Al-Salamah, I.S. and Nassar, I.N., J. Appl. Sci., 2009, vol. 9, no. 19, p. 3555.CrossRefGoogle Scholar

Copyright information

© Pleiades Publishing, Ltd. 2016

Authors and Affiliations

  1. 1.Department of Plant Production and ProtectionQassim UniversityAl-QassimSaudi Arabia
  2. 2.Department of Plant ProtectionAin Shams UniversityCairoEgypt

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