Accurate and Sensitive Determination Method for Procymidone and Chlorflurenol in Municipal Wastewater, Medical Wastewater and Irrigation Canal Water by GC–MS After Vortex Assisted Switchable Solvent Liquid Phase Microextraction

  • Fatih Kapukıran
  • Merve Fırat
  • Dotse Selali Chormey
  • Sezgin BakırdereEmail author
  • Nizamettin ÖzdoğanEmail author


In this study, the detection power of a gas chromatography mass spectrometer (GC–MS) for procymidone and chlorflurenol was significantly enhanced using switchable solvent liquid phase microextraction (SS-LPME) as a preconcentration tool. This was achieved by a comprehensive optimization of significant parameters to the SS-LPME method such as switchable solvent amount, concentration and amount of sodium hydroxide, pH effect and mixing effect. The optimum experimental conditions obtained were used to determine analytical figures of merit for the analytes. The limits of detection obtained were 0.44 and 2.9 ng/mL for procymidone and chlorflurenol, respectively. The optimum method was applied to water sampled from an irrigation canal and two wastewater samples. The samples were spiked at two concentrations and the percent recovery results obtained ranged between 86 and 115% for both analytes. The recovery results together with the low standard deviations recorded validated the method as accurate and precise.


Pesticide Switchable solvent GC–MS Procymidone Chlorflurenol 


  1. Alavanja MCR, Hoppin JA, Kamel F (2004) Health effects of chronic pesticide exposure: cancer and neurotoxicity. Annu Rev Public Health 25:155–197CrossRefGoogle Scholar
  2. Al-Rawi SM (2005) Contribution of man-made activities to the pollution of the tigris within mosul area/IRAQ. Int J Environ Res Public Health 2:245–250CrossRefGoogle Scholar
  3. Cao X, Limbach PA (2017) Mass Spectrometry: Nucleic Acids and Nucleotides Studied Using MS☆. In: Lindon JC, Tranter GE, Koppenaal DW (eds) Encyclopedia of spectroscopy and spectrometry, 3rd edn. Academic Press, Oxford, pp 764–771CrossRefGoogle Scholar
  4. Coskun O (2016) Separation techniques: chromatography. North Clin Istanb 3:156–160Google Scholar
  5. Dalvie MA, Cairncross E, Solomon A, London L (2003) Contamination of rural surface and ground water by endosulfan in farming areas of the Western Cape, South Africa. Environ Health 2:1CrossRefGoogle Scholar
  6. Damalas CA, Koutroubas SD (2016) Farmers’ exposure to pesticides: toxicity types and ways of prevention. Toxics 4:1CrossRefGoogle Scholar
  7. Dooley EE (2005) EHPnet: UNEP.Net freshwater portal. Environ Health Perspect 113:A451–A451Google Scholar
  8. Gondo TT, Obuseng VC, Mmualefe LC, Okatch H (2016) Employing solid phase microextraction as extraction tool for pesticide residues in traditional medicinal plants. J Anal Methods Chem 2016:2890219CrossRefGoogle Scholar
  9. Kponee KZ, Chiger A, Kakulu II, Vorhees D, Heiger-Bernays W (2015) Petroleum contaminated water and health symptoms: a cross-sectional pilot study in a rural Nigerian community. Environ Health 14:86CrossRefGoogle Scholar
  10. Liu Y, He M, Chen B, Hu B (2015) Solidification of floating organic drop microextraction combined with gas chromatography-flame photometric detection for the analysis of organophosphorus pesticides in water samples. Anal Methods 7:6182–6189CrossRefGoogle Scholar
  11. Memon ZM, Yilmaz E, Soylak M (2017) Switchable solvent based green liquid phase microextraction method for cobalt in tobacco and food samples prior to flame atomic absorption spectrometric determination. J Mol Liq 229:459–464CrossRefGoogle Scholar
  12. Oertel P, Bergmann A, Fischer S, Trefz P, Küntzel A, Reinhold P, Köhler H, Schubert JK, Miekisch W (2018) Evaluation of needle trap micro-extraction and solid-phase micro- extraction: obtaining comprehensive information on volatile emissions from in vitro cultures. Biomed Chromatogr 32:e4285CrossRefGoogle Scholar
  13. Özdoğan N, Kapukıran F, Mutluoğlu G, Chormey DS, Bakırdere S (2018) Simultaneous determination of iprodione, procymidone and chlorflurenol in lake water and wastewater matrices by GC-MS after multivariate optimization of binary dispersive liquid-liquid microextraction. Environ Monit Assess 190:607CrossRefGoogle Scholar
  14. Parrón T, Requena M, Hernández AF, Alarcón R (2014) Environmental exposure to pesticides and cancer risk in multiple human organ systems. Toxicol Lett 230:157–165CrossRefGoogle Scholar
  15. Pastor-Belda M, Garrido I, Campillo N, Viñas P, Hellín P, Flores P, Fenoll J (2015) Dispersive liquid–liquid microextraction for the determination of new generation pesticides in soils by liquid chromatography and tandem mass spectrometry. J Chromatogr A 1394:1–8CrossRefGoogle Scholar
  16. Qaqish BM, Al-Dalahmah O, Al-Motassem Y, Battah A, Ismail SS (2016) Occupational exposure to pesticides and occurrence of the chromosomal translocation t(14;18) among farmers in Jordan. Toxicol Rep 3:225–229CrossRefGoogle Scholar
  17. Raks V, Al-Suod H, Buszewski B (2018) Isolation, separation, and preconcentration of biologically active compounds from plant matrices by extraction techniques. Chromatographia 81:189–202CrossRefGoogle Scholar
  18. Reigart JR (2009) Recognition and management of pesticide poisonings. DIANE Publishing, WashingtonGoogle Scholar
  19. Seebunrueng K, Santaladchaiyakit Y, Soisungnoen P, Srijaranai S (2011) Catanionic surfactant ambient cloud point extraction and high-performance liquid chromatography for simultaneous analysis of organophosphorus pesticide residues in water and fruit juice samples. Anal Bioanal Chem 401:1703CrossRefGoogle Scholar
  20. Sosa-Ferrera Z, Mahugo-Santana C, Santana-Rodríguez JJ (2013) Analytical methodologies for the determination of endocrine disrupting compounds in biological and environmental samples. Biomed Res Int 2013:674838CrossRefGoogle Scholar
  21. Soylak M, Khan M, Yilmaz E (2016) Switchable solvent based liquid phase microextraction of uranium in environmental samples: a green approach. Anal Methods 8:979–986CrossRefGoogle Scholar
  22. Tongo I, Ezemonye L (2015) Human health risks associated with residual pesticide levels in edible tissues of slaughtered cattle in Benin City, Southern Nigeria. Toxicol Rep 2:1117–1135CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  • Fatih Kapukıran
    • 1
  • Merve Fırat
    • 2
  • Dotse Selali Chormey
    • 2
  • Sezgin Bakırdere
    • 2
    Email author
  • Nizamettin Özdoğan
    • 1
    Email author
  1. 1.Environmental Engineer DepartmentInstitute of Science, Bülent Ecevit UniversityZonguldakTurkey
  2. 2.Faculty of Art and Science, Chemistry DepartmentYıldız Technical UniversityİstanbulTurkey

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