Determination of Organochlorines Pesticide Residues in Water Samples Using Liquid-Liquid Extraction Method

Öz

In this study, chlorinated cyclic hydrocarbon pesticides were extracted from water using a solvent mixture (hexane: dichloromethane), and their content was determined by GC-MS equipped with electron ionization (EI) and selected ion monitoring (SIM) methods. Additionally, the validation parameters for the method used were established. The recovery ratios of the spike levels varied between 82.7% and 95.4%. Heptachlor had the lowest recovery value, 82.7%, at a concentration of 1.480 µg/L, while Aldrin had the highest recovery value, 95.4%, at 11.200 µg/L. A satisfactory linearity was found for each pesticide at the four varied spike levels during the extraction procedure. Trans-Heptachlor > Heptachlor > trans-Chlordane > cis-Chlordane was the order in which the recovery efficiency of pesticides containing chlorine cyclo rings declined. Trans-Chlordane > trans-Heptachlor >Endosulfan > Dieldrin > Heptachlor > Aldrin > cis-Chlordane was followed by a decline in the relevant value of pesticides having two or more cyclic rings for the seven pesticides that made up the entire analysis period in this experiment a sufficient differentiation was made in around 18 minutes.

Anahtar Kelimeler

• Residue
• Analysis
• Pesticide
• Extraction

Kaynakça

1. Abrams, P.A. (1995). Implications of dynamically variable traits for identifying, classifying, andmeasuring direct and indirect effects in ecological communities, TheAmerican.Naturalist, 146, 112–134.
2. Ago, K.A., Kitte, S.A., Chirfa, G. and Gure, A. (2023). Determination effervescent powder-assisted floating organic solvent-based dispersive liquid-liquid microextraction for determination of organochlorine pesticides in water by GC–MS. Heliyon, 9, 1-10. https://doi.org/10.1016/j.heliyon.2023.e12954
3. Ahmadi, F., Assadi Y., Hosseini S.M.R. M. and Rezaee M. (2006). Determination of organophosphorus pesticides in water samples by single drop microextraction and gas chromatography-flame photometric detector. Journal of Chromatography A, 1101, 307-312.
4. Alexandratos, N. and Bruinsma. J. (2012). World agriculture towards. 2030/2050., ESA Working paper, No.12-03.
5. Bevan, M.W., Flavell, R. B. and Chilton M.D.A. (1983). Chimaeric antibiotic resistance gene as a selectable marker for plant cell transformation. Nature, 304, 184–187.
6. Biswasa, S., Mondal, R., Mukherjee, A., Sarkara, M. and Kole R.K. (2019). Simultaneous determination and risk assessment of fipronil and its metabolites in sugarcane, using GC-ECD and confirmation by GC-MS/MS. Food Chemistry, 272, 559–567.
7. Bock, B. R. (1984). Efficient use of nitrogen in cropping systems. Nitrogen in Crop Production. American Society of Agronomy, Wisconsin, https://doi.org/10.2134/1990.nitrogenincropproduction.c18
8. Brito, N.M., Navickiene, S., Polese, L., Jardim, E.F.G., Abakerli, R.B. and Ribeiro, M.L. (2002). Determination of pesticide residues in coconut water by liquid–liquid extraction and gas chromatography with electron-capture plus thermionic specific detection and solid-phase extraction and high-performance liquid chromatography with ultraviolet detection. Journal of Chromatography, A, 957, 201-209.

9. Corcia, A.D. and Marchetti, M. (1991). Multiresidue method for pesticides in drinking water using a graphitized carbon black cartridge extraction and liquid chromatography analysis. Analytical Chemistry, 63, 580-585.
10. Douglas, L., MacKinnon, G., Cook, G., Duncan, H., Briddon, A. and Seamark, S. (2018). Determination of chlorpropham (CIPC) residues, in the concrete flooring of potato stores, using quantitative (HPLC UV/VIS) and qualitative (GCMS) methods. Chemosphere, 195, 119-124.
11. Ferrer, M.C., Gomez, J.F., Garc, R.F.J., Ferrer, I.E., Thurman, M. and Fernandez-A.A.R. (2005). Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography tandem mass spectrometry. Journal of Chromatography A, 1069, 183-194, https://doi.org/10.1016/j.chroma.2005.02.015
12. Fillion, J., Sauve, F. and Selwyn, J.(2000). Multiresidue method for the determination of residues of 251 pesticides in fruits and vegetables by gas chromatography/mass spectrometry and liquid chromatography with fluorescence detection. Journal Of Aoac Internatıonal, 83, 698-713.
13. Frenich, A.G., Gonzalez, R.M.J, Arrebola, F.J. and Vida J.L.M. (2005). Potentiality of gas chromatography-triple quadrupole mass spectrometry in vanguard and rearguard methods of pesticide residues in vegetables. Analytical Chemistry, 77, 4640-4648.
14. Garcia, R.J.F., Gilbert, L.B. and Molina, D.A. (2008). Determination of pesticide residues in fruit-based soft drinks. Analytical Chemistry, 80, 8966–8974.
15. Grimalt, S., Pozo, O.J., Sancho, J.V. and Hernandez, F. (2007). Use of liquid chromatography coupled to quadrupole time-of-flight mass spectrometry to investigate pesticide residues in fruits, Analytical Chemistry, 79, 2833-2843.
16. Harshit, D., Charmy, K. and Nrupesh, P. (2017). Organophosphorus pesticides determination by novel hplc and spectrophotometric method. Food Chemistry, 230, 448-453. https://doi.org/10.1016/j.foodchem.2017.03.083
17. Hayward, D.G. and Wong J. W. (2009). Organohalogen and organophosphorous pesticide method for ginseng roots a comparison of gas chromatography-single quadrupole mass spectrometry with high resolution time-of-flight mass spectrometry. Analytical Chemistry, 81, 5716-5723. https://doi.org/10.1021/ac900494a
18. Hernández, A.F., Parrón, T., Tsatsakis, A.M., Requena, M., Alarcon, R.and Guarnido O. (2013). Toxic effects of pesticide mixtures at a molecular level: Their relevance to human health.Toxicology, 307, 136-145.
19. Kusvuran, E., Yildirim, D., Mavruk, F. and Ceyhan M. (2012). Removal of chloropyrifos ethyl, tetradifon and chlorothalonil pesticide residues from citrus by using ozone. Journal of Hazardous Materials, 241, 287-300.
20. Lawrence, J.F. (1976). A comparison of electron-capture GLC, electrolytic-conductivity GLC and UV-absorption HPLC for the analysis of some herbicides in foods, Journal of Chromatographic Science, 14, 557-559.
21. Lehotay, S.J. (2005). Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. Journal Of AOAC International, 88, 595-614.
22. Machado, I., Gérez, N., Pistón, M., Heinzen, H. and Cesio, M.V. (2017). Determination of pesticide residues in globe artichoke leaves and fruits by GC–MS and LC–MS/MS using the same QuEChERS procedure. Food Chemistry, 227, 227-236. https://doi.org/10.1016/j.foodchem.2017.01.025
23. Mao, X., Wan, Y., Li, Z., Chen, L., Lew, H. and Yang, H. (2019). Analysis of organophosphorus and pyrethroid pesticides in organic and conventional vegetables using QuEChERS combined with dispersive liquidliquid microextraction based on the solidification of floating organic droplet. Food Chemistry, 309, 1-9, doi: https://doi.org/10.1016/j.foodchem.2019.125755.
24. Pellicer, C.E., Belenguer, C., Sapiña, C. B., Amorós, P. , Haskouri, J. E., Herrero, M.J. M.and Mauri, A. R. (2022). Mesoporous silica sorbent with gold nanoparticles for solid-phase extraction of organochlorine pesticides in water samples. Journal of Chromatography A, 1662, 462-729. https://doi.org/10.1016/j.chroma.2021.462729
25. Pengpumkiat, S., Nammoonnoy, J., Wongsakoonkan, W., Konthonbut, P. and Kongtip, P. (2020). A microfluidic paper-based analytical device for type-ıı pyrethroid targets in an environmental water sample. Sensors, 20(4107), 1-15. doi:10.3390/s20154107
26. Public health ımpact of pesticides used in agriculture,(2019). Geneva, WHO, accessed 8 june 2019.
27. Rissatoa, S.R., Galhiane, M.S., Knoll F.R.N. and Apon B.M. (2004). Supercritical fluid extraction for pesticide multiresidue analysis in honey: determination by gas chromatography with with electron-capture and mass spectrometry detection. Journal of Chromatography A, 1048, 153-159. https://doi.org/10.1016/j.chroma.2004.07.053
28. Santos, D.M.J., Rubio, B.S., Fernández, T.G.T. and Polo, D.L.M. (2001). Stability studies of carbamate pesticides and analysis by gas chromatography with flame ionization and nitrogen–phosphorus detection. Journal of Chromatography A, 921, 287-296.
29. Sereshti, H., Seraj, M., Soltani, S., Nodeh, H.M. AliAbadi, M.H.S. and Taghizadeh.M. (2022). Development of a sustainable dispersive liquid–liquid microextraction based on novel 243 hydrophobic and hydrophilic natural deep eutectic solvents for the analysis of multiclass pesticides in water. Microchemical Journal, 175, 107-226.
30. Shabeer, T.P.A., Girame, R., Utture, S., Oulkar, D., Banerjee, K., Ajay, D., Arimboor, R. and Menon, K.R.K. (2018). Optimization of multi-residue method for targeted screening and quantitation of 243 pesticide residues in cardamom (Elettaria cardamomum) by gas chromatography tandem mass spectrometry (GC-MS/MS) analysis. Chemosphere, 193, 447-453. https://doi.org/10.1016/j.chemosphere.2017.10.133
31. Thier, HP. and Zeumer, H. (1992). Manual of pesticide residue analysis, Weinheim: Wiley VCH, II, 26–28.
32. Van, Z.P. (1998). Analytical methods for residues of pesticides in foodstuffs. 6th edition, Part I. Annex B. The hague: General inspectorate for health protection, 1–8.
33. Wu J., Tragas, C., Lord, H. and Pawliszyn J. (2002). Analysis of polar pesticides in water and wine samples by automated in-tube solid-phase microextraction coupled with high-performance liquid chromatography–mass spectrometry. Journal of Chromatography A, 976, 357-367.
34. Xiao-qin, L., Yun-fei, L., Wen-ting, M., Dong-xiang, L., Sun, H., Ling, T. and Sun, G. (2016). A multi-residue method for simultaneous determination of 74 pesticides in Chinese material medica using modified QuEChERS sample preparation procedure and gas chromatography tandem massspectrometry. Journal of Chromatography B, 1015(1016), 1-12. http://dx.doi.org/10.1016/j.jchromb.2016.01.029