In collaboration with Payame Noor University and Iranian Chemical Science and Technologies Association

Document Type : Full research article

Authors

1 Department of Chemistry, College of Natural Sciences, Jimma University, P. O. Box 378, Jimma, Ethiopia

2 Department of Chemistry, College of Natural Sciences, Jimma University, P. O. Box 378, Jimma, Ethiopia; The Regional Government of Oromia Science and Technology Development Agency, Addis Ababa, Ethiopia

Abstract

In this study, vortex-assisted low density based dispersive liquid-liquid microextraction followed by high performance liquid chromatography with ultraviolet detector has been developed for the determination of three pesticides including chlorflurenol-methyl, chlorfenvinphos, and diazinon from environmental water samples. Different parameters influencing the extraction efficiency such as the type and volume of extraction and disperser solvent, sample pH, salt addition as well as vortex and centrifugation time were investigated and the optimal conditions were obtained. Under the optimum conditions, the calibration curves were linear in the concentration range of 8.5–100, 3.1–100 and 36.5–600 ng/mL for chlorflurenol-Methyl, chlorfenvinphos and diazinon, respectively, with coefficient of determination (r2) of 0.993 or better. The limits of detection and quantification of the analytes, which were determined at 3 and 10 signal-to-noise ratio (S/N) ranged from 0.9–11 and 3.1–36.8 ng/mL, respectively. The proposed method has been successfully applied to the analysis of real water samples. The relative recoveries (%RR) studied at two spiking concentration levels were ranging from 76–108%, with the corresponding relative standard deviation (%RSD) ranging from 1.9–9.9%.  The results of study demonstrated that the proposed method is efficient for extraction and/or preconcentration of the three pesticides prior to quantitative determination utilizing HPLC–UV/Vis instrument.

Keywords

 
[1]     M.C.R. Alavanja, Pesticides use and exposure extensive worldwide, Rev. Environ. Health. 24 (2009) 303–309.
[2]     WHO/FAO. International code of conduct on the distribution and use of pesticides: guidelines for the registration of pesticides, Rome, Italy. 2010.
[3]     F.P. Garcia, S.Y.C. Ascencio, J.C.G. Oyarzun, A.C. Hernandez and P.V. Alavarado, Pesticides: classification, uses and toxicity. Measures of exposure and genotoxic risks, Int. J. Environ. Sci. Toxic. Res. 1 (2012) 279–293.
[4]     M. Galrilescu, Review: Fate of pesticides in the environment and its bioremediation, Eng. Life Sci. 5 (2005) 497–526. 
[5]     A.d.S. Pinheiro and J.B.d. Andrade, Development, validation and application of a SDME/GC-FID methodology for the multiresidue determination of organophosphate and pyrethroid pesticides in water, Talanta 79 (2009) 1354–1359.
[6]     C.A. Damalas and I.G. Eleftherohorinos, Pesticide Exposure, Safety Issues, and Risk Assessment Indicators, Int. J. Environ. Res. Public Health 8 (2011) 1402–1419.
[7]     WHO. Organophosphorous pesticides in the environment-integrated risk assessment, Geneva: 2001.
[8]     S. Wang, B. Xiang and Q. Tang, Trace determination of dichlorvos in environmental samples by room temperature ionic liquid-based dispersive liquid-phase microextraction combined with HPLC, J. Chromatogr. Sci. 50 (2012) 702–708.
[9]     T. Bedassa, A. Gure and N. Megersa, Low density solvent based dispersive liquid ⎯liquid microextraction and preconcentration of multiresidue pesticides in environmental waters for liquid chromatographic analysis, J. Anal. Chem. 70 (2015) 1199–1206.
[10] Q. Zhou, H. Bai, G. Xie and J. Xiao, Trace determination of organophosphorus pesticides in environmental samples by temperature controlled ionic liquid dispersive liquid-phase microextraction, J. Chromatogr. A 1188 (2008) 148–153.
[11] T. Tolcha, Y. Merdassa and N. Megersa, Low-density extraction solvent based solvent-terminated dispersive liquid–liquid microextraction for quantitative determination of ionizable pesticides in environmental waters, J. Sep. Sci. 36 (2013) 1119–1127.
[12] C. Wang, Q. Wu, C. Wu and Z. Wang, Determination of some organophosphorus pesticides in water and watermelon samples by microextraction prior to highperformance liquid chromatography, J. Sep. Sci. 34 (2011) 3231–3239.
[13] A. Cappiello, G. Famiglini and P. Palma, Trace level determination of organophosphorus pesticides in water with the new direct-electron ionization LC/MS interface. Anal. Chem. 74 (2002) 3547–3554.
[14]  N. Dujaković, S. Grujić, M. Radišić, T. Vasiljević and M. Laušević, Determination of pesticides in surface and ground waters by liquid chromatography-electrospray–tandem mass spectrometry, Anal. Chim.Acta 678 (2010) 63–72.
[15] C. Crescenzi, A. Di Cocia, E. Gurrriero, and R. Samperi, Development of a multiresidue method for analyzing pesticide traces in water based on solid-phase extraction and electrospray liquid chromatography mass spectrometry, Environ. Sci. Technol. 31 (1997) 479-488.
[16] M.A. Farajzadeh, S.E. Seyedi, M.S. Shalamzari and T.M. Bamorowa, Dispersive liquid–liquid microextraction using extraction solvent lighter than water. J. Sep. Sci. 32 (2009) 3191–3200.
[17] P.G. Su, and S.D. Huang, Determination of organophosphorus pesticides in water by solid-phase microextraction, Talanta 49 (1999) 393–402.
[18] B. Albero, C. Sanchez-Brunete and J.L. Tadeo, Determination of organophosphorus pesticides in fruit juices by matrix solid-phase dispersion and gas chromatography. J. Agri. Food Chem. 51 (2003) 6915–6921.
[19] F. Rodrigues, P. Mesquita, L. Oliveira, F. Oliveira, A. Filho, A. Pearo and J.  Andrae, Development of head space solid-phase microextraction/gas chromatography–mass spectrometry method for determination of organophosphorus pesticide residues in cow milk. Microchim. J. 98 (2011) 56–61.
[20]  M. Rezaee, Y. Assadi, M. Hosseini, E. Aghaee, F. Ahmadia and S. Berijani, Determination of organic compounds in water using dispersive liquid–liquid microextraction. J. Chromatogr. A. 1116, (2006) 1–9.
[21]  J. Ma, R. Xiao, J. Li, X. Zhao, B. Shi and S. Li, Determination of organophosphorus pesticides in underground water by SPE-GC–MS, J. Chromatogr. Sci.47 (2009) 111-115.
[22] T.A. Albanis and D.G. Hela, Multi-residue pesticide analysis in environmental water samples using solid-phase extraction discs and gas chromatography with flame thermionic and mass-selective detection, J. Chromatogr. A 707 (1995) 283–292.
[23] H. Çabuk, M. Akyüz and Ş. Ata, A simple solvent collection technique for a dispersive liquid–liquid m icroextra ction of parabens from aqueous samples using low-density organic solvent, J. Sep. Sci. 35 (2012) 2645–2652.
[24] P. Soisungnoen, R. Burakham and S. Srijarana Determination of organophosphorus pesticides using dispersive liquid–liquid microextraction combined with reversed electrode polarity stacking mode -micellar electrokinetic chromatography, Talanta 98 (2012) 62–68.
[25] L. Zhou, Z. Luo, S. Wang, Y. Hui, Z. Hu and X. Chen, In-capillary derivatization and laser-induced fluorescence detection for the analysis of organophosphorus pesticides by micellar electrokinetic chromatography, J. Chromatogr. A, 1149 (2007) 377–384.
[26] H. C. Liang, N. Bilon and M. T. Hay, Analytical methods for pesticide residues, Water Environ. Res. 85 (2013) 2114-2138.
[27] Y. Chen, Z. Guo, X. Wang and C. Qiu, Review: Sample preparation, J. Chromatogr. A 1184 (2008) 191–219,
[28] T. Padrón, A. Olivares, C. Ferrera and Z. Rodríguez, Microextraction techniques coupled to liquid chromatography with mass spectrometry for the determination of organic micro pollutants in environmental water samples, Molecules 19 (2014) 10320-10349.
[29] C. Nerín, J. Salafranca, M. Aznar and R. Batlle, Critical review on recent developments in solventless techniques for extraction of analytes, Anal. Bioanal. Chem. 393 (2009) 809–833
[30] M. Rezaee, Y. Yamini and M. Faraji, Evolution of dispersive liquid–liquid microextraction method, J. Chromatogr. A 1217 (2010) 2342–2357.
[31] L. Kocúrová, I.S. Balogh, J. Šandrejová and, V. Andruch, Recent advances in dispersive liquid–liquid microextraction using organic solvents lighter than water. A review, Microchem. J. 102 (2012) 11–17.
[32] A. Gure, F.J. Lara, A.M. García-Campaña, N. Megersa, and M. del Olmo-Iruela, Vortex-assisted ionic liquid dispersive liquid–liquid microextraction for the determination of sulfonylurea herbicides in wine samples by capillary high-performance liquid chromatography, Food Chem. 170 (2015) 348–353.
[33] C. Wu, H. Liu, W. Liu, Q. Wu, C.H. Wang and Z. Wang, Determination of organophosphorus pesticides in environmental water samples by dispersive liquid–liquid microextraction with solidification of floating organic droplet followed by high performance liquid chromatography, Anal. Bioanal. Chem., 397 (2010) 2543–2549.
[34] C.K. Zacharis, P.D. Tzanavaras, K. Roubos and K. Dhima, Solvent-based de-emulsification dispersive liquid–liquid microextraction combined with gas chromatography–mass spectrometry for determination of trace organochlorine pesticides in environmental water samples. J. Chromatogr. A 1217 (2010) 5896–5900.
[35] M.I. Leong and S.D. Huang, Dispersive liquid–liquid microextraction method based
on solidification of floating organic drop for extraction of organochlorine pesticides in water samples, J. Chromatogr. A 1216 (2009) 7645–7650.
[36]  H., Chen, R., Chena and S. Li, Low-density extraction solvent-based solvent terminated dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry for the determination of carbamate pesticides in water samples. J. Chromatogr. A 1217 (2010) 1244–1248.
[37]  L. Guo and H.K. Lee, Low-density solvent based ultrasound-assisted emulsification microextraction and on-column derivatization combined with gas chromatography–mass spectrometry for the determination of carbamate pesticides in environmental water samples, J. Chromatogr. A 1235 (2012) 1235, 1–9.
[38] D. Moreno González, L. Gámiz Gracia, J.M. Bosque Sendraand and A.M. GarcíaCampaña, Dispersive liquid-liquid microextraction using a low density extraction solvent for the determination of 17 N-methylcarbamates by micellar electrokinetic chromatography-electrospray-mass spectrometry employing a volatile surfactant, J. Chromatogr. A 1247 (2012) 26–34.
[39] Z. Yang, Y. Lu, Y. Liu, T. Wu, Z. Zhou and D. Liu, Vortex-assisted surfactantenhanced emulsification liquid–liquid microextraction, J. Chromatogr. A  1218 (2011) 7071–7077.
[40] K. Seebunrueng, Y. Santaladchaiyakit and S. Srijaranai, Vortex-assisted low density solvent based demulsified dispersive liquid–liquid microextraction and high-performance liquid chromatography for the determination of organophosphorus pesticides in water samples, Chemosphere 103 (2014) 51–58.
[41] EUROPEAN COMMISSION:  Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed. SANTE/11945/2015; Supersedes SANCO/12571/2013, Implemented by 01/01/2016.