Development, Validation, and Application of a Method Based on Reverse-Phase HPLC for the Simultaneous Determination of Six Organochlorine Pesticides in Surface and Groundwater Samples Collected from Northeast Libya


  • Osama I. G. Khreit Department of Pharmacology, Forensic Medicine, and Toxicology, Faculty of Veterinary Medicine, Omar Al-Mukhtar University, Elbeida City, Libya
  • Ifdil O. El Awamy Department of Plant Protection, Pesticide Chemistry, Faculty of Agriculture, Omar Al-Mukhtar University, Elbeida City, Libya.
  • Omukalthum A. Abduljalil Department of Plant Protection, Pesticide Chemistry, Faculty of Agriculture, Omar Al-Mukhtar University, Elbeida City, Libya.



HPLC, Validation; Residues, Surface Water, Groundwater


The contamination by organochlorine pesticides (OCPs) of the selected sites in the eastern region of Libya was investigated to estimate the current status of pollution in surface and groundwater sources. This study was conducted to determine the concentrations of some OCPs residue in surface and groundwater samples collected from thirty different sites around Al-Jabal Al-Akhdar northeast of Libya during the summer, autumn, and winter seasons of 2016. A simple and rapid method based on the liquid-liquid extraction method followed by an HPLC with reversed-phase was developed to determine six OCPs in water samples simultaneously. An HPLC instrument was supplied with a C18 column (250 mm × 4 mm; 4.6 μm particle size) and a UV detector at 238 nm. The mobile phase was composed of 0.1% propanol in water and acetonitrile (25/75, v/v). The method was validated using reference standards of these six OPCs at different concentration levels and shows good linearity in the concentrations between 5.0 and 25 µg mL− 1. The LOD and LOQ ranged from 0.71 to 2.24 μg mL -1 and 2.16 to 6.79 μg mL-1, respectively. Relative standard deviation (%RSD) ranged from 0.026 to 0.673 %. The only OCP residue found in the area of study was 2, 4-D, with a variation of its residue levels during the seasons. The overall results showed that surface water was more polluted with 2, 4-D than groundwater, which was detected in the wide range of concentration of 0.037 to 0.385 μg mL-1, 0.003 to 0.047 μg mL -1 and 0.012 to 0.039 μg mL-1 during summer, autumn, and winter, respectively.


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Adeyemi, D., Anyakora, C., Ukpo, G., Adedayo, A., & Darko, G. (2011). Evaluation of the levels of organochlorine pesticide residues in water samples of Lagos Lagoon using solid phase extraction method. Journal of Environmental Chemistry and Ecotoxicology, 3(6), 160-166.

Afful, S., Anim, A., & Serfor-Armah, Y. (2010). Spectrum of organochlorine pesticide residues in fish samples from the Densu Basin. Res J Environ Earth Sci, 2(3), 133-138.

Akan, J., Sodipo, O., Mohammed, Z., & Abdulrahman, F. (2014). Determination of organochlorine, organophosphorus and pyrethroid pesticide residues in water and sediment samples by high performance liquid chromatography (HPLC) with UV/visible detector. Journal of Analytical & Bioanalytical Techniques, 5(6), 1. DOI:

Akoto, O., Azuure, A. A., & Adotey, K. (2016). Pesticide residues in water, sediment and fish from Tono Reservoir and their health risk implications. SpringerPlus, 5(1), 1849. DOI:

APHA. (1995). Standard methods for the examination of water and wastewater. American Public Health Association, American Water Works association, Water Environment Federation, Washington(5), 4-12.

APHA. (1998). Standard methods for the examination of water and wastewater. Water Environment Federation(2), 9-31.

Ara, A. G., Haque, W., & Hasanuzzaman, M. (2014). Detection of Organochlorine and organophosphorus pesticides residues in water samples of Taragong thana in Rangpur district in Bangladesh. Research Journal of Environmental and Earth Sciences, 6(2), 85-89. DOI:

Azad, H. N., Kafilzadeh, F., Malekpour, R., & Shiva, A. H. (2012). Determination of Organochlorine Pesticide Residues inWater, Sediments and Fish from Lake Parishan, Iran. World, 4(2), 150-154.

Boussahel, R., Bouland, S., Moussaoui, K., Baudu, M., & Montiel, A. (2002). Determination of chlorinated pesticides in water by SPME/GC. Water research, 36(7), 1909-1911. DOI:

Chen, X., Zhang, H., Wan, Y., Chen, X., & Li, Y. (2018). Determination of 2, 4-Dichlorophenoxyacetic acid (2, 4-D) in rat serum for pharmacokinetic studies with a simple HPLC method. PLoS ONE, 13(1), e0191149. DOI:

Chowdhury, M. A. Z., Banik, S., Uddin, B., Moniruzzaman, M., Karim, N., & Gan, S. H. (2012). Organophosphorus and carbamate pesticide residues detected in water samples collected from paddy and vegetable fields of the Savar and Dhamrai Upazilas in Bangladesh. International journal of environmental research and public health, 9(9), 3318-3329. DOI:

Coady, K., Marino, T., Thomas, J., Sosinski, L., Neal, B., & Hammond, L. (2013). An evaluation of 2, 4-dichlorophenoxyacetic acid in the amphibian metamorphosis assay and the fish short-term reproduction assay. Ecotoxicology and environmental safety, 90, 143-150. DOI:

Cooper, J., & Dobson, H. (2007). The benefits of pesticides to mankind and the environment. Crop Protection, 26(9), 1337-1348. DOI:

Demoliner, A., Caldas, S. S., Costa, F. P., Gonçalves, F. F., Clementin, R. M., Milani, M. R., & Primel, E. G. (2010). Development and validation of a method using SPE and LC-ESI-MS-MS for the determination of multiple classes of pesticides and metabolites in water samples. Journal of the Brazilian Chemical Society, 21(8), 1424-1433. DOI:

Dores, E. F., Carbo, L., Ribeiro, M. L., & De-Lamonica-Freire, E. M. (2008). Pesticide levels in ground and surface waters of Primavera do Leste Region, Mato Grosso, Brazil. Journal of chromatographic science, 46(7), 585-590. DOI:

El-Ghit, H. M. A. (2016). Impact of Post-Emergence Application of Dichlorophenoxy Acetic Acid (2, 4-D) Herbicide on Growth and Development of Three Weeds Associated with Maize Growth. Int. J. Curr. Microbiol. App. Sci, 5(2), 794-801. DOI:

El-Osmani, R., Net, S., Dumoulin, D., Baroudi, M., Bakkour, H., & Ouddane, B. (2014). Solid phase extraction of organochlorine pesticides residues in groundwater (akkar plain, north Lebanon). International Journal of Environmental Research, 8(4), 903-912.

El-Saeid, M., Al-Turki, A., Al-Wable, M., & Abdel-Nasser, G. (2011). Evaluation of pesticide residues in Saudi Arabia ground water. Research Journal of Environmental Sciences, 5(2), 171. DOI:

El Bouraie, M. M., El Barbary, A., & Yehia, M. (2011). Determination of organochlorine pesticide (OCPs) in shallow observation wells from El-Rahawy contaminated area, Egypt. Environmental Research, Engineering and Management, 57(3), 28-38.

Erkmen, B., Yerli, S. V., Erk'akan, F., & Kolankaya, D. (2013). Persistent organochlorine pesticide residues in water and sediment samples from Lake Manyas, Turkey. Journal of environmental biology, 34(2), 171.

Hashmi, T. A. S., & Menon, S. K. (2015). Accumulation and distribution of persistent organochlorine pesticides and their contamination of surface water and sediments of the Sabarmati River, India. Journal of Advances in Environmental Health Research, 3(1).

Hellar-Kihampa, H. (2011). Pesticide residues in four rivers running through an intensive agricultural area, Kilimanjaro, Tanzania. Journal of Applied Sciences and Environmental Management, 15(2).

Hong, H., Chen, W., Xu, L., Wang, X., & Zhang, L. (1999). Distribution and fate of organochlorine pollutants in the Pearl River Estuary. Marine Pollution Bulletin, 39(1), 376-382. DOI:

Hunt, D. T. E., & Wilson, A. L. (1986). The chemical analysis of water: general principles and techniques (Vol. 2). Royal Society of Chemistry.

Ismail, M., Sayed, M., Khan, H. M., & Cooper, W. J. (2014). Analysis of pesticides in water samples and removal of monocrotophos by gamma irradiation. J Anal Bioanal Tech, 5(1), 1-10.

Ize-Iyamu, O., Asia, I., & Egwakhide, P. (2007). Concentrations of residues from organochlorine pesticide in water and fish from some rivers in Edo State Nigeria. International Journal of Physical Sciences, 2(9), 237-241.

Jamal, H. M. (2011). Occurrence of organochlorine pesticide residues in groundwater and soil from Syrian coastal area. Agriculture and Biology Journal of North America, 2(3), 488-492. DOI:

Jayashree, R., & Vasudevan, N. (2007). Organochlorine pesticide residues in ground water of Thiruvallur district, India. Environmental monitoring and assessment, 128(1-3), 209. DOI:

Lari, S. Z., Khan, N. A., Gandhi, K. N., Meshram, T. S., & Thacker, N. P. (2014a). Comparison of pesticide residues in surface water and ground water of agriculture intensive areas. Journal of Environmental Health Science and Engineering, 12(1), 1.

Lari, S. Z., Khan, N. A., Gandhi, K. N., Meshram, T. S., & Thacker, N. P. (2014b). Comparison of pesticide residues in surface water and ground water of agriculture intensive areas. Journal of Environmental Health Science and Engineering, 12(1), 11. DOI:

Leong, K. H., Tan, L. B., & Mustafa, A. M. (2007). Contamination levels of selected organochlorine and organophosphate pesticides in the Selangor River, Malaysia between 2002 and 2003. Chemosphere, 66(6), 1153-1159. DOI:

Mansour, S. A. (2004). Pesticide exposure—Egyptian scene. Toxicology, 198(1-3), 91-115. DOI:

Mariyono, J. (2008). Direct and indirect impacts of integrated pest management on pesticide use: a case of rice agriculture in Java, Indonesia. Pest management science, 64(10), 1069-1073. DOI:

Maurya, A., & Kumar, A. (2013). Organochlorine pesticides in the surface waters from sharda river region, Uttar Pradesh, India. The SIJ Transactions on Advances in Space Research & Earth Exploration (ASREE), 1(1), 8-10. DOI:

Munn, M. D., & Gruber, S. J. (1997). The relationship between land use and organochlorine compounds in streambed sediment and fish in the Central Columbia Plateau, Washington and Idaho, USA. Environmental Toxicology and Chemistry, 16(9), 1877-1887. DOI:

Nie, N. H., Bent, D. H., & Hull, C. H. (1970). SPSS: Statistical package for the social sciences.

Oerke, E.-C., & Dehne, H.-W. (2004). Safeguarding production—losses in major crops and the role of crop protection. Crop Protection, 23(4), 275-285. DOI:

Okoya, A. A., Ogunfowokan, A. O., Asubiojo, O. I., & Torto, N. (2013). Organochlorine pesticide residues in sediments and waters from Cocoa producing areas of Ondo State, Southwestern Nigeria. ISRN Soil Science, 2013. DOI:

Que Hee, S., & Sutherland, R. (1981). The phenoxyalkanoic herbicides. Vol. I. Chemistry, analysis, and environmental pollution. CRC Pres, Inc, Boca Raton, 319.

Saha, A., Gajbhiye, V., Gupta, S., & Kumar, R. (2012). Development of multi-residue method for determination of pesticides in river, ground and lake water in Delhi using gas chromatography. International Journal Agriculture Environment Biotechnology, 5(3), 199-205.

Sankararamakrishnan, N., Sharma, A. K., & Sanghi, R. (2005). Organochlorine and organophosphorous pesticide residues in ground water and surface waters of Kanpur, Uttar Pradesh, India. Environment international, 31(1), 113-120. DOI:

Shakerkhatibi, M., Mosaferi, M., Jafarabadi, M. A., Lotfi, E., & Belvasi, M. (2014). Pesticides residue in drinking groundwater resources of rural areas in the northwest of Iran. Health promotion perspectives, 4(2), 195.

Shamsipur, M., Yazdanfar, N., & Ghambarian, M. (2016). Combination of solid-phase extraction with dispersive liquid–liquid microextraction followed by GC–MS for determination of pesticide residues from water, milk, honey and fruit juice. Food chemistry, 204, 289-297. DOI:

Smilanick, J. L. (2008). Postharvest pathogens and disease management. HortScience, 43(6), 1932-1933. DOI:

Tang, Z., Yang, Z., Shen, Z., Niu, J., & Cai, Y. (2008). Residues of organochlorine pesticides in water and suspended particulate matter from the Yangtze River catchment of Wuhan, China. Environmental monitoring and assessment, 137(1), 427-439. DOI:

Tata Rao, S., Ch, V., Reddy, A., Veeraiah, K., & Padmavathi, P. (2014). Research article determination of organochlorine pesticides residues in the water of paddy fields of Prakasam district, Andhra Pradesh, India.

Uddin, A., Kumar, P., & Sarma, J. (2007). Early orogenic history of the eastern Himalayas: compositional studies of Paleogene sandstones from Assam, northeast India. International Geology Review, 49(9), 798-810. DOI:

WHO. (2004). 2,4-D in drinking water. Background document for development of WHO Guidelines for Drinking-Water Quality. DOI:

Yusiasih, R., Nugraha, W., & Hudayya, A. (2017). Determination of carbofuran in a river water sample using LC-MS/MS. IOP Conference Series: Earth and Environmental Science, DOI:

Zhao, L., & Lee, H. K. (2001). Application of static liquid-phase microextraction to the analysis of organochlorine pesticides in water. Journal of Chromatography A, 919(2), 381-388. DOI:




How to Cite

Khreit , O. I. G. . ., El Awamy, I. O. ., & Abduljalil, O. A. . (2020). Development, Validation, and Application of a Method Based on Reverse-Phase HPLC for the Simultaneous Determination of Six Organochlorine Pesticides in Surface and Groundwater Samples Collected from Northeast Libya. Al-Mukhtar Journal of Sciences, 35(2), 116–129.



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