Development and Validation of New Clean-Up Approach for 21 Organo-Chlorinated Pesticides (OCPs)
More details
Hide details
Kuwait Institute for Scientific Research (KISR), Deputy Director General Office for Research, 13109 Safat, P.O. Box 24885, Kuwait
Amal Al-Rashdan   

Kuwait Institute for Scientific Research (KISR), Deputy Director General Office for Research, 13109 Safat, P.O. Box 24885, Kuwait
Publication date: 2017-10-05
Eurasian J Anal Chem 2014;9(2):66–78
A validated procedure was developed for the separation and clean-up of Organo-Chlorinated Pesticides (OCPs) extracted from fish samples, using different adsorbent materials and different solvents composition. Pressurized liquid extraction (PLE) has been utilized for the extraction of OCPs. PLE provides one of the best alternative to conventional extraction methods. The different adsorbent materials as well as solvents composition were evaluated for the best clean-up steps of OCPs extracted from fish samples. Among the eight examined adsorbent materials, florisil and alumina were selected with hexane: ethylacetate (8:2, v/v) solvent mixture throughout the experiment. The highest recoveries were obtained (75-99.8 %). Detection was performed by GC-MS in Negative Chemical Ionization (NCI) mode, due to its high sensitivity and selectivity to chlorinated compounds. Bio-Beads SX-3 Based on Gel permeation Chromatography (GPC) was utilized for the removal of fat. The accuracy of the method (n= 5) is expressed as recovery (%) that was calculated to be between 56% and 98%, and the precision of the method is expressed as Relative Standard Deviation (RSD), that was obtained to be between 5% and 28 %.
Wania F, Mackay D (1996) Tracking the Distribution of Persistent Organic Pollutants. Environ. Sci. Technol. 30: 390A-396A.
Bjorklund E, Nilson T, Bowadt S (2000) Pressurised liquid extraction of persistent organic pollutants in environmental analysis. Trends Anal. Chem. 19(7): 434-445.
Giergielewicz-Mozajska H, Dabrowski L, Namiesnik J (2001) Accelerated Solvent Extraction (ASE) in the Analysis of Environmental Solid Samples — Some Aspects of Theory and Practice. Crit. Rev. Anal. Chem. 31(3): 149-165.
Willett KL, Ulrich EM, Hites RA (1998) Differential toxicity and environmental fates of hexachlorocyclohexane isomers. Environ Sci Technol 32: 2197–2207.
Haib J, Hofer I, Renand JM (2003) J. Chromatogr. A., 1020: 173-187.
Barriada-Pereira M, Concha-Grana E, Gonzalez-Castro MJ, Muniategui-Lorenzo S, Lopez-Mahia P, Prada-Rodriguez D, Fernandez-Fernandez E (2003) J. Chromatogr. A, 1008: 115-122.
M. Barriada-Pereira, M.J. Gonzalez-Castro, S. Muniategui-Lorenzo, P. LopezMahia, D. Prada-Rodriguez, E. Fernandez-Fernandez. 2005. Chemosphere, 58: 571- 1578.
K. Vorkamp, J.H. Christensen, M. Glasius, F.F. Riget. 2004. Marine Pollut. Bull., 48: 111-121.
K.S. Kumar, K. Kannan, J.P. Giesy, S. Masunaga. 2002. Environ. Sci. Technol., 36: 2789-2796.
M.K. So, X. Zhaug, J.P. Giesy, C.N. Fung, H.W. Fong, J. Zheng, M.J. Kramer, H. Yoo, P.K.S. Lam. 2005. Mar. Pollut. Bull., 51: 677-687.
S. Jayaraman, R.J. Pruell, R. Mc Kinney. 2001. Chemosphere 44: 181-191.
C. Nerin, R. Batle, M. Sartaguda, C. Pedrocchi. 2002. Anal. Chim. Acta, 464: 303- 312.
J. Hong, H.-Y. Kim, D.-G. Kim, J. Seo, K.-J. Kim. 2004. J. Chromatogr. A, 1038: 27-35.
J. Meadows, D. Tillitt, J. Huckins, D. Schroeder. 1993. Chemosphere 11: 1993-2006.
Internet Website:
B.E. Richter, B.A. Jones, J.L. Ezzell, N.L. Porter, N. Avdalovic, C. Pohl. 1996. Anal. Chem. 68: 1033.
J. Saulo, M. Abalos, E. Abad, J. Perera, M.G. Martrat, M.A. Adrados, J.R. Austrui, K. Martinez, J. Revera. 2005. Mass Spectromerty Lab., Dept of Ecotechnologies, IIQAB-CSIC C/Jordi Girona,.
18: 08034, Spain. 18. M. Numata, T. Yarita, Y. Aoyagi, Y. Tsuda, M. Yamazaki, A. Takatsu, K. Ishikawa, K. Chiba, K. Okamaoto. 2007. Anal. Bioanal. Chem. 387: 2313-2323.
J.J. Ramos, C. Dietz, M.J. Gonzalez, L. Ramos. 2007. J. Chromatogr. A. 1152: 254- 261..
U.N. Fidalgo, G.E. Blanco, M.A. Sanz. 2007. Anal Chim Acta 590: 1-16.
Z. Zhang, E. Ohiozebau, S.M. Rhind. 2011. J. Chromatogr. A, 1218: 1203-1209.
P. Suchan, J. Pulkrabova, J. Hajslova, V. Kocourek. 2004. Anal. Chim. Acta. 520: 193-200.
M.I.H. Helaleh, A. Al-Rashdan. 2012. J. Environ. Protect. accepted for publication.
Helaleh MIH, Al-Rashdan A, Ibtisam A (2012) Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power Prep™ clean-up. Talanta, 94: 44-49.
Yang N, Matsuda M, Kawano M, Wakimoto T (2006) PCBs and organochlorine pesticides (OCPs) in edible fish and shellfish from China. Chemosphere 63(8): 1342- 1352.
Jie F, Kai-Xiong W (2007) Multiresidual Analysis of Organochlorine Pesticides, Polychlorinated Biphenyls and Polycyclic Aromatic Hydrocarbons in Marine Shellfishes by Gas Chromatography-Ion Trap Mass Spectrometry. Chin. J. Anal. Chem. 35(11): 1607-1613.