title: Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power Prep™ clean-up.
abstract: An automated pressurized liquid extraction (PLE) method followed by Power Prep™ clean-up was developed for organochlorinated pesticide (OCP) and polychlorinated biphenyl (PCB) analysis in environmental marine samples of fish, squid, bivalves, shells, octopus and shrimp. OCPs and PCBs were simultaneously determined in a single chromatographic run using gas chromatography-mass spectrometry-negative chemical ionization (GC-MS-NCI). About 5 g of each biological marine sample was mixed with anhydrous sodium sulphate and placed in the extraction cell of the PLE system. PLE is controlled by means of a PC using DMS 6000 software. Purification of the extract was accomplished using automated Power Prep™ clean-up with a pre-packed disposable silica column (6 g) supplied by Fluid Management Systems (FMS). All OCPs and PCBs were eluted from the silica column using two types of solvent: 80 mL of hexane and a 50 mL mixture of hexane and dichloromethane (1:1). A wide variety of fish and shellfish were collected from the fish market and analyzed using this method. The total PCB concentrations were 2.53, 0.25, 0.24, 0.24, 0.17 and 1.38 ng g(-1) (w/w) for fish, squid, bivalves, shells, octopus and shrimp, respectively, and the corresponding total OCP concentrations were 30.47, 2.86, 0.92, 10.72, 5.13 and 18.39 ng g(-1) (w/w). Lipids were removed using an SX-3 Bio-Beads gel permeation chromatography (GPC) column. Analytical criteria such as recovery, reproducibility and repeatability were evaluated through a range of biological matrices.
authors.affiliation: Kuwait Institute for Scientific Research (KISR), Central Analytical Laboratory (CAL), Chromatography Section, P.O. Box 24885, Safat 13109, Kuwait. murad.helaleh@lycos.com
authors.forename: Murad I H
authors.initials: MI
authors.lastname: Helaleh
authors.forename: Amal
authors.initials: A
authors.lastname: Al-Rashdan
authors.forename: A
authors.initials: A
authors.lastname: Ibtisam
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry; D002850:Chromatography, Gel; D049832:Decapodiformes / Q000737:chemistry; D004785:Environmental Pollutants / Q000032:analysis*; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry; D006586:Hexanes / Q000737:chemistry; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D059625:Liquid-Liquid Extraction / Q000379:methods*; D008752:Methylene Chloride / Q000737:chemistry; D049831:Octopodiformes / Q000737:chemistry; D033561:Penaeidae / Q000737:chemistry; D010575:Pesticides / Q000032:analysis*; D011078:Polychlorinated Biphenyls / Q000032:analysis*; D011312:Pressure; D015203:Reproducibility of Results; D013431:Sulfates / Q000737:chemistry
chemical_list: D004785:Environmental Pollutants; D006586:Hexanes; D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D013431:Sulfates; C012036:sodium sulfate; D008752:Methylene Chloride; D011078:Polychlorinated Biphenyls