Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power Prep™ clean-up

• Published in: Talanta (Oxford) 2012-05, Vol.94, p.44-49
• Main Authors: Helaleh, Murad I.H., Al-Rashdan, Amal, Ibtisam, A.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Animals; Applied sciences; Bivalvia - chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Gel; Clean-up system; Decapodiformes - chemistry; Environmental Pollutants - analysis; Exact sciences and technology; Fast analysis; Fishes; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry; Global environmental pollution; Hexanes - chemistry; Hydrocarbons, Chlorinated - analysis; Liquid-Liquid Extraction - methods; Marine sample; Methylene Chloride - chemistry; OCPs and PCBs; Octopodiformes - chemistry; Other chromatographic methods; Penaeidae - chemistry; Pesticides - analysis; Pollution; Polychlorinated Biphenyls - analysis; Pressure; Reproducibility of Results; Spectrometric and optical methods; Sulfates - chemistry
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2012.02.031

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 5g 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 (6g) supplied by Fluid Management Systems (FMS). All OCPs and PCBs were eluted from the silica column using two types of solvent: 80mL of hexane and a 50mL 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 1.38ngg−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 18.39ngg−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.