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

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• 作者：Murad I.H. Helaleh ; ^{murad.helaleh@lycos.com} ; Amal Al-Rashdan ; A. Ibtisam
• 关键词：Fast analysis ; Marine sample ; Clean-up system ; OCPs and PCBs
• 刊名：Talanta
• 出版年：2012
• 期刊代码：106_00399140
• 类别：ch
• 出版时间：30 May, 2012
• 卷：94
• 期：Complete
• 页码：44-49
• 文件大小：306 K

摘要

An automated pressurized liquid extraction (PLE) method followed by Power Prep鈩?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鈩?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^鈭? (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^鈭? (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.