Analysis of persistent organic pollutants in marine sediments using a novel microwave assisted solvent extraction and liquid-phase microextraction technique

A simple and novel analytical method for quantifying persistent organic pollutants (POPs) in marine sediments has been developed using microwave assisted solvent extraction (MASE) and liquid-phase microextraction (LPME) using hollow fibre membrane (fIFM). POPs studied included twelve organochlorine pesticides (OCP) and eight polychlorinated biphenyl (PCB) congeners. MASE was used for the extraction of POPs from 1g of sediment using 10 ml of ultrapure water at 600 W for 20 min at 80 degrees C. The extract was subsequently subjected to a single step LPME-HFM cleanup and enrichment procedure. Recovery varied between 73 and 111% for OCPs; and 86-110% for PCBs, and exceeded levels achieved for conventional multi-step Soxhlet extraction coupled with solid-phase extraction. The method detection limit for each POP analyte ranged from 0.07 to 0.70 ng g(-1), and peak areas were proportional to analyte concentrations in the range of 5-500 ng g(-1). Relative standard deviations of less than 20% was obtained, based on triplicate sample analysis. The optimized technique was successfully applied to POP analysis of marine sediments collected from the northeastern and southwestern areas of Singapore's coastal environment. (c) 2005 Elsevier B.V. All rights reserved.