Analysis of PCBs in soils and sediments by microwave-assisted extraction,headspace-SPME and high resolution gas chromatography with ion-trap tandem mass spectrometry |
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Authors: | Paulo Herbert Simone Morais Paula Paíga Arminda Alves Lúcia Santos |
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Institution: | 1. LEPAE—Laboratory of Process , Environment and Energy Engineering. Engineering Faculty , University of Porto , Rua Dr. Roberto Frias, 4200-465 Porto, Portugal;2. Requimte/Instituto Superior de Engenharia do Instituto Politécnico do Porto, Departamento de Engenharia Química , Rua S. Tomé, 4200 Porto, Portugal |
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Abstract: | A procedure for the determination of seven indicator PCBs in soils and sediments using microwave-assisted extraction (MAE) and headspace solid-phase microextraction (HS-SPME) prior to GC-MS/MS is described. Optimization of the HS-SPME was carried out for the most important parameters such as extraction time, sample volume and temperature. The adopted methodology has reduced consumption of organic solvents and analysis runtime. Under the optimized conditions, the method detection limit ranged from 0.6 to 1?ng/g when 5?g of sample was extracted, the precision on real samples ranged from 4 to 21% and the recovery from 69 to 104%. The proposed method, which included the analysis of a certified reference material in its validation procedure, can be extended to several other PCBs and used in the monitoring of soil or sediments for the presence of PCBs. |
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Keywords: | Microwave-assisted extraction Solid-phase microextraction Polychlorinated biphenyls Soil Sediments |
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