Analysis of PCBs in soils and sediments by microwave-assisted extraction, headspace-SPME and high resolution gas chromatography with ion-trap tandem mass spectrometry

摘要

A procedure for the determination of seven indicator PCBs in soils and sediments usingmicrowave-assisted extraction (MAE) and headspace solid-phase microextraction(HS-SPME) prior to GC-MS/MS is described. Optimization of the HS-SPME was carriedout for the most important parameters such as extraction time, sample volume andtemperature. The adopted methodology has reduced consumption of organic solvents andanalysis runtime. Under the optimized conditions, the method detection limit ranged from0.6 to 1 ng/g when 5 g of sample was extracted, the precision on real samples ranged from4 to 21% and the recovery from 69 to 104%. The proposed method, which included theanalysis of a certified reference material in its validation procedure, can be extendedto several other PCBs and used in the monitoring of soil or sediments for the presenceof PCBs.