Validation of an Analytical Procedure for Selected Polychlorinated Biphenyls Determination in Sediment Samples
K. Szyrwinska, J. Lulek
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Department of Inorganic and Analytical Chemistry, Poznań University of Medical Sciences,
Grunwaldzka 6, 60-780 Poznań, Poland
Pol. J. Environ. Stud. 2006;15(4):593-602
This paper describes the method for determining 15 individual polychlorinated biphenyls in sediments, using fexIKA extraction. The analytical procedure included extraction and clean-up of extracts with concentrated sulfuric acid and solid phase extraction (SPE) on Florisil. The identification and quantification of analytes were carried out by capillary gas chromatography (GC) with electron capture detector (ECD) and/or low resolution mass spectrometry (LRMS). The method detection and quantification limits varied from 0.06 to 0.12 and from 0.2 to 0.4 ng/g dry weight, respectively. the relative standard deviations in repeatability and intra-laboratory reproducibility studies varied from 3.2 to 11.2%. recoveries of analytes from spiked sediment samples were between 74.0% and 108.8%. the method was linear and characterized by good correlation coefficients (>0.99) for all compounds studied. The quality of the method under validation was verified by the analysis of certified reference material and by participation in an interlaboratory exercise.
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