Sensitive GC/MS determination of 15 isomers of chlorobenzoic acids in accelerated solvent extracts of soils historically contaminated with PCBs and validation of the entire method

0440241 - MBÚ 2015 RIV CH eng J - Článek v odborném periodiku
Křesinová, Zdena - Hostačná, Lucie - Medková, Jaroslava - Čvančarová, Monika - Stella, Tatiana - Cajthaml, Tomáš
Sensitive GC/MS determination of 15 isomers of chlorobenzoic acids in accelerated solvent extracts of soils historically contaminated with PCBs and validation of the entire method.
International Journal of Environmental Analytical Chemistry. Roč. 94, č. 8 (2014), s. 822-836. ISSN 0306-7319. E-ISSN 1029-0397
Grant CEP: GA ČR(CZ) 13-28283S; GA TA ČR TE01020218
Institucionální podpora: RVO:61388971
Klíčová slova: chlorobenzoic acid * GC/MS * separation * PCB * contamination
Kód oboru RIV: CB - Analytická chemie, separace
Impakt faktor: 1.295, rok: 2014

Chlorobenzoic acids (CBAs) are the major metabolite of aerobic bacterial degradation of polychlorinated biphenyls (PCBs). A rapid and simple simultaneous derivatisation method has been developed for gas chromatography-mass spectrometry determination in historically PCB-contaminated soils for 15 isomers of mono-, di-, tri-, tetra-, and pentachlorobenzoic acids in CBA mixtures. Two derivatisation agents (diazomethane and methyl chloroformate) and various conditions were evaluated (temperature, time, solvents, catalysts) in terms of efficiency. The optimised derivatisation method with diazomethane and 1% methanol running 1 hour at 5 degrees C was used for derivatisation of extracts of soils and river sediment from historically PCB-contaminated sites; the extracts were prepared using accelerated solvent extraction by a previously described method. Methylated CBAs were separated by gas chromatography using a system with two different common columns, DB-5 and DB-200, in series-coupled (tandem) arrangement and detected by EI-MS. A clean-up with a gel permeation chromatography was carried out to remove soil interfering matrix compounds as well as major portion of PCBs. The limits of quantification ranged between 1 and 10ngg(-1) of individual CBA in the soil. The procedure was applied to various soil samples from Lhenice (Czech Republic) highly contaminated with PCBs. CBAs were found in all tested soils and also in the river sediment. The most contaminated soil contained all CBAs representatives under the study with a total concentration of 3.1 mu gg(-1) of dry soil.
Trvalý link: http://hdl.handle.net/11104/0243357