A Selective Gas Chromatography-Selected Ion Monitoring Mass Spectrometry (GC‑MS/SIM) Method to Determine Polychlorinated Biphenyls in Fuller's Earth

Abstract

Polychlorinated biphenyls (PCBs) are carcinogenic to humans and can be found in Fuller's earth used for the regeneration of used transformer oil. This work describes a highly selective gas chromatographic-selected ion monitoring mass spectrometric method (GC-MS/SIM) for the simultaneous determination of three Aroclor PCB congener mixtures (1242, 1254, and 1260). The separation of the PCBs could be systematically varied by changing the temperature conditions of the chromatographic column. Methods were first selected from the literature, and the resolution of the PCBs was then optimized by adjusting k* (effective retention), α (selectivity), and N (column efficiency), enabling the detection of 83 PCBs in 35 min. The extract of PCBs from Fuller's earth was obtained by ultrasonication (employing hexane and acetone as solvents) and cleanup with Florisil and was concentrated to about 500 µL. The ions analyzed in SIM mode were divided into groups according to the similarity (m/z) of the PCB fragmentation profiles. The limits of detection (LOD) and quantification (LOQ) were 0.19 and 0.64 µg kg-1 , respectively. The method developed was used to determine the PCBs present in Fuller's earth provided by an electric power company. The mean total PCBs concentration was found 1.9 µg kg-1 in Fuller's earth.