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Polychlorinated biphenyls (PCBs), a group of persistent organic pollutants, are ubiquitous in the environment. The concentrations of PCBs and their metabolites are crucial to understand their impact on the environment. Here, a simultaneous method is reported to determine PCB101 and its hydroxylated, methoxylated and methyl sulfonated metabolites in aquatic organisms by gas chromatography–microelectron capture detection (GC-μECD). Several operational parameters, including the extraction solvent, volume of concentrated sulfuric acid for lipid removal, elution procedure, and solid-phase extraction (SPE) eluent volume, were optimized for the analytes in the muscle tissue of carp ( Carassius auratus ). Under the optimum conditions, the linearity of the method was from 2.5 to 100 ng/mL with correlation coefficients ( R2 ) &gt; 0.9961. The limit of detection was 2.00 μg/kg, and the limit of quantitation was equal to 5.00 μg/kg. The spiked recoveries of the targets in carp muscles were from 84.4% to 104%, and the relative standard deviation (RSD) was from 4.02% to 8.75%. The developed method was successfully applied to different aquatic samples. The precursor and metabolites were simultaneously detected in aquatic products. The metabolites of PCBs were present in marine samples collected from the East China Sea. For the first time, the methoxylated metabolite of PCB101 was identified in aquatic organisms. The results provide support for further study on the environmental properties and biological transmission of PCBs.

analytical letters

Simultaneous Determination of Polychlorinated Biphenyl 101 (PCB101) and Its Hydroxylated, Methoxylated and Methyl Sulfonated Metabolites in Aquatic Organisms by Solid-Phase Extraction (SPE) and Gas Chromatography–Microelectron Capture Detection (GC-μECD)