The Development of an Automated Clean-up for Fat Extracts in the Routine Analysis of Organochlorine Compounds in Fish Meat

Ana Andreea CIOCA, Olaf HEEMKEN, Marian MIHAIU


The present work describes the development of a new, automatic High Performance Liquid Chromatography (HPLC) Clean-up step, in the methodology of sample preparation and multi-residue determination of organochlorine compounds (OCs) in fish meat. 24 OCs were taken into study. In addition 7 Polychlorinated Biphenyls (PCBs), 7 chlorobenzene compounds and one 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) were investigated. The HPLC conditions were established in accordance with the validated traditional Clean-up step of the laboratory. The technique was applied on a dilution of analytes of interest in order to establish the period of time in which the compounds are eluted. Another set of experiments involved fish oil, in order to identify and separate the fat fraction from the analytes. To confirm the findings of the experiments mentioned above, extracts of fish samples obtained after Accelerated Solvent Extraction (ASE) were examined. The samples were spiked with the analytes of interest before HPLC clean-up step and quantified through Gas Chromatography coupled with tandem Mass Spectrometry (GC-MS/MS). A HPLC clean-up technique lasting 38 minutes/sample was developed. The method is not suitable for OCs such as Endosulfansulfat and Endrine Ketone due to the very low recovery results. 


High Performance Liquid Chromatography Clean-up, fish, organochlorine compounds

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