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

Abstract

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 OCswere 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 throughGas Chromatography coupled with tandem Mass Spectrometry (GC-MS/MS). A HPLC clean-up technique lasting 38 minutes/ sample was developed. The method is not suitablefor OCs such as Endosulfansulfat and Endrine Ketonedue to the very low recovery results.

Methodologies and Results Concerning the Determination of Ocs And Pcbs From Fish Meat

“…A daring approach among the purification techniques is the development of an automated high pressure liquid chromatography (HPLC) clean-up for OCs and PCBs (Cioca et al, 2017b). The overall technique is still to be optimized from the perspectives of analyte recovery, reduction of process time and solvent consumption.…”