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Miniaturised selective pressurised liquid extraction of polychlorinated biphenyls from foodstuffs

journal contribution
posted on 2023-05-17, 18:06 authored by Ramos, J, Christian DietzChristian Dietz, Gonzalez, M, Ramos, L
The feasibility of miniaturised pressurised liquid extraction (PLE) with in-cell purification and subsequent gas chromatography with microelectron capture detection (GC–micro-ECD) for the determination of prioritary and toxic polychlorinated biphenyls (PCBs) in a variety of foodstuffs (fat contents in the range 22–49%, w/w, on a freeze-dried basis) has been investigated. After optimisation of the several experimental parameters affecting the efficiency of the selective PLE process, the developed method provided quantitative recoveries of the endogenous PCBs studied and complete fat elimination in a single step using n-hexane as extraction solvent. A total solvent volume of 3.5mL was used for the two consecutive 7 min static PLEs of 100-mg samples. Detection limits using GC–micro-ECD were below 0.2 ng/g freeze dried sample for all 22 PCBs investigated in real-life foodstuffs, and the repeatability of the complete PLE plus GC–micro-ECD method as calculated for the analysis of the endogenous PCBs in general was better than 14%. Comparison of the miniaturised PLE method developed with either conventional Soxhlet extraction or matrix solid phase dispersion with subsequent (off-line) clean-up for the analysis of non-spiked samples showed that the efficiency of PLE was similar to or better (recoveries in the range 83–133%, as calculated for the endogenous analytes) than for the other two extraction methods assayed.

History

Publication title

The Journal of Chromatography A

Volume

1152

Pagination

254-261

ISSN

0021-9673

Publisher

Elsevier Science Bv

Place of publication

Po Box 211, Amsterdam, Netherlands, 1000 Ae

Rights statement

Copyright 2006 Elsevier B.V

Repository Status

  • Restricted

Socio-economic Objectives

Diagnosis of human diseases and conditions

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