Determination of organophosphorous flame retardants in fish tissues by matrix solid-phase dispersion and gas chromatography |
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Authors: | Luca Campone Anna Lisa Piccinelli Conny Östman Luca Rastrelli |
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Institution: | 1. Dipartimento di Scienze Farmaceutiche (DIFARMA), Università degli Studi di Salerno, Via Ponte Don Melillo, 84084, Fisciano (SA), Italy 2. Department of Analytical Chemistry, Stockholm University, 106 91, Stockholm, Sweden
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Abstract: | Organophosphate esters (OPEs), utilized as flame retarding agents and/or plasticizers, are almost ubiquitous in environmental
compartments, and biota and foods could be contaminated by bioaccumulation or during the treatment processes. A multiresidue
method is proposed for the determination of 13 OPEs in fish tissues: analytes were simultaneously extracted and purified using
the matrix solid phase dispersion technique and then determined by gas chromatography with nitrogen–phosphorus detection.
The main parameters affecting extraction yield and selectivity, such as the type of dispersant material, clean-up co-sorbent,
rinse and elution solvents, were evaluated to obtain lipid-free extracts and quantitative recoveries for OPEs. Under optimal
conditions, 0.5 g of samples was dispersed with 2 g Florisil and 1 g anhydrous sodium sulphate and transferred to a solid
phase extraction cartridge containing 1 g alumina. The lipids were removed using 5 mL n-hexane/dichloromethane (1:1) and analytes were recovered with 10 mL n-hexane/acetone (6:4) and directly analysed. The method developed provided recoveries between 70 and 110% for different kinds
of fish, and the day-to-day variability was between 1 and 9%. This procedure constitutes the first analytical method for the
analysis of OPEs in a food matrix and it is applicable to analyse a large number of samples to evaluate the occurrence and
sources of OPEs in biota and foods. |
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