Optimization of the procedure for the determination of polycyclic aromatic hydrocarbons and their derivatives in fish tissue: Estimation of measurements uncertainty

Authors: Jánská, M.; Tomaniová, M.; Hajšlová, J.; Kocourek, V.

Source: Food Additives and Contaminants, Volume 23, Number 3, March 2006 , pp. 309-325(17)

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Abstract:

Three alternative procedures were employed for the isolation of polycyclic aromatic hydrocarbons (PAHs; 15 of 16 US EPA priority pollutants and benzo[ e ]pyrene), their methyl-derivatives and sulphur analogues from fish tissue: (1) Soxhlet extraction, (2) batch extraction enhanced by sonication, and (3) saponification of the sample followed by re-extraction of analytes into hexane. Soxhlet extraction using hexane-acetone (1:1, v/v) was the most efficient extraction technique, with analyte recoveries in the range 70–108%. Within optimization of the clean-up step, several types of gel permeation chromatography (GPC) systems were tested: two types of polystyrene divinylbenzene copolymer gels (PSDVB), both `soft' gel type (Bio-Beads S-X3) and `rigid' gels type (PL gel and Envirogel) in combination with various mobile phases were compared. Bio-Beads S-X3 and mobile phase chloroform were the most appropriate for purifying of crude extracts before the final determinative step. High-performance liquid chromatography with fluorimetric detection (HPLC/FLD) was used for identification and quantification of PAHs in purified fish extracts. The uncertainties of PAHs measurements were estimated by employing two alternative approaches. Both provided similar results: the expanded uncertainties obtained for individual PAHs by the `top–down' approach were in the range 9–53%, their values resulting from application of the `bottom–up' approach were in the range 16–52%.

Keywords: Polycyclic aromatic hydrocarbons (PAHs); uncertainty; clean-up; gel permeation chromatography (GPC); extraction; fish tissue

Document Type: Research article

DOI: http://dx.doi.org/10.1080/02652030500401207

Affiliations: 1: Technická 3, Institute of Chemical Technology, Prague, Czech Republic

Publication date: 2006-03-01

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