Optimisation of procedure for determination of polycyclic aromatic hydrocarbons and their derivatives in fish tissue; estimation of measurements uncertainty

Marie Janska (1) , Monika Tomaniova (2) , Jana Hajslova (2) , Vladimir Kocourek (3)

1 Food Chemistry and Analysis
2 Food Chemistry and Analysis
3 Food Chemistry and Analysis

Three alternative procedures were employed for 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: (i) Soxhlet extraction, (ii) batch extraction enhanced by sonication and (iii) saponification of sample followed by reextraction of analytes into hexane. Soxhlet extraction using hexane-acetone (1:1, v/v) was found as the most efficient extraction technique, with analyte recoveries in the range 70-108%. Within optimisation of 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 found as the most appropriate for purifying of crude extracts prior to 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 employing two alternative approaches. Both provided similar results: the expanded uncertainties obtained for individual PAHs by “top-down” approach were in the range 9-53 %, their values resulting from application of “bottom-up” were in the range 16-52 %.

Mots clés: Life Sciences

Marie Janska, Monika Tomaniova, Jana Hajslova, Vladimir Kocourek. Optimisation of procedure for determination of polycyclic aromatic hydrocarbons and their derivatives in fish tissue; estimation of measurements uncertainty. Food Additives and Contaminants, 2006, 23 (03), pp.309. ⟨10.1080/02652030500401207⟩. ⟨hal-00577567⟩