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

• Published in: Food additives and contaminants Vol. 23; no. 3; pp. 309 - 325
• Main Authors: Janska, M, Tomaniova, M, Hajslova, J, Kocourek, V
• Format: Journal Article
• Language: English
• Published: London Taylor & Francis Group 01.03.2006; Taylor & Francis
• Subjects: Animals; benzopyrene; Biological and medical sciences; Carcinogens, Environmental - analysis; Chloroform; Chromatography, Gel - methods; Chromatography, High Pressure Liquid - methods; clean-up; dynamic programming; estimation; extraction; fish; Fish and seafood industries; fish fillets; Fish Products - analysis; fish tissue; food analysis; Food Contamination - analysis; Food engineering; Food industries; Fundamental and applied biological sciences. Psychology; gel permeation chromatography; gel permeation chromatography (GPC); General aspects; Indicators and Reagents; Mutagens - analysis; Noxae - analysis; Perciformes; pollutants; pollution load; polycyclic aromatic hydrocarbons; Polycyclic aromatic hydrocarbons (PAHs); Polycyclic Aromatic Hydrocarbons - analysis; Polystyrenes; quantitative analysis; Solvents; Sonication; uncertainty; Measurement; fish tissue; Edible fish; gel permeation chromatography (GPC); Uncertainty; Polycyclic aromatic hydrocarbons (PAHs); Hydrocarbon; clean-up; Extraction; Polycyclic aromatic compound; Optimization; Gel permeation chromatography
• ISSN: 0265-203X; 1464-5122
• DOI: 10.1080/02652030500401207

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%.