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Simon, R; Palme, S; Anklam, E
Journal of AOAC International, 05/2006, Volume: 89, Issue: 3Journal Article
A collaborative study was conducted to validate an analytical method for quantification of the 15 polycyclic aromatic hydrocarbons (PAHs) regarded in 2002 as a health concern by the former Scientific Committee on Food of the European Commission (SCF) in primary smoke condensates. The method is based on gas chromatography/mass spectrometry of a cyclohexane extract with solid-phase cleanup through silica gel. The analytes were detected in the selected-ion monitoring mode and quantified by using 3 isotopically labeled internal standard compounds. Seventeen laboratories participated in the collaborative validation study, of which 12 reported valid results. The data were subjected to Cochran, single Grubbs, and double Grubbs tests for statistical outliers. A maximum of 2 outliers was eliminated before further statistical evaluation of the method performance characteristics. Depending on the analyte, the results showed relative standard deviations for repeatability between 4.2 and 30% and for reproducibility from 9.9 to 60%. The recoveries varied between about 50 and 85%, except those for cyclopentacdpyrene, dibenzoa,ipyrene, and dibenzoa,hpyrene. Nevertheless, because Commission Directive 2005/10/EC allows for a recovery range of 50-120% for (BaP) benzoapyrene in various foods, it can be concluded that the method performs appropriately within the analytical range between 5 and 25 microgram/kg of primary smoke condensate. For BaP the validated analytical range covered 5-20 microgram/kg, and for benzoaanthracene (BaA) 10-25 microgram/kg. The method is suitable for monitoring BaP and BaA at their respective maximum permitted levels of 10 and 20 microgram/kg. Three analytes, benzob-, benzoj-, and benzok-fluoranthene could not be separated by all of the participants and were therefore treated as the sum. Nevertheless, with this method the pattern of the respective concentrations of these 15 PAHs can be monitored in primary smoke condensate as suggested by the SCF.
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