Single-laboratory Validation of a Gas Chromatography-mass Spectrometry Method for Quantitation of 15 European Priority Polycyclic Aromatic Hydrocarbons in Spiked Smoke Flavourings
2006 | 2007
SIMON Rupert | PALME Sonja | ANKLAM Elke
A method was developed and validated in-house according to the IUPAC harmonised guideline for the determination of 15 carcinogenic and mutagenic polycyclic aromatic hydrocarbons in primary smoke condensates that are used in food products. The method was based on gas chromatography with mass spectrometric detection. Sample preparation consisted of alkaline saponification, liquid/liquid extraction with cyclohexane, and solid phase clean-up with silica gel. Limits of detection (LOD) varied between 0.1 and 1.3 µg/kg, limits of quantification (LOQ) between 0.5 and 4 µg/kg for the various PAHs in primary smoke condensate (PSC). The coefficient of variance of the repeatability was between 0.7% (benzo(a)pyrene) and 30% (dibenzo(a,h)pyrene) relative standard deviation, depending on the analyte. The recoveries varied between 100-102% (dibenzo(a,l)pyrene) and 69-83% (dibenzo(a,h)pyrene) over the analytical range of 5-35 µg/kg.
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