Optimizing the Extraction and Clean-up Step for Determination of Polycyclic Aromatic Hydrocarbons in Malt Using HPLC-FLD

This study presents an optimization and validation of a new method for the determination of 12 polycyclic aromatic hydrocarbons (PAHs) in barley malt samples. The sample preparation operates on the principle of a Quick, Easy, Cheap, Efficient, Rugged, and Safe (QuEChERS) extraction method. Lipidic compounds are then frozen out and finally cleared away by an additional dSPE clean-up. For this reason, the mixture of primary secondary amine (PSA) and zirconium dioxide–based sorbent (Z-Sep) granted the most efficient choice. A comparison with a more conventional extraction method and agreement with the EC Regulations confirmed the aptness of our new method. The comparison and validation were carried out using a spiked malt sample. The recoveries ranged from 84 to 134% and LOQs from 0.3 to 0.7 µg/kg. The analysis alone was performed by HPLC with fluorescence detection. This approach provides not only satisfactory results but also an opportunity to prepare more samples at once in a relatively short time.