Solid-phase extraction clean-up procedure for the analysis of PAHs in lichens

A clean-up procedure based on a solid-phase extraction column was optimized for determination of polycyclic aromatic hydrocarbons (PAHs) in lichen extracts to remove co-extracted compounds from the matrix in the final extract. Several kinds of solid phases were evaluated: normal phase (-NH2 and alumina), strong anion exchange and reversed phase. The -NH2 columns were the most effective by using a packed solid bed of 500 mg. The lichen raw extract was loaded on the column previously conditioned with dichloromethane and hexane. Hexane (0.5 mL) was used as rinsing solvent, and PAHs were quantitatively eluted (80-97%) using 2mL of hexane-dichloromethane (65-35) as eluting solvent. In these conditions, even the heaviest PAHs were quantitatively eluted. The optimized SPE method provides a short time and low-solvent-consumption sample clean-up compared with other conventional methods based on column chromatography. The analytical procedure, dynamic sonication-assisted extraction, followed by the optimized solid-phase extraction clean-up, was used to determine the 16 EPA priority PAHs from native lichens collected from the Aragon valley in central Pyrenees. The PAH concentrations in lichen samples ranged from 352 to 1654 ng g(-1), and the minimum concentration value was established as the regional reference PAH levels in the area.