Rapid determination of benzo(a)pyrene in olive oil samples with solid-phase extraction and low-pressure, wide-bore gas chromatography-mass spectrometry and fast liquid chromatography with fluorescence detection

Benzo(a)pyrene (13(a)P) was extracted from olive oil using solid-phase extraction on columns filled with Florisil and Nucleoprep C18. The extracts were analyzed with GC-MS, using standard capillary column and low-pressure wide-bore column (LP-GC-MS), as well as with HPLC on standard column and short donor-acceptor complex chromatography (DACC) column. Quantitation was done with isotope dilution method (GC-MS and LP-GC-MS) or with internal standard benzo(k)fluoranthene (HPLC). Limits of detection were 1 ng/g for GC-MS on standard column, 1.6 ng/g on LP-column, 0.5 ng/g for HPLC on standard column, and 0.3 ng/g on DACC column, respectively. The applied extraction method allowed handling over 50 samples per day and assured recovery over 80%. Matrix solid-phase dispersion, tried as an alternative isolation method, appeared less advantageous. Fast chromatographic methods (LP-GC-MS and HPLC on DACC) made it possible to reduce analysis time to 8 and 5 min, respectively. The method was applied to routine analysis of B(a)P in olive oil samples. (C) 2003 Elsevier B.V. All rights reserved.