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Abstract
The chromatographic determination of 15 polycyclic aromatic hydrocarbons (PAHs) in cookies has been improved in order to obtain a fast method with a low limit of detection through the combination of microwave-assisted extraction (MAE), oil saponification and solid-phase extraction clean-up before the injection of purified extracts in a C18 201TP52 (5 µm, 250 × 2.1 mm) column. Using acetonitrile–water as mobile phase, with a 50% to 95% w/w acetonitrile gradient for a fixed flow of 0.250 ml min−1, 15 PAHs were separated in 45 min. The column temperature was maintained at 15°C; and fluorimetric detection was made at a fixed excitation wavelength of 264 nm and emission measurements at the best wavelength for each analyte, from 352 nm for 11H-benzo[b]fluorene to 500 nm for indeno[1,2,3-c,d]pyrene. Recoveries for all 15 PAHs varied between 96 ± 4 and 105% ± 4%; and the limits of detection ranged from 0.015 ng g−1 for chrysene to 0.7 ng g−1 for phenantrene. Results were compared with those obtained by conventional Soxhlet extraction during 8-h refluxing with toluene, demonstrating that the methodology proposed is appropriate to quantify PAHs in cookies. Furthermore, the microwave-assisted method was faster and used less solvent than the conventional and ultrasound-assisted methods. The extraction time was reduced to 9 min compared with the 8 h required for Soxhlet extraction and 60 min required for ultrasound-assisted treatment, and the solvent consumption has been reduced to 25 ml compared with the 155 and 90 ml required using Soxhlet and ultrasound, respectively.
Acknowledgements
The authors acknowledge the financial support of the Laboratorio de Higiene Laboral y Ambiental of the University of Valencia.