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Determination of Polycyclic Aromatic Hydrocarbons in Extra Virgin Olive Oils via Cryogenic Zone Compression GC-MS Analysis
* 1 , 2 , 3 , 3, 4
1  Department of Mathematical and Computer Science, Physical Sciences and Earth Sciences, University of Messina, Messina, Italy
2  Chromaleont s.r.l., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, former Veterinary School, University of Messina, Messina, Italy
3  Messina Institute of Technology c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy
4  Chromaleont s.r.l., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy
Academic Editor: Nuno R. Neng

Abstract:

The present study is based on the development of a straightforward method for the determination (semi-quantification) of 16 polycyclic aromatic hydrocarbons in extra virgin olive oil using "cryogenic-zonecompression" gas chromatography–single quadrupole mass spectrometry. By employing the "cryogenic-zonecompression" approach, the method significantly enhances signal-to-noise ratios, on average by 14 times, allowing for a streamlined sample preparation that requires only a single extraction with 500 μL of acetonitrile, without any step of clean-up or concentration. This approach aligns with green analytical chemistry principles by reducing solvent use and procedural complexity.

The method demonstrated quantification limits ranging from 0.07 to 8.33 μg kg-1. Accuracy at concentration levels of 2 and 10 μg kg-1 ranged from 82% to 103%, while intra-day and inter-day precision were between 1.9 and 14.7% and 5.9 and 9.1%, respectively. Recovery rates at 10 μg kg-1 varied widely from 24% to 99%, and a positive matrix effect was observed for all PAHs analyzed. Among the ten EVOO samples tested, two PAHs were detected in six samples, with no more than one PAH per sample.

ACKNOWLEDGMENTS

The authors acknowledge the Shimadzu Corporation and Merck Life Science for their support. Funding: This research was supported by the Ministry University and Research within project PRIN 2022 PNRR titled “gReen analytical methods for PAHs detection in EVOO: from lABoratory to smart LabEl (RELIABLE)”, Prot. P2022842MJ, CUP J53D23014520001.

Keywords: Polycyclic aromatic hydrocarbons, extra virgin olive oil, gas chromatography, mass spectrometry, green sample preparation.
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