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Abstract :
[en] Within the lipids, the sterol fraction is considered the fingerprint of the the botanical origin, thus they are used for detecting potential adulteration , particularly in extra virgin olive oil. The official analytical method for their determination includes a saponification step, liquid-liquid extraction, and subsequent purification using thin-layer chromatography (TLC), derivatization of the fraction of interest, and chromatographic analysis on monodimensional gas chromatography coupled with flame ionization detector (GC-FID).
Despite its effectiveness, this approach is time-intensive, requiring approximately eight hours, substantial solvent volumes, and extensive manual handling. These factors not only limit its efficiency when processing large sample quantities but also raise concerns regarding environmental sustainability, conflicting with the principles of green analytical chemistry. Recent advancements, including the methods proposed by Gorassini [1] and Mascrez [2], have reduced analysis times to 4 and 3 hours, respectively, by replacing traditional thin-layer chromatography (TLC) with solid-phase extraction (SPE) and incorporating microwave-assisted saponification (MAS).
The analytical method developed in this research aims to further streamline the process by introducing automation, minimizing solvent use, and reducing waste . Specifically, the saponification and liquid-liquid extraction steps, performed separately in previous methods, were combined using a microwave-assisted saponification and extraction (MASE) approach. The purification step was optimized starting from the SPE methods proposed by Gorassini and Mascrez, with modifications to reduce organic solvent volumes and improve the greenness of the method.
Overall, the proposed method proved faster, simpler, and greener, reducing analysis time from 8 to approximately 2 hours. In summary, the proposed method simplifies sterol analysis while maintaining accuracy comparable to the official method.
