The olive oil sector is experiencing significant growth, driven by the global appreciation of olive oil as a high-nutritional food. However, its industrial production generates large amounts of by-products, including olive pomace (OP)—mainly water, pulp, and seeds—and olive oil mill wastewater (OOMW), a dark liquid rich in organic carbon, especially phenolic and polyphenolic compounds. These residues, if not properly treated, may pose environmental hazards due to their phytotoxic and antimicrobial properties. On the other hand, they are rich in bioactive compounds with antioxidant potential, making them valuable for creating eco-sustainable and economically beneficial co-products. Established chromatographic methods are typically optimized for either polyphenolic or lipophenolic compounds, reflecting their distinct solubility properties and chemical structures [1,2]. Indeed, their simultaneous determination is analytically demanding, especially when selecting solvents compatible with both solubilization processes and chromatographic eluents. In this study, a comprehensive determination of (lipo)phenolic compounds in olive oil by-products was conducted using a UHPLC-LTQ Orbitrap XL HRMS system with a heated electrospray ionization (HESI) source. A dual-injection single-run approach was applied, integrating an on-line focusing step for trapping lipophenols, followed by injection of polyphenols. Then, the method involves two consecutive injections combined into a single run using a binary gradient program, enabling efficient separation of phenolic and (lipo)phenolic compounds with high-throughput workflows. A baseline separation of the target analytes was obtained in less than 25 min. Overall, the analysis requires a total time of 34 min, including the step of column conditioning for the next run. Finally, the method was applied for both targeted and untargeted profiling of OP, OOMW, and leaves from three Olea europaea cultivars. [1] R. Moreno-González, M.E. Juan, J.M. Planas. Journal of Chromatography A 1609 (2020) 460434. [2] C. Benincasa, C. La Torre, A. Fazio, E. Perri, M.C. Caroleo, P. Plastina, E. Cione. Antioxidants 10 (2021) 1051.
Simultaneous determination of (lipo)phenolic compounds in olive oil by-products by dual-injection single-run LC-MSMS analysis
Wadir Mario Valentino Marchesiello;Donatella Nardiello
;Maurizio Quinto;
2025-01-01
Abstract
The olive oil sector is experiencing significant growth, driven by the global appreciation of olive oil as a high-nutritional food. However, its industrial production generates large amounts of by-products, including olive pomace (OP)—mainly water, pulp, and seeds—and olive oil mill wastewater (OOMW), a dark liquid rich in organic carbon, especially phenolic and polyphenolic compounds. These residues, if not properly treated, may pose environmental hazards due to their phytotoxic and antimicrobial properties. On the other hand, they are rich in bioactive compounds with antioxidant potential, making them valuable for creating eco-sustainable and economically beneficial co-products. Established chromatographic methods are typically optimized for either polyphenolic or lipophenolic compounds, reflecting their distinct solubility properties and chemical structures [1,2]. Indeed, their simultaneous determination is analytically demanding, especially when selecting solvents compatible with both solubilization processes and chromatographic eluents. In this study, a comprehensive determination of (lipo)phenolic compounds in olive oil by-products was conducted using a UHPLC-LTQ Orbitrap XL HRMS system with a heated electrospray ionization (HESI) source. A dual-injection single-run approach was applied, integrating an on-line focusing step for trapping lipophenols, followed by injection of polyphenols. Then, the method involves two consecutive injections combined into a single run using a binary gradient program, enabling efficient separation of phenolic and (lipo)phenolic compounds with high-throughput workflows. A baseline separation of the target analytes was obtained in less than 25 min. Overall, the analysis requires a total time of 34 min, including the step of column conditioning for the next run. Finally, the method was applied for both targeted and untargeted profiling of OP, OOMW, and leaves from three Olea europaea cultivars. [1] R. Moreno-González, M.E. Juan, J.M. Planas. Journal of Chromatography A 1609 (2020) 460434. [2] C. Benincasa, C. La Torre, A. Fazio, E. Perri, M.C. Caroleo, P. Plastina, E. Cione. Antioxidants 10 (2021) 1051.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
