Extraction and Mass Spectrometric Characterization of Terpenes Recovered from Olive Leaves Using a New Adsorbent-Assisted Supercritical CO2 Process.

This work reports the use of GC-QTOF-MS to obtain a deep characterization of terpenoid compounds recovered from olive leaves, which is one of the largest by-products generated by the olive oil industry. This work includes an innovative supercritical CO2 fractionation process based on the online coupling of supercritical fluid extraction (SFE) and dynamic adsorption/desorption for the selective enrichment of terpenoids in the different olive leaves extracts. The selectivity of different commercial adsorbents such as silica gel, zeolite, and aluminum oxide was evaluated toward the different terpene families present in olive leaves. Operating at 30 MPa and 60 °C, an adsorbent-assisted fractionation was carried out every 20 min for a total time of 120 min. For the first time, GC-QTOF-MS allowed the identification of 40 terpenoids in olive leaves. The GC-QTOF-MS results indicate that silica gel is a suitable adsorbent to partially retain polyunsaturated C10 and C15 terpenes. In addition, aluminum oxide increases C20 recoveries, whereas crystalline zeolites favor C30 terpenes recoveries. The different healthy properties that have been described for terpenoids makes the current SFE-GC-QTOF-MS process especially interesting and suitable for their revalorization.