Exhausted olive pomace (EOP) is the waste generated from the drying and subsequent extraction of residual oil from the olive pomace. In this work, the effect of different aqueous solvents on the recovery of antioxidant compounds from this lignocellulosic biomass was assessed. Water extraction was selected as the best option for recovering bioactive compounds from EOP, and the influence of the main operational parameters involved in the extraction was evaluated by response surface methodology. Aqueous extraction of EOP under optimised conditions (10% solids, 85 ºC, and 90 min) yielded an extract with concentrations (per g EOP) of phenolic compounds and flavonoids of 44.5 mg gallic acid equivalent and 114.9 mg rutin equivalent, respectively. Hydroxytyrosol was identified as the major phenolic compound in EOP aqueous extracts. Moreover, these extracts showed high antioxidant activity, as well as moderate bactericidal action against some food-borne pathogens. In general, these results indicate the great potential of EOP as a source of bioactive compounds, with potential uses in several industrial applications.
Olive-derived biomass is not only a renewable bioenergy resource but also it can be a source of bioproducts, including antioxidants. In this study, the antioxidant composition of extracted olive pomace (EOP) and a new byproduct, the residual fraction from olive pit cleaning (RFOPC or residual pulp) was characterized and compared to olive leafy biomass, which have been extensively studied as a source of antioxidants and other bioactive compounds with pharmacological properties. The chemical characterization showed that these byproducts contain a high amount of extractives; in the case of EOP, it was even higher (52.9%) than in olive leaves (OL) and olive mill leaves (OML) (35.8–45.1%). Then, ultrasound-assisted extraction (UAE) was applied to recover antioxidants from the extractive fraction of these biomasses. The solubilization of antioxidants was much higher for EOP, correlating well with the extractives content and the total extraction yield. Accordingly, this also affected the phenolic richness of the extracts and the differences between all biomasses were diminished. In any case, the phenolic profile and the hydroxytyrosol cluster were different. While OL, OML, and EOP contained mainly hydroxytyrosol derivatives and flavones, RFOPC presented novel trilignols. Other compounds were also characterized, including secoiridoids, hydroxylated fatty acids, triterpenoids, among others, depending on the bioresource. Moreover, after the UAE extraction step, alkaline extraction was applied recovering a liquid and a solid fraction. While the solid fraction could of interest for further valorization as a biofuel, the liquid fraction contained proteins, sugars, and soluble lignin, which conferred antioxidant properties to these extracts, and whose content depended on the biomass and conditions applied.
Currently, interest in finding new feedstock as sources of natural food antioxidants is growing. The extracted olive pomace (EOP), which is an agro-industrial residue from the olive pomace extracting industries, is generated yearly in big amounts, mainly in the Mediterranean countries. EOP was subjected to an ultrasound assisted extraction with ethanol-water mixtures. The effect of main parameters, such as ethanol concentration (30–70% v/v), ultrasound amplitude (20–80%), and extraction time (5–15 min), on the extraction of antioxidant compounds was evaluated according to a Box–Behnken experimental design. The antioxidant capacity of the resulting extracts was determined by measuring their content in total phenolic compounds (TPC) and flavonoids (TFC), as well as their antioxidant activity by DPPH, ferric reducing antioxidant power (FRAP), and ABTS assays. Considering the simultaneous maximization of these five responses, the optimal conditions were found to be 43.2% ethanol concentration, 70% amplitude, and 15 min. The ultrasound assisted extraction of EOP under these optimized conditions yielded an extract with a phenolic and flavonoid content (per gram of EOP) of 57.5 mg gallic acid equivalent (GAE) and 126.9 mg rutin equivalent (RE), respectively. Likewise, the values for DPPH, ABTS, and FRAP assay (per gram of EOP) of 56.7, 139.1, and 64.9 mg Trolox equivalent, respectively were determined in the optimized extract.
Olive-derived biomasses contain bioactive compounds with health promoting effects as well as antioxidant and sweet-tasting properties. However, their sequential extraction has not been attained. In the present study, firstly antioxidants and mannitol were extracted from exhausted olive pomace (EOP) by an eco-friendly method, ultrasound-assisted water extraction (UAWE). The amplitude (20–80%), extraction time (2–18 min) and solid loading (2–15%, w/v) were evaluated according to a Box–Behnken experimental design. Using the response surface methodology, the optimal conditions for extraction were obtained: 80% amplitude, 11.5% solid loading and 16 min. It enabled the multi-response optimization of the total phenolic content (TPC) (40.04 mg/g EOP), hydroxytyrosol content (6.42 mg/g EOP), mannitol content (50.92 mg/g EOP) and antioxidant activity (ferric reducing power or FRAP, 50.95 mg/g EOP; ABTS, 100.64 mg/g EOP). Moreover, the phenolic profile of the extracts was determined by liquid chromatography-UV and mass spectrometry, identifying hydroxytyrosol as the main phenolic compound and other minor derivatives could be characterized. Scanning electron microscopy was used to analyze the morphological changes produced in the cellular structure of EOP after UAWE. In addition, the chemical composition of the extracted EOP solid was characterized for further valorization. Then, a second extraction step was performed in order to extract bioactive triterpenes from the latter solid. The triterpenes content in the extract was determined and the effect of the previous UAWE step on the triterpenes extraction was evaluated. In this case, the use of ultrasound enhanced the extraction of maslinic acid and oleanolic acid from pelletized EOP with no milling requirement. Overall, UAWE can be applied to obtain antioxidant compounds and mannitol as first extraction step from pelletized EOP while supporting the subsequent recovery of triterpenic acids.
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