Examinando por Autor "Carvalheiro, Florbela"
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Ítem An integrated olive stone biorefinery based on a 1 two-step fractionation strategy(Elsevier, 2022) Padilla-Rascón, Carmen; Carvalheiro, Florbela; Duarte, Luís C.; Roseiro, Luisa B.; Ruiz, Encarnación; Castro, EulogioOlive stones (OS) constitute a waste lignocellulosic material produced by the olive oil industry in great amounts, that currently is only used as a low-value energy source for industrial or domestic boilers. Having in view its full valorization, this work proposes and validates an integrated strategy aiming to obtain three different streams of sugars / lignin-derived compounds. Dilute acid hydrolysis was used to obtain a xylose-rich hydroysate that was chemically converted into furfural with a 48.7 % yield. The resulting acid-pretreated solid biomass that consisted mainly of lignin and cellulose, was subjected to a catalyzed ethanol-based organosolv delignification. Temperature, time, and sulphuric acid concentration were optimized in order to recover added-value lignin products and digestible cellulose. At the optimal conditions (190 ᵒC and 30 min), a 50 % delignification was reached, together with the highest enzymatic hydrolysis yields (190 g glucose/kg of OS). Phenolic compounds content in organosolv liquors reached 41.6 mg GAE/g OS. This extract presented an antioxidant capacity up to 10.9 mg TE/g OS. The pretreated solid fraction was used as a substrate for ethanol production by a pre-saccharification and simultaneous saccharification and fermentation process, enabling to obtain an ethanol concentration of 47 g/L, with a fermentation yield of 61.4% of the theoretical maximum. Globally, from 100 kg of OS processed according to this experimental scheme, 6.9 kg of furfural, 6.2 kg of ethanol, 7.4 kg of lignin, and 4.2 kg of phenolics compounds can be obtained as main products, thus constituting a way of valorization of renewable material in a multiproduct biorefinery strategy.Ítem Combined Extraction and Ethanol Organosolv Fractionation of Exhausted Olive Pomace for Bioactive Compounds(Wiley Online Library, 2022-01-25) Gómez-Cruz , Irene; Romero, Inmaculada; Contreras Gámez , María del Mar; Labidi, Jalel; Hernández-Ramos, Fabio; Roseiro, Luisa B.; Duarte, Luis C.; Castro , Eulogio; Carvalheiro, FlorbelaThe olive pomace oil extracting industry generates large amounts of exhausted olive pomace (EOP), a lignocellulosic waste that needs to be managed according to sustainable criteria. The aim of this work is to devise an integrated strategy to valorize EOP by applying two-step extraction, and to evaluate the effect of an ethanol organosolv pretreatment on the delignification and enzymatic hydrolysis of the extracted EOP. Once the extraction and organosolv pretreatment conditions are selected, solubilized lignin is recovered from the pretreatment liquor using different methods. In addition to those organosolv lignin samples, a lignin-rich solid is obtained after enzymatic saccharification of the pretreated solid. All the lignin samples are fully characterized aiming at further valorization. The selected two-step aqueous extraction (85 °C, 90 min, 10% biomass) removes 89% of the extractives content in raw EOP and achieves the full recovery of phenols and mannitol content in that fraction, 4.7 mg gallic acid equivalents per g EOP and 4.5 mg g−1 EOP, respectively. The organosolv pretreatment (50% ethanol catalyzed with 1% H2SO4, 140 °C, 60 min, 15% biomass) results in a delignified solid with 81% of enzymatic digestibility and a high purity organosolv lignin (>71%), rich in guaiacyl units.Ítem Recovery of Bioactive Compounds from Industrial Exhausted Olive Pomace through Ultrasound-Assisted Extraction(MDPI, 2021-06-10) Gómez-Cruz , Irene; Contreras Gámez, María del Mar; Carvalheiro, Florbela; Duarte, Luis C.; Roseiro , Luisa B.; Romero , Inmaculada; Castro , EulogioExhausted olive pomace (EOP) is the main agro-industrial waste of the olive pomace extracting industries. It contains phenolic compounds and mannitol, so the extraction of these bioactive compounds should be considered as a first valorization step, especially if EOP is used as biofuel. Therefore, EOP was subjected to bath-type ultrasound-assisted extraction (UAE), and the effects of the acetone concentration (20–80%, v/v), solid load (2–15%, w/v), and extraction time (10–60 min) on the extraction of antioxidant compounds were evaluated according to a Box–Behnken experimental design. By means of the response surface methodology, the optimum conditions were obtained: 40% acetone, 8.6% solids, and 43 min. For all the extracts, the total phenolic content (TPC), flavonoid content (TFC), and antioxidant activity (DPPH, ABTS, and FRAP) were determined. With the aim of shortening the extraction time, a two-level factorial experiment design was also carried out using a probe-type UAE, keeping the solid load at 8.6% (w/v) and the acetone concentration at 40% (v/v), while the amplitude (30–70%) and the extraction time (2–12 min) were varied to maximize the aforementioned parameters. Finally, a maximum of phenolic compounds was reached (45.41 mg GAE/g EOP) at 12 min and 70% amplitude. It was comparable to that value obtained in the ultrasonic bath (42.05 mg GAE/g EOP), but, remarkably, the extraction time was shortened, which translates into lower costs at industrial scale. Moreover, the bioactive compound hydroxytyrosol was found to be the major phenolic compound in the extract, i.e., 5.16 mg/g EOP (bath-type UAE) and 4.96 mg/g EOP (probe-type UAE). Other minor phenolic compounds could be detected by capillary zone electrophoresis and liquid-chromatography–mass spectrometry. The sugar alcohol mannitol, another bioactive compound, was also found in the extract, and its content was determined. Thus, the use of this technology can support the valorization of this waste to obtain bioactive compounds, including mannitol, hydroxytyrosol, and other derivatives, before being applied for other uses.Ítem Strategies for the purification of hydroxytyrosol-rich extracts obtained from exhausted olive pomace(Elsevier, 2023-11-15) Gómez-Cruz , Irene; Contreras Gámez , María del Mar; Romero, Inmaculada; Ribeiro, Belina; Roseiro, Luisa B.; Duarte, Luis C.; Carvalheiro, Florbela; Castro , EulogioExhausted olive pomace (EOP) is a residual biomass from which hydroxytyrosol can be recovered. This compound has applications in the food/pharma sectors, but its extraction yields complex extracts that require further purification for some applications. This work explores purification strategies based on membrane technology, liquid–liquid extraction (LLE), and solid-phase extraction with adsorbents and resins. The hydroxytyrosol content, phenolic profile, antioxidant activity, and inhibition of α-glucosidase and α-amylase were monitored. Hydroxytyrosol stood out in all purified extracts. The best hydroxytyrosol recovery (88.8%) was achieved using LLE with ethyl acetate as the extractant, while the purest extracts in phenolic compounds, including hydroxytyrosol, were obtained using the latter solvent and C18 (529 mg/g), DSC-8 (873 mg/g), and Purosorb PAD910 (523 mg/g). Conversely, mannitol and glucose, at high concentrations in the extract, were selectively retained in the aqueous phases. The developed strategies are discussed regarding their suitability to provide hydroxytyrosol-concentrated extracts, up to 291 mg/g, with antioxidant and antidiabetic functionalities