Hydroxytyrosol Enrichment of Olive Leaf Extracts via Membrane Separation Processes.

Antioxidants isolated from plant materials, such as phenolics, have attracted a lot of attention because of their potential uses. This contributes to the idea of the biorefinery, which is a way to produce useful products from biomass waste. Olea europaea byproducts have been extensively investigated for their large contents in phenolics. Oleuropein is a phenolic compound abundant in olive leaves, with its molecule containing hydroxytyrosol, elenolic acid, and glucose. In this work, olive leaf extracts were treated using different combinations of ultrafiltration and nanofiltration membranes to assess their capacity of facilitating the production of hydroxytyrosol-enriched solutions, either by separating the initially extracted oleuropein or by separating the hydroxytyrosol produced after a hydrolysis step. The best performance was observed when an ultrafiltration membrane (UP010, 10,000 Da) was followed by a nanofiltration membrane (TS40, 200-300 Da) for the treatment of the hydrolyzed extract, increasing the purity of the final product from 25% w/w of the total extracted compounds being hydroxytyrosol when membrane processes were not used to 68% w/w.

High-Yield Production of a Rich-in-Hydroxytyrosol Extract from Olive (Olea europaea) Leaves.

The aim of the present study was to explore the high-yield production of hydroxytyrosol, a phenolic compound with very high antioxidant capacity. Olea europaea leaves were chosen as feedstock as they contain significant amounts of oleuropein, which can be hydrolyzed to hydroxytyrosol. The chosen techniques are widely used in the industry and can be easily scaled up. Olive leaves underwent drying and mechanical pretreatment and extractives were transported to a solvent by solid-liquid extraction using water-ethanol mixtures. The use of approximately 60-80% ethanol showed an almost 2-fold increase in extracted phenolics compared to pure water, to approximately 45 g/kg of dry leaves. Extracted oleuropein was hydrolyzed with hydrochloric acid and the hydrolysate was extracted with ethyl acetate after pH adjustment. This step led to a hydroxytorosol content increase from less than 4% to approximately 60% w/w of dry extract, or 10-15 g of hydroxytyrosol recovery per kg of dry leaves.

Isolation of organic compounds with high added values from agro-industrial solid wastes.

Phenols are organic compounds with high antioxidant activity. Occurring mainly in plants, where they act as pigments or even as part of defense mechanisms against insects and herbivores. Given the positive impact on on human health, their isolation and purification from agricultural products is of particular interest for the production of nutritional, pharmaceutical and cosmetics supplements. In our study different materials rich in phenolic compounds were used, in order to separate the phenolic content and maximum condensation using physicochemical methods such as solvent extraction, filtration through membranes, adsorption/desorption on resins and vacuum distillation. The materials tested were solid wastes from winery, cocoa residuals, olive leaves, etc. The first step for the treatment was the extraction of phenolic content using water-ethanol solutions which was initially optimized. Then, sequential membrane filtration of the extracts by Ultrafiltration membranes, Nanofiltration and Reverse Osmosis was performed to separate the contained compounds, based on their molecular weight. To remove non-polar compounds, with similar molecular weights with phenols, methods of adsorption/desorption on specific resins were developed, in order final ethanolic solutions rich in phenolic compounds to be obtained. Finally, the ethanol was removed by vacuum evaporation at low temperatures. The purification of olive leaf phenols is illustrated in details in the present work. The final obtained concentrate, was a rich phenolic concentrate and contained 98 g/L phenols in gallic acid equivalents. This technique, after modification, can be applied to a variety of phenol-rich byproducts, allowing the operation of phenol separation plant adjustable to local agricultural activities.

Purification of olive mill wastewater phenols through membrane filtration and resin adsorption/desorption.

Olive tree cultivation has a long history in the Mediterranean countries, and even today consists an important cultural, economic, and environmental aspect of the area. The production of olive oil through 3-phase extraction systems, leads to the co-production of large quantities of olive mill wastewater (OMW), with toxic compounds that inhibit its biodegradation. Membrane filtration has been used for the exploitation of this byproduct, through the isolation of valuable phenolic compounds. In the current work, a fraction of the waste occurring from a membrane process was used. More specifically the reverse osmosis concentrate, after a nanofiltration, containing the low-molecular-weight compounds, was further treated with resin adsorption/desorption. The non ionic XAD4, XAD16, and XAD7HP resins were implemented, for the recovery of phenols and their separation from carbohydrates. The recovered phenolic compounds were concentrated through vacuum evaporation reaching a final concentration of 378 g/L in gallic acid equivalents containing 84.8 g/L hydroxytyrosol.

Membrane filtration of agro-industrial wastewaters and isolation of organic compounds with high added values.

The aim of the current study was the exploitation of agro-industrial wastes or by-products such as olive mill wastewater (OMW) and defective wines. A cost-effective system for their maximum exploitation is suggested, using a combined process of membrane filtration and other physicochemical processes. Wastewaters are first treated in a membrane system (prefiltration, ultrafiltration, nanofiltration, and reverse osmosis) where pure water and other organic fractions (by-products) are obtained. Organic fractions, called hereafter byproducts and not wastes, are further treated for the separation of organic compounds and isolation of high added value products. Experiments were performed with OMW and defective wines as characteristic agro-industrial wastewaters. Profit from the exploitation of agro-industrial wastewaters can readily help the depreciation of the indeed high cost process of membrane filtration. The simple phenolic fraction of the OMW was successfully isolated from the rest of the waste, and problems occurring during winemaking, such as high volatile acidity and odours, were tackled.