The production of olive oil and wine are two of the main agri-food economic activities in Southern Europe. They generate large amounts of solid and liquid wastes (e.g., olive pomace, olive mill wastewater, grape pomace, grape stems, wine lees, and wine processing wastewater) that represent a major environmental problem. Consequently, the management of these residues has become a big challenge for these industries, since they are harmful to the environment but rich in bioactive compounds, such as polyphenols. In recent years, the recovery of phenolic compounds has been proposed as a smart strategy for the valorization of these by-products, from a circular economy perspective. This review aims to provide a comprehensive description of the state of the art of techniques available for the analysis, extraction, and purification of polyphenols from the olive mill and winery residues. Thus, the integration and implementation of these techniques could provide a sustainable solution to the olive oil and winery sectors.

In this study, the recovery of polyphenols from olive oil mill and winery waste was investigated. The performance of ultrasound assisted extraction (UAE), microwave assisted extraction (MAE), and pressurized liquid extraction (PLE) was assessed using ethanol–water mixtures, which are compatible with food, nutraceutical, and cosmetic applications. The extraction efficiency from olive pomace and lees samples was evaluated in terms of total polyphenol content (TPC), determined by high performance liquid chromatography (HPLC) and Folin–Ciocalteu assay. The effect of solvent composition, temperature, and time was analyzed by response surface methodology. Ethanol:water 50:50 (v/v) was found to be a suitable solvent mixture for both kinds of samples and all three extraction techniques. The performance of the extraction techniques was evaluated, under optimal experimental conditions, with a set of different representative samples of residues from olive oil and wine production. Overall, the best extraction efficiency for olive pomace residues was provided by MAE (ethanol:water 50:50 (v/v), 90 °C, 5 min), and for wine residues by PLE (ethanol:water 50:50 (v/v), 100 °C, 5 min, 1 cycle). However, the results provided by UAE (ethanol:water 50:50 (v/v), 30 min) were also suitable. Considering not only extraction performance, but also investment and operational costs, UAE is proposed for a future scaling up evaluation. Regarding olive pomace as a source for natural phenolic antioxidants, olive variety and climatic conditions should be taken into account, since both influence TPC in the extracts, while for winery residues, lees from red wines are more suitable than those from white wines.

Winery and olive mill industries generate large amounts of wastes causing important environmental problems. The main aim of this work is the evaluation of different membrane separation processes like microfiltration, ultrafiltration, nanofiltration, and reverse osmosis for the recovery of polyphenols from winery and olive mill wastes in aqueous solutions. Membrane processes were tested separately in a closed-loop system, and by an integration in a concentration mode sequential design (open-loop). Feed flow rate was varied from 1 to 10 mL min^-1, and permeate samples were taken in order to measure the polyphenols concentration. The separation and concentration efficiency were evaluated in terms of total polyphenol content, and by polyphenols families (hydroxybenzoic acids (HB), hydroxycinnamic acids (HC), and flavonoids (F)), using high performance liquid chromatography. Results showed that MF and UF membranes removed suspended solids and colloids from the extracts. NF was useful for polyphenols separation (HB rejections were lower than for HC and F: HB rejections of 50 and 63% for lees filters and olive pomace extracts, respectively), and RO membranes were able to concentrate polyphenols streams (86 and 95% rejection from lees filters and olive pomace, respectively). Membranes sequential designs for lees filters and olive pomace extracts, using a selective membrane train composed by UF, NF and RO membranes, were able to obtain polyphenol rich streams and high-quality water streams for reuse purposes.

Phenolic compounds recovery by mechanical stirring extraction (MSE) was studied from orange and spinach wastes using water as a solvent. The statistical analysis showed that the highest total polyphenol content (TPC) yield was obtained using 15 min, 70 °C, 1:100 (w/v) solid/solvent ratio and pH 4 for orange; and 5 min, 50 °C, 1:50 (w/v) solid/solvent ratio and pH 6 for spinach. Under these conditions, the TPC was 1 mg gallic acid equivalent (GAE) g⁻¹ fresh weight (fw) and 0.8 mg GAE g⁻¹ fw for orange and spinach, respectively. MSE substantially increased the phenolic compounds yields (1-fold for orange and 2-fold for spinach) compared with ultrasound-assisted extraction. Furthermore, the antioxidant activity of orange and spinach extracts was evaluated using DPPH, FRAP and ABTS. The obtained results pointed out that the evaluated orange and spinach residues provided extracts with antioxidant activity (2.27 mg TE g⁻¹ and 0.04 mg TE g⁻¹, respectively).