The aim of this study was to evaluate the efficiency of successive extraction (using solvents of increasing polarity, namely hexane, ethyl acetate, acetone, ethanol, and water) of polyphenols from Cistus creticus L. The results were compared with the ones obtained from a single-solvent extraction (ethanol, water, and 50% ethanol: water). According to the results, each solvent used for extraction had a significant effect on the yield of extracted polyphenols and the antioxidant activity of the extracts. The highest extraction yield for successive extraction was achieved with ethanol (95.33 mg GAE/g), whereas a comparable amount could also be extracted with 50% ethanol: water mixture single-solvent extraction (96.51 mg GAE/g). The ethanolic and aqueous extracts had the highest antioxidant activity as indicated by their lowest IC₅₀ values in the DPPH assay, specifically 350.99 μg/mL for ethanolic extract of successive extraction and 341.18 μg/mL for 50% ethanol: water mixture of single-solvent extraction, followed by the extract produced using acetone. However, the acetone extract contained more flavonoids than the other two extracts up to 28.03 mg QE/g. The results obtained were in line with those for the single-solvent extraction. It is concluded that using a range of solvents in succession is a more efficient way of extracting higher amounts of antioxidant compounds with varying antioxidant activity.

More and more research is being focused on the production of value-adding products from waste materials. Food waste is not only a major global issue, but also an excellent source of bioactive compounds. In this study, the parameters that affect the extraction of the bioactive compounds (polyphenols, ascorbic acid, hesperidin, carotenoids) from orange peels, and their antioxidant properties, were optimized, using a response surface methodology (RSM) (examining the extraction temperature, time, and composition of the extraction solvent). In addition, the effect of two more techniques was examined [ultrasound (US) and pulsed electric field (PEF)], either separately or combined, so as to determine whether they can enhance the extraction of the compounds. From our results, it was apparent that orange peels are an excellent source of many bioactive compounds since the extracts contained hesperidin (16.26 mg/g dw), total polyphenols (34.71 mg GAE/g dw), ascorbic acid (1228.93 mg/100 g dw) and total carotenoids (52.98 μg CtE/g dw).

Olive leaves (OLL) are reported as a source of valuable antioxidants and as an agricultural by-product/waste. Thus, a twofold objective with multi-level cost and environmental benefits arises for a “green” standalone extraction technology. This study evaluates the OLL waste valorization through maximizing OLL extracts polyphenol concentration utilizing an emerging “green” non-thermal technology, Pulsed Electric Field (PEF). It also provides further insight into the PEF assistance span for static solid-liquid extraction of OLL by choosing and fine-tuning important PEF parameters such as the extraction chamber geometry, electric field strength, pulse duration, pulse period (and frequency), and extraction duration. The produced extracts were evaluated via comparison amongst them and against extracts obtained without the application of PEF. The Folin-Ciocalteu method, high-performance liquid chromatography, and differential scanning calorimetry were used to determine the extraction efficiency. The optimal PEF contribution on the total polyphenols extractability (38% increase with a 117% increase for specific metabolites) was presented for rectangular extraction chamber, 25% v/v ethanol:water solvent, pulse duration (t_pulse) 2 μs, electric field strength (E) 0.85 kV cm⁻¹, 100 μs period (Τ), and 15 min extraction duration (t_extraction), ascertaining a significant dependence of PEF assisting extraction performance to the parameters chosen.

Due to the worldwide consumption of coffee, many tons of spent coffee grounds (SCGs) are discarded each year, as a by-product of coffee preparation. Not only their disposal is costly, but also it may cause the release of compounds that can endanger the environment. However, there are valuable chemical compounds that can be extracted from SCGs and used in the food industry. The aim of this study was to investigate the main parameters affecting the extraction of caffeine and polyphenols (i.e., chlorogenic acid, neochlorogenic acid, and caffeic acid) and to evaluate the antioxidant properties of the extracts. To this end, extraction solvent, temperature, time, and liquid-to-solid ratio were studied. A response surface methodology was used to optimize the extraction process. According to the results, the caffeine content of the optimum extract was found to be 6.14 mg/g in dry SCGs, the total polyphenol content was 19.85 mg gallic acid equivalents/g, while the ferric reducing antioxidant power and DPPH scavenging values were 136.69 μmoL ascorbic acid equivalents/g and 230.41 μmoL DPPH/g, respectively. The experimental values were in close agreement with the predicted ones, highlighting the potential of SCGs to be used for the isolation of bioactive compounds with the proposed extraction procedure.

Tocopherols are natural bioactive compounds with several health benefits. This study evaluated the effect of different ratios of α- and δ- tocopherol homologs to protect sunflower oil (SO) and olive pomace oil (OPO) against oxidation. A synergistic effect was recorded when the two tocopherols were combined at a ratio of 7:1 (α-T/δ-T). The oil samples were exposed to accelerated oxidation conditions using a Rancimat (90 °C and airflow of 15 L/h for 24 h) and protection from tocopherols was compared with that from butylated hydroxytoluene (BHT). Assessment of oil stability was examined using well-known parameters such as peroxide value (PV), thiobarbituric acid reactive substances (TBARS), p-anisidine value (p-AV), conjugated dienes (CD) and trienes (CT), and total oxidation (Totox) value, which were all significantly reduced when tocopherols were added at a ratio of 7:1 α-T/δ-T. Primary oxidative compounds measured according to PV were only reduced in SO samples (6.11%). Off-flavor compounds measured via TBARS assay in SO samples were reduced by above 20%, while p-AV was also reduced. CD_value was correlated with PV in SO samples, while the 7:1 mixture was more effective than BHT for CT_value. Total oxidation values in SO samples and OPO samples were reduced by 6.02% and 12.62%, respectively. These values in SO samples also provided a remarkable correlation (R² > 0.95) with incubation time. Moreover, the synergistic effect was not only effective in reducing the oxidation values of oil samples, but also in lowering the degradation rate of tocopherols. Protective effects from tocopherols were mainly observed in SO samples, as OPO samples were more resistant to oxidation processes. This effect was even observed in fatty acid analysis, where the 7:1 mixture provided better results than BHT-spiked samples. Thus, it is suggested that tocopherol mixtures might be used as a natural preservative in the food industry to restrain lipid oxidation processes.

Olive leaves (OLL), an agricultural waste by-product, are considered a significant bioresource of polyphenols, known as bioactive compounds. This study evaluates the pulsed electric field (PEF) technique for the extraction of polyphenols from OLL. The study parameters included a series of “green” solvents (ethanol, water as well as mixtures of them at a 25% step gradient) and different input values for the pulse duration of PEF. The phytochemical extraction degree was evaluated using total phenol concentration (Folin–Ciocalteu method) and high-performance liquid chromatography (HPLC) analyses, while the antioxidant activity was assessed using differential scanning calorimetry (DSC). The results obtained from the PEF extracts were compared with those of the extracts produced without the PEF application. The highest PEF effect was observed for aqueous ethanol, 25% v/v, using a pulse duration of 10 μs. The increase in the total polyphenols reached 31.85%, while the increase in the specific metabolites reached 265.67%. The recovery in polyphenols was found to depend on the solvent, the pulse duration of treatment and the structure of the metabolites extracted.