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By-products of essential oils (EOs) in the industry represent an exploitable material for natural and safe antioxidant production. One representative group of such by-products is distilled solid residues, whose composition is properly modulated by the distillation method applied for the recovery of EOs. Recently, in terms of Green Chemistry principles, conventional extraction and distillation processes are considered outdated and tend to be replaced by more environmentally friendly ones. In the present study, microwave-assisted hydro-distillation (MAHD) was employed as a novel and green method for the recovery of EOs from three aromatic plants (rosemary, Greek sage and spearmint). The method was compared to conventional ones, hydro-distillation (HD) and steam-distillation (SD), in terms of phytochemical composition of distilled solid residues, which was estimated by spectrophotometric and chromatographic methods. Total phenolic content (TPC), total flavonoid content (TFC) and antioxidant activity (ABTS, DPPH and FRAP) results highlighted the distilled solid residues as good sources of antioxidants. Moreover, higher antioxidant activity was achieved for MAHD extracts of solid residues in comparison to HD and SD extracts. A metabolomics approach was carried out on the methanolic extracts of solid residues obtained by different distillation methods using LC-MS analysis followed by multivariate data analysis. A total of 29 specialized metabolites were detected, and 26 of them were identified and quantified, presenting a similar phenolic profile among different treatments, whereas differences were observed among different species. Rosmarinic acid was the most abundant phenolic compound in all extracts, being higher in MAHD extracts. In rosemary and Greek sage extracts, carnosol and carnosic acid were quantified in significant amounts, while trimers and tetramers of caffeic acid (salvianolic acids isomers) were identified and quantified in spearmint extracts, being higher in MAHD extracts. The obtained results pointed out that MAHD extracts of distilled solid by-products could be a good source of bioactives with potential application in the food, pharmaceutical and cosmetic industries, contributing to the circular economy.

Rosemary solid distillation waste (SWR), a by-product of the essential oil industry, represents an important source of phenolic antioxidants. Green technologies such as ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), and accelerated solvent extraction (ASE) of phenolic compounds from SWR were optimized as valorization routes to maximize yield, rosmarinic acid (RMA), carnosol (CARO) and carnosic acid (CARA) contents. Response surface methodology was used in this context, with ethanol concentration (X1), extraction temperature (X2), and time (X3) being the independent variables. A second-order polynomial model was fitted to the data, and multiple regression analysis and analysis of variance were used to determine model fitness and optimal conditions. Ethanol concentration was the most influential extraction parameter, affecting phenolic compounds, while the influence of other parameters was moderate. The optimized conditions were as follows: X1: 67.4, 80.0, and 59.0%, X2: 70, 51, and 125 °C, and X3: 15, 10, and 7 min for MAE, UAE, and ASE, respectively. A comparison of optimized MAE, UAE, and ASE with conventional Soxhlet extraction techniques indicated that ASE provided a higher extraction yield and content of phenolic compounds. However, UAE represented the best process from an environmental point of view, allowing an improved extraction of phenolics from SWR with high energy efficiency and low energy costs.

The objective of this study was to evaluate the effects of different stabilization treatments—namely, dry-heating, infrared-radiation, and microwave-heating—on the nutritional, antinutritional, functional, and bioactivity attributes of rice bran (RB). Among the heating treatments, infrared-radiation exerted the strongest inactivation, resulting in 34.7% residual lipase activity. All the stabilization methods were found to be effective in the reduction of antinutrients, including phytates, oxalate, saponins, and trypsin inhibitors. No adverse effect of stabilization was noted on chemical composition and fatty acid profile of RB. Instead, stabilization by all heat treatments caused a significant decrease of vitamin E and total phenolics content in RB; the same trend was observed for the antioxidant activity as evaluated by the DPPH test. The antioxidant activity, as evaluated by ABTS and FRAP tests, and water absorption capacity were improved by the stabilization of RB, whereas the oil absorption capacity and emulsifying properties decreased. Microwave-heating enhanced the foaming properties, whereas infrared-radiation improved the water solubility index and swelling power of RB. Consequently, treatment of RB with infrared-radiation has a potential for industrialization to inactivate the lipase and improve some functional properties of this material for uses as a nutraceutical ingredient in food and cosmetic products.

Plant solid residues obtained from the essential oil industry represent a rich source of phenolic compounds with bioactive properties to be used in the food and pharmaceutical industries. A selective and sensitive liquid chromatography-mass spectrometry (LC-MS) method was developed for the simultaneous determination of phenolic compounds in solid residues of the Lamiaceae family plants. A total of 48 compounds can be separated within 35 min by using the Poroshell-120 EC-C18 column, and a gradient mobile phase of 0.1% formic acid and acetonitrile with flow rate of 0.5 mL/min; salicylic acid was used as internal standard. The calibration curves showed good linearity in the tested concentration range for each analyte (R2 > 0.9921), while recoveries ranged from 70.1% to 115.0% with an intra-day and inter-day precision of less than 6.63% and 15.00%, respectively. Based on the retention behavior, as well as absorption and mass spectra, 17 phenolic acids, 19 flavonoids and 2 phenolic diterpenes were identified and quantified in the solid residues obtained by distillation of six aromatic plants: oregano, rosemary, sage, satureja, lemon balm, and spearmint. The method constitutes an accurate analytical and quality control tool for the simultaneous quantitation of phenolics present in solid waste residues from the essential oil industry.

The purpose of the present study was to compare the polyphenolic compounds extracted from five Sideritis species grown in Greece; S. scardica, S. clandestina, S. raeseri, S. euboea, and S. syriaca, using the Microwave-Assisted Extraction (MAE) process. To maximize the extraction yield (EY), total phenolic compounds (TPC), hypolaetin (HYP) and isoscutellarein (ISC), derivative contents (target phenolics), the response surface methodology was used for S. scardica. A Box–Behnken design was undertaken to study the effect of ethanol concentration (30–100%), extraction temperature (40–100 °C), and extraction time (5–25 min) on the responses. The optimal MAE parameters were 87.9% (v/v) ethanol, 25 min, and 100 °C. Under these conditions, there was a good agreement between experimental and predicted values, indicating the reliability of the predictions for Sideritis extracts. Phenolic compounds were then extracted under these conditions, from the five Sideritis species under investigation. The TPC, total flavonoid content (TFC), antioxidant activity based on DPPH, ABTS, and FRAP assays as well as the phenolic profile of different Sideritis extracts, evaluated via HPLC-DAD-MS, were compared. A similar phenolic profile was observed among the five Sideritis species, with HYP and ISC derivatives showing variations in their contents as a function of Sideritis species. MAE Sideritis extracts could be considered green and natural antioxidants for medicinal, cosmetic, and food purposes, accompanied by sustainable approaches.

Rice by-products are extensively abundant agricultural wastes from the rice industry. This study was designed to optimize experimental conditions for maximum recovery of free and bound phenolic compounds from rice by-products. Optimized conditions were determined using response surface methodology based on total phenolic content (TPC), ABTS radical scavenging activity and ferric reducing power (FRAP). A Box-Behnken design was used to investigate the effects of ethanol concentration, extraction time and temperature, and NaOH concentration, hydrolysis time and temperature for free and bound fractions, respectively. The optimal conditions for the free phenolics were 41–56%, 40 °C, 10 min, whereas for bound phenolics were 2.5–3.6 M, 80 °C, 120 min. Under these conditions free TPC, ABTS and FRAP values in the bran were approximately 2-times higher than in the husk. However, bound TPC and FRAP values in the husk were 1.9- and 1.2-times higher than those in the bran, respectively, while bran fraction observed the highest ABTS value. Ferulic acid was most evident in the bran, whereas p-coumaric acid was mostly found in the husk. Findings from this study demonstrates that rice by-products could be exploited as valuable sources of bioactive components that could be used as ingredients of functional food and nutraceuticals.

Nowadays, eco-friendly extraction techniques are often used to develop natural plant extracts for commercial use. In the current investigation, Greek oregano (Origanum vulgare) phenolic extracts from different cultivated accessions were recovered employing ultrasonic-assisted extraction (UAE), microwave-assisted extraction (MAE), and accelerated solvent extraction (ASE). The phytochemical profile of the oregano extracts, as determined by spectrophotometric and chromatographic techniques, as well as antioxidant activity (ABTS, DPPH, and FRAP assays), was used to compare the three extraction approaches. The results showed that oregano phenolic extracts obtained by MAE held the highest total phenolic content, total flavonoid content, and also a higher content of the main phenolic compounds identified, rosmarinic acid, salvianolic acid B and carvacrol, as determined by LC-MS analysis, followed by those extracted by UAE and ASE. All of the tested extracts exhibited relatively high antioxidant activities, especially the MAE extracts. Oregano extracts produced by various extraction techniques were subjected to a multivariate data analysis to highlight differences in phytochemical profiles, and their correlation to antioxidant activity. According to our findings, it was evident that MAE offers more efficient and effective extraction of bioactive compounds in terms of obtaining phytochemical-rich oregano extracts, with applications in the food and pharmaceutical industries.

The essential oil production of Salvia fruticosa L. generates considerable amounts of post-distillation solid residues (PRES) which are rich in phenolic compounds. In the present work, the recovery of phenolic antioxidants from PRES by using Microwave-Assisted Extraction (MAE) and Ultrasound-Assisted Extraction (UAE) were separately optimized, according to the Box–Behnken experimental design. The optimization was based on extraction yield, total phenolic content (TPC), total flavonoid content (TFC), rosmarinic acid (RMA), carnosol (CARO), carnosic acid (CARA), and antioxidant activity. The optimal processing parameters were 72% and 68% ethanol, a 15- and 10-min extraction time, a 40 °C and 47 °C extraction temperature, and a 1:30 and 1:10 solid-to-solvent ratio, for MAE and UAE, respectively. Results showed that the levels of RMA, CARO, and CARA in UAE extracts were influenced mainly by ethanol concentration, extraction time, and extraction temperature, while MAE extracts were only influenced by the first two factors. Experimenting with the optimal conditions revealed MAE as more effective than UAE in the recovery of RMA and CARA. The experimental values were in good agreement with the predicted ones, indicating model efficacy in MAE and UAE optimization to effectively extract phenolic compounds from PRES for their further application in food and pharmaceutical industries.

The phenolic profile of Greek chamomile populations was investigated by HPLC-PDA-MS. For comparison, three commercial varieties (Banatska, Lutea and Goral) cultivated under the same conditions were included in the study. All samples exhibited similar qualitative patterns but differed in their quantitative characteristics. Overall, 29 constituents were detected, belonging to phenolic acids, flavonol glycosides, flavone glycosides (mainly apigenin derivatives) and acylated polyamines. Quantitative results showed that both Greek populations had a high content in apigenin derivatives (0.39 and 0.31 %w/w) and caffeoylquinic acids (0.96 and 0.81 %w/w), whereas they had the highest amount of flavonol glycosides among the tested samples. Greek populations were comparable to the Banatska variety, while they were superior to the Lutea and Goral varieties cultivated under the same conditions. Results demonstrate that Greek chamomile populations studied here, are an excellent source of a wide range of phenolics which contribute to the medicinal and antioxidant properties of this herbal remedy. Antioxidant tests showed that chamomile extracts from the studied materials, especially from the Greek populations possess antioxidant activity, corresponding to their polyphenol content. This is the first report on the phenolic constituents of Matricaria recutita growing in Greece and well-established chamomile varieties.

For a long time, sulfur dioxide (SO2) has been the most universally used additive in winemaking. With its wide range of effects, ease of use, and low cost, sulfur dioxide has not yet been completely replaced by any process or substance. Since the expected trend for the near future is to keep reducing the concentration of sulfites, many investigations focus on alternative chemical, biological, or physical processes. This study aims to evaluate the chemical, antioxidant, and sensory impact of a plant-based product used as sulfur dioxide replacement (SDR) in white, rosé, and red wines produced as a result of the application of different vinification protocols. The physicochemical and sensory evaluation of the different wines produced showed that this plant-based product could be a good candidate, but appropriate winemaking treatments and optimization are needed to limit wine defects.