Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (Thymus serpyllum L.) Extracts.

Wild thyme (Thymus serpyllum L.) herbal dust has been recognized as a potential underutilized resource for the recovery of antioxidants. The aim of this paper was to optimize natural deep eutectic solvent (NADES) extraction of polyphenols to obtain improved antioxidant activity of extracts determined by selected in vitro assays (DPPH, FRAP, and ABTS). Twenty different NADES systems were investigated in the first step of the screening of the extraction solvent and l-proline (Pro)-glycerine (Gly) based solvents provided the best results. Preliminary experiments organized by 25-1 fractional factorial design narrowed down the number of extraction factors from five (temperature, extraction time, NADES type, water content and L/S ratio) to three and determined their experimental domain for the final step. A face-centered central composite design with temperature (40-55-70 °C), extraction time (60-120-180 min) and L/S ratio (10-20-30 g NADES/g sample) was applied for influence analysis and process optimization. Multi-response optimization suggested a temperature of 65 °C, time of extraction of 180 min and L/S ratio of 28 g NADES/g DW as optimal extraction parameters. Experimental validation confirmed good agreement between experimental and predicted results in the extract obtained at optimal conditions and the interactions in the most suitable NADES (N16; Pro-Gly-H2O; 1:2:1) were confirmed by the 1H-NMR.

Pressurized-Liquid Extraction as an Efficient Method for Valorization of Thymus serpyllum Herbal Dust towards Sustainable Production of Antioxidants.

The aim of this study was to valorize Thymus serpyllum herbal dust, a particular fraction distinguished as an industrial waste from filter-tea production. Pressurized liquid extraction (PLE) was used with the aim of overcoming certain obstacles of conventional extraction techniques in terms of shortening extraction time, reducing solvent consumption and energy costs, using "green" solvents and obtaining high yield and quality products. In order to optimize PLE of T. serpyllum herbal dust, the preliminary screening of the independent variables in order to define the most influential parameters and their domain was done first. After the screening, the optimization study using the face-centered central composite experimental design (CCD) with response surface methodology (RSM) was implemented. Additionally, taking into account the high awareness of the positive influence of antioxidants on the human health and associating it with high content of polyphenolic compounds in various members of Lamiaceae family, PLE has proven to be a great approach for antioxidants recovery from T. serpyllum herbal dust.

Extraction of Peppermint Essential Oils and Lipophilic Compounds: Assessment of Process Kinetics and Environmental Impacts with Multiple Techniques.

Consumers are becoming more mindful of their well-being. Increasing awareness of the many beneficial properties of peppermint essential oil (EO) has significantly increased product sales in recent years. Hydrodistillation (HD), a proven conventional method, and a possible alternative in the form of microwave-assisted hydrodistillation (MWHD) have been used to isolate peppermint EO. Standard Soxhlet and alternatively supercritical fluid (SFE), microwave-assisted, and ultrasound-assisted extraction separated the lipid extracts. The distillations employed various power settings, and the EO yield varied from 0.15 to 0.80%. The estimated environmental impact in terms of electricity consumption and CO2 emissions suggested that MWHD is an energy efficient way to reduce CO2 emissions. Different extraction methods and solvent properties affected the lipid extract yield, which ranged from 2.55 to 5.36%. According to the corresponding values of statistical parameters, empiric mathematical models were successfully applied to model the kinetics of MWHD and SFE processes.

Green Extraction Approach for Isolation of Bioactive Compounds in Wild Thyme (Thymus serpyllum L.) Herbal Dust-Chemical Profile, Antioxidant and Antimicrobial Activity and Comparison with Conventional Techniques.

The aim of this study was to provide a chemical profile and determine the antioxidant and antimicrobial activity of the essential oil (EO) and lipid extracts of Thymus serpyllum L. herbal dust obtained via conventional (hydrodistillation (HD) and Soxhlet extraction (SOX)) and novel extraction techniques (supercritical fluid extraction (SFE)). In addition, a comparative analysis of the chemical profiles of the obtained EO and extracts was carried out, as well as the determination of antioxidant, antibacterial and antifungal activity of the lipid extracts. According to the aforementioned antioxidant and antimicrobial activities and the monoterpene yield and selectivity, SFE provided significant advantages compared to the traditional techniques. In addition, SFE extracts could be considered to have great potential in terms of their utilization in the pharmaceutical and cosmetic industries, as well as appropriate replacements for synthetic additives in the food industry.

Polyphenols Recovery from Thymus serpyllum Industrial Waste Using Microwave-Assisted Extraction-Comparative RSM and ANN Approach for Process Optimization.

The aim of this study was to valorize Thymus serpyllum L. herbal dust, the particular fraction distinguished as industrial waste from filter-tea production. This work demonstrated comparable analysis considering model fitting, influence analysis and optimization of microwave-assisted extraction (MAE) of bioactive compounds from the aforementioned herbal dust using face-centered central composite experimental design within the response surface methodology (RSM), as well as artificial neural networks (ANN). In order to increase yield and amount of compounds of interest and minimize solvent, time and energy consumption, the ethanol concentration (45, 60 and 75%), extraction time (5, 12.5 and 20 min), liquid-solid ratio (10, 20 and 30 mL/g) and irradiation power (400, 600 and 800 W) were used as independent variables. Total extraction yield (Y), total phenols yield (TP), as well as antioxidant activity parameters obtained by DPPH and ABTS assays, were selected as responses. It could be concluded that the MAE technique is an efficient approach for the extraction of biologically active compounds from T. serpyllum herbal dust, which represents a high-value source of natural antioxidants with great potential for further use in various forms within different branches of industry.

Innovative and Conventional Valorizations of Grape Seeds from Winery By-Products as Sustainable Source of Lipophilic Antioxidants.

The aim of this study was to valorize the oil recovery from red and white grape seeds (Vitis vinifera L.) that remains as by-product after the winemaking process. Oils were extracted by modern techniques, ultrasound assisted (UAE), microwave assisted (MAE) and supercritical fluid extraction (SFE), and compared to the Soxhlet extraction (SE). Firstly, SFE was optimized at different operating conditions: pressure (250-350 bar), temperature (40-60 °C), CO2 flow rate (0.2, 0.3 and 0.4 kg h-1), and particle size (315-800 µm and >800 µm). The highest extraction yields were achieved by SFE at the optimal conditions: 350 bar, 60 °C, 0.4 kg h-1. Afterwards, SFE was compared to SE, UAE and MAE with respect to oil extraction yields, and analyzed for fatty acid composition and antioxidant capacity. Considering the general classification of fatty acids, it was found that samples had high content of polyunsaturated fatty acids, regardless of extraction technology. Tocopherol content was significantly influenced by all extraction methods, whereas UAE and MAE resulted in extracts richer with lipophilic antioxidants. In conclusion, modern extractions that are suited for industrial applications had better performance as compared to SE, as judging by the oil yield and quality.