In this study, sustainable technology microwave-assisted extraction (MAE) in association with green solvents was applied to recover phenolic compounds from spent coffee grounds (SCGs). A design of experiments (DOE) was used for process optimization. Initially, a 24−1 two level Fractional Factorial Design was used and ratios “solvent to solute” and “ethanol to water” were identified as the significant experimental factors. Consequently, Central Composite Design (CCD) was applied to analyze the effects of the significant variables on the response yield, total polyphenols content (TPC), and antioxidant activity (AA) by the DPPH assay method, and quadratic surfaces to optimize those responses were generated. The values of the significant factors of 16.7 (solvent/solute) and 68.9% (ethanol/water) were optimized simultaneously the yield (%) at 6.98 ± 0.27, TPC (mg GAE/g) at 117.7 ± 6.1, and AA (µmol TE/g) at 143.8 ± 8.6 and were in excellent agreement with those predicted from the CCD model. The variations of the compositions of the lipids, caffeine, pentacyclic diterpenes, and FAME as a function of the dominant factor % ethanol in the solvent mixture were analyzed by applying NMR and GC-FID, and the results obtained confirmed their determinative significance.
This study was aimed at identifying new efficient antioxidant juniper species and their metabolites, which are responsible for this activity. About 30 juniper representatives were assayed for antioxidant activity (DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2′-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) radical scavenging) and total polyphenol content (TPC). The most active species were identified, and their most abundant polyphenols were quantified by the LC-electrospray ionization (ESI)-MS/MS-multiple reaction monitoring (MRM) method. In the group of studied species, J. ashei (mountain cedar) leaf extract was outlined as the best antioxidant with the highest TPC. Catechin was revealed as the most abundant polyphenol in the J. ashei extract, contributing to its superior antioxidant properties. An in-depth analysis of antioxidant capacity was also performed. The higher metal-chelating activity was observed in the case of J. sibirica (0.83 mg DE/mL), whereas the lowest was observed for J. communis (3.2 mg dry extract (DE)/mL) extracts. All efficient antioxidant extracts were also able to inhibit lipoxygenase. EC50 values ranged from 1.77 to 2.44 mg DE/mL. The most effective inhibitors were J. ashei and J. formozana extracts, which acted as uncompetitive lipoxygenase (LOX) inhibitors. The presented results have potential application in the pharmacy and cosmetics for the generation of antioxidant compositions based on naturally derived lead compounds for the prevention of oxidative-stress associated organ-degenerative diseases, cancer, or other free radical-induced disorders.
Sunflower seed hulls and meal are among the most abundant by-products of the food industry. They are an example of waste and, at the same time, a plentiful biomass that cannot be utilized directly in human and animal diets due to their hard digestibility and low nutritional value. Besides their main compounds—carbohydrates, lipids, and proteins—they possess valuable constituents such as vitamins, minerals, and especially phenolics that contribute to their antioxidant capacity. Numerous benefits can be retrieved from such by-products. Since sunflower meal and seed hulls are cheap renewable sources of beneficial substances, their potential in relation to the improvement in our daily life needs to be studied. This is the reason why, in recent years, there has been such a serious interest in their utilization and valorization towards the concept of a circular bio-based economy and process sustainability. This review aims to trace the potential applications and implementation of sunflower meal and hulls in the different fields of industry and environmental protection strategies.
This work investigates the prospects for exploitation of Gnaphalium viscosum (Kunth) abundant but with limited applications till present biomass. The feasibility of traditional techniques (two-phase solvent, and the benchmark Soxhlet extraction) and supercritical extraction without/with a cosolvent at T = 40–60 °C and p = 30–50 MPa was examined to explore the possibility of recovering phytochemicals from G. viscosum leaves, flowers and stems. The efficiency of the techniques was assessed and compared based on yield, influence of solvents used, total phenolic content and antioxidant activity of the extracts. Phenolics of different complexities were identified and quantified by applying LC (LC–MS/MS, and LC–HRAM), while the fatty acid profile was determined by GC–FID. The results of this extensive study demonstrated the huge valorization potential and prospects of G. viscosum, since highly potent antioxidants such as kaempferol, kaempferol-3-O-β-d-glucoside (astragalin), and chlorogenic acid were ascertained in considerable amounts. Furthermore, for the first time, the presence of leontopodic acid, a greatly substituted derivative of glucaric acid, was detected in the species.
Podophyllotoxin (PPT) is a precursor for the synthesis of drugs against cancer and other diseases. The present sources of PPT (Sinopodophyllum hexandrum and Podophyllum peltatum) are endangered species, with PPT production highly dependent on their growing conditions. In connection with the identification of new sources of PPT, the present study aimed to recover PPT from Juniperus virginiana leaves via atmospheric or high pressure extraction methods with a focus on using eco-friendly solvents. PPT quantification was determined by UHPLC/HRMS/MS. A thorough study of conventional extraction was carried out to reveal the optimal conditions (solvent ethyl acetate at room temperature and a duration of 1 h) for maximizing the PPT recovery (about 30 mg/g of dry extract and 3 mg/g of dry initial plant material). Peleg’s equation was applied for process kinetics modeling. The best PPT content in the final dry extract (42–45 mg/g of dry extract) was obtained by high pressure methods under supercritical (scCO2 with ethanol or ethyl acetate, 30 MPa, 50 °C and 100 min) or accelerated solvent extraction conditions (solvent ethyl acetate, 10.35 MPa, 20 °C and 3 cycles for 15 min). Seasonal stability and storage stability of the raw material were also determined. The present results have potential applications in the pharmacy for the delivery of PPT from juniper leaves.
Sangre de drago, the sap of Croton lechleri Müll. Arg. tree, has been used for centuries in traditional medicine owing to its diverse biological activities. Extracts derived from different parts of the species contain a multitude of phytochemicals with varied applications. Twigs, however, are among the least studied parts of the plant. This study unveils new biological activities of Croton lechleri twig extracts recovered by applying Soxhlet and advanced green techniques. For all extracts, total phenolic content and antioxidant activity were determined. Subsequently, four were selected, and their cytotoxic effects were assessed on both normal (HaCat) and malignant melanoma (A375) skin cell lines using the MTT assay and trypan blue exclusion assay. All showed dose-dependent cytotoxicity, with the Soxhlet ethanol extract demonstrating the highest selectivity towards A375 cells over HaCat cells. The extracts induced apoptosis and necrosis, as confirmed by Annexin V/PI dual-labeling and flow cytometry, highlighting their ability to trigger programmed cell death in cancer cells. The selective inhibition of cell cycle progression in A375 compared to HaCat observed both for Soxhlet ethanol and pressurized ethanol extracts induces cell cycle arrest at multiple points, primarily in the G1 and G2/M phases, and significantly reduces DNA synthesis as evidenced by the decrease in the S-phase population, confirmed by the EdU assay. Consequently, the Soxhlet extract composition was analyzed using LC-MS, which revealed their richness in polyphenolic compounds, particularly flavonoids from the flavonol subclass.