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In response to the global challenge of food wastage and high perishability of blackberries, this study evaluated the use of ultrasound-assisted hot air drying (US-HAD) to convert downgraded blackberries into powders, comparing it with traditional hot air drying (HAD). US-HAD reduced the drying time and achieved a final moisture content of 12%. Physicochemical analyses (colourimetry, total soluble solids, titratable acidity, and total phenolic content) were conducted on fresh fruit, powders, and fortified cookies. US-HAD cookies exhibited promising antioxidant activity, with ABTS values ranging from 8.049 to 8.536 mmol TEAC/100 g and DPPH values from 8.792 to 9.232 mmol TEAC/100 g, significantly higher than control cookies. The TPC was 13.033 mgGAE/g in HAD cookies and 13.882 mgGAE/g in US-HAD cookies. UHPLC-ESI-MS analysis showed an increase in phenolic compounds content in fortified cookies compared to the control. Sensory analysis highlighted a superior blackberry flavour and overall acceptability in US-HAD cookies, with statistical analysis confirming their superior nutritional and sensory qualities. Integrating US-HAD blackberry powder into cookies helps reduce food waste and enhances the nutritional profiles of baked goods, offering functional foods with health benefits. This work provides a scientific basis for developing enriched functional cookies, offering a healthy and sustainable alternative for utilising damaged fruits.

Monoamine oxidase and xanthine oxidase inhibitors represent useful multi-target drugs for the prevention, attenuation, and treatment of oxidative damage and neurodegenerative disorders. Chimeric molecules, constituted by naturally derived compounds linked to drugs, represent lead compounds to be explored for the discovery of new synthetic drugs acting as enzyme inhibitors. We have previously reported that seven hydroxytyrosol-donepezil hybrid compounds play a protective role in an in vitro neuronal cell model of Alzheimer’s disease. In this work, we analyzed the effects exerted by the hybrid compounds on the activity of monoamine oxidase A (MAO-A) and B (MAO-B), as well as on xanthine oxidase (XO), enzymes involved in both neurodegenerative disorders and oxidative stress. The results pointed to the identification, among the compounds tested, of selective inhibitors between the two classes of enzymes. While the 4-hydroxy-3-methoxyphenethyl 1-benzylpiperidine-4-carboxylate- (HT3) and the 4-hydroxyphenethyl 1-benzylpiperidine-4-carboxylate- donepezil derivatives (HT4) represented the best inhibitors of MAO-A, with a scarce effect on MAO-B, they were almost ineffective on XO. On the other hand, the 4,5-dihydroxy-2-nitrophenethyl 1-benzylpiperidine-4-carboxylate donepezil derivative (HT2), the least efficient MAO inhibitor, acted like the best XO inhibitor. Therefore, the differential enzymatic targets identified among the hybrid compounds synthesized enhance the possible applications of these polyphenol-donepezil hybrids in neurodegenerative disorders and oxidative stress.

A renewed understanding of eco-friendly principles is moving the industrial sector toward a shift in the utilization of less harmful solvents as a main strategy to improve manufacturing. Green analytical chemistry (GAC) has definitely paved the way for this transition by presenting green solvents to a larger audience. Among the most promising, surely DESs (deep eutectic solvents), NaDESs (natural deep eutectic solvents), HDESs (hydrophobic deep eutectic solvents), and HNaDESs (hydrophobic natural deep eutectic solvents), with their unique features, manifest a wide-range of applications, including their use as a means for the extraction of small bioactive compounds. In examining recent advancements, in this review, we want to focus our attention on some of the most interesting and novel ‘solvent-free‘ extraction techniques, such as microwave-assisted extraction (MAE) and ultrasound-assisted extraction (UAE) in relation to the possibility of better exploiting DESs and NaDESs as plausible extracting solvents of the phenolic compounds (PCs) present in different matrices from olive oil components, such as virgin olive pomace, olive leaves and twigs, virgin and extra virgin olive oil (VOO and EVOO, respectively), and olive cake and olive mill wastewaters (OMWW). Therefore, the status of DESs and NaDESs is shown in terms of their nature, efficacy and selectivity in the extraction of bioactive phytochemicals such as secoiridoids, lignans, phenolic acids and alcohols. Related studies on experimental design and processes’ optimization of the most promising DESs/NaDESs are also reviewed. In this framework, an extensive list of relevant works found in the literature is described to consider DESs/NaDESs as a suitable alternative to petrochemicals in cosmetics, pharmaceutical, or food applications.

Citrus fruits exert various beneficial health effects due to the large amount of polyphenols they contain. Citrus peels, often considered food waste, contain several health-promoting polyphenols. Among these, flavonoids have long been quantified through colorimetric assays which, if not adequately applied, can lead to conflicting results. Flavonoids possess strong antioxidant properties and can decrease circulating free radicals, thereby reducing oxidative stress phenomena. Quantifying flavonoids and properly estimating their antioxidant capacity allows us to predict plausible beneficial effects of citrus fruits on human health. The aim of this research was to analyze the advantageous phenolic compounds found in the peels of citrus fruits commonly found in the Mediterranean region. The objective was to measure their antioxidant capacity and ability to neutralize free radicals. To achieve this purpose, UV-visible spectrophotometric analyses, liquid chromatography (LC) and Electron Paramagnetic Spectroscopy (EPR) were utilized and compared, finally suggesting an innovative approach for assessing the overall flavonoid content by the nitrite-aluminum assay. HPLC data demonstrated that hesperidin was the most abundant flavonoid in all peel extracts except for orange peels, in which naringin was the predominant flavonoid. The total flavonoid content was greater than 1.3 mg/mL in all extracts, with tangerine and orange yielding the best results. Citrus peel polyphenols exerted strong antioxidant and free radical scavenging effects, inhibiting up to 75% of the free radicals used as reference in the EPR analyses.

The beneficial properties of extra virgin olive oil (EVOO) on lipids blood levels were recognized by the European Food Safety Authority (EFSA) with a health claim, specifically referring to EVOOs containing at least 5 mg of hydroxytyrosol and its secoiridoids derivatives per 20 g of oil. The main purpose of the work was to characterize the phenolic profile of two commercially available Calabrian monovarietal EVOOs (Nocellara del Belice, VN; Dolce di Rossano, VDR), and to study the effect of one-year storage on secoiridoids composition, by monthly controls. A new UHPLC-ESI-HRMS method was developed and validated, thus facilitating the EFSA claim application and allowing producers to valorize their products. Seven biologically active compounds were chosen: tyrosol, hydroxytyrosol, oleocanthal, oleacein, oleuropein aglycone, verbascoside, and oleuropein. LODs and LOQs were 0.001–0.02 mg g−1 and 0.002–0.08 mg g−1, respectively. The variation coefficients were ≤20% and the percentage of recovery was between 89–109%. During the 12-month storage period, the concentration of selected compounds ranged between 1258.78–1478.91 mg Kg−1 for VN, and 1408.22–2071.45 mg Kg−1 for VDR, with a decrease of 15% and 32% respectively. The method allows an accurate quantification of EVOO phenols thus being useful to certify the nutraceutical properties of olive oil.

Alzheimer’s disease (AD) is the most common neurodegenerative pathology among progressive dementias, and it is characterized by the accumulation in the brain of extracellular aggregates of beta-amyloid proteins and neurofibrillary intracellular tangles consisting of τ-hyperphosphorylated proteins. Under normal conditions, beta-amyloid peptides exert important trophic and antioxidant roles, while their massive presence leads to a cascade of events culminating in the onset of AD. The fibrils of beta-amyloid proteins are formed by the process of fibrillogenesis that, starting from individual monomers of beta-amyloid, can generate polymers of this protein, constituting the hypothesis of the “amyloid cascade”. To date, due to the lack of pharmacological treatment for AD without toxic side effects, chemical research is directed towards the realization of hybrid compounds that can act as an adjuvant in the treatment of this neurodegenerative pathology. The hybrid compounds used in this work include moieties of a hydroxytyrosol, a nitrohydroxytyrosol, a tyrosol, and a homovanillyl alcohol bound to the N-benzylpiperidine moiety of donepezil, the main drug used in AD. Previous experiments have shown different properties of these hybrids, including low toxicity and antioxidant and chelating activities. The purpose of this work was to test the effects of hybrid compounds mixed with Aβ 1–40 to induce fibrillogenesis and mimic AD pathogenesis. This condition has been studied both in test tubes and by an in vitro model of neuronal differentiated human SH-SY5Y neuroblastoma cells. The results obtained from test tube experiments showed that some hybrids inhibit the activity of the enzymes AChE, BuChE, and BACE-1. Cell experiments suggested that hybrids could inhibit fibrillogenesis, negatively modulating caspase-3. They were also shown to exert antioxidant effects, and the acetylated hybrids were found to be more functional and efficient than nonacetylated forms.

Olive tree by-products have been deeply studied as an invaluable source of bioactive compounds. Several in vitro and in vivo studies showed that olive leaf extract (OLE) has anti-inflammatory and antioxidant properties. Here, we wanted to assess the valuable benefits of two less-studied OLE components—3,4-DHPEA-EDA (Oleacin, OC) and 3,4-DHPEA-EA (Oleuropein-Aglycone, OA)—directly purified from OLE using a cost-effective and environmentally sustainable method, in line with the principles of circular economy. OLE, OC and OA were then tested in human cellular models involved in acute and chronic inflammation and in the pathogenesis of viral infections, i.e., lipopolysaccharide (LPS)-treated monocyte/macrophages (THP-1) and endothelial cells (HUVECs), senescent HUVECs and Poly(I:C)-treated small airway epithelial cells (hSAECs). Results showed that OC and OA are efficient in ameliorating almost all of the pro-inflammatory readouts (IL-1β, TNF-α, IL-8, ICAM, VCAM) and reducing the release of IL-6 in all the cellular models. In hSAECs, they also modulate the expression of SOD2, NF-kB and also ACE2 and TMPRSS2, whose expression is required for SARS-CoV-2 virus entry. Overall, these data suggest the usefulness of OLE, OC and OA in controlling or preventing inflammatory responses, in particular those associated with viral respiratory infections and aging.

Cold-pressed pomegranate seed oil (PSO) is a product of the extraction of non-edible pomegranate seeds. Its unique chemical composition in terms of both polyunsaturated fatty acids, especially punicic acid (PA), and secondary metabolites, such as phytosterols, tocopherols and phenols, make it an interesting functional ingredient for food enrichment. It is not clear if the biomarkers profile of PSO depends to factors connected to the geographical origin of seeds. This work presents a statistical comparative analysis, concerning biomolecules composition and geographical origin of 32 commercial cold-pressed PSOs, performed by principal component analysis. The study discriminates between Turkish and Italian PSOs, on the base of the fatty acid profile and phytosterols, and not on the tocopherols and phenols. These results confirmed PA as the main characteristic biomarker of oil genuineness and, for the first time, disclosed a statistically relevant variability of phytosterols, which can be proposed as quality biomarkers for discrimination of geographical origins.

Immunosenescence and inflammaging facilitate the insurgence of chronic diseases. The Mediterranean diet is a non-invasive intervention to improve the chronic low-grade inflammatory status associated with aging. Olive oil oleuropein (OLE) and hydroxytyrosol (HT) demonstrated a controversial modulatory action on inflammation in vitro when tested at concentrations exceeding those detectable in human plasma. We studied the potential anti-inflammatory effects of OLE and HT at nutritionally relevant concentrations on peripheral blood mononuclear cells (PBMCs) as regards cell viability, frequency of leukocyte subsets, and cytokine release, performing an age-focused analysis on two groups of subjects: Adult (age 18–64 years) and Senior (age ≥ 65 years). OLE and HT were used alone or as a pre-treatment before challenging PBMCs with lipopolysaccharide (LPS). Both polyphenols had no effect on cell viability irrespective of LPS, but 5 µM HT had an LPS-like effect on monocytes, reducing the intermediate subset in Adult subjects. OLE and HT had no effect on LPS-triggered release of TNF-α, IL-6 and IL-8, but 5 µM HT reduced IL-10 secretion by PBMCs from Adult vs. Senior group. In summary, nutritionally relevant concentrations of OLE and HT elicit no anti-inflammatory effect and influence the frequency of immune cell subsets with age-related different outcomes.

The rheological and chemical quality of pasta samples, which were obtained using the durum wheat semolina fortified with the hemp seed solid residue, after oil extraction, sieved at 530 μm (Hemp 1) or 236 μm (Hemp 2) at different percentages of substitution (5%, 7.5%, and 10%, were evaluated. The total polyphenolic content in hemp flour was quantified in the range of 6.38–6.35 mg GAE/g, and free radical scavenging was included in the range from 3.94–3.75 mmol TEAC/100 g in Hemp 1 and Hemp 2, respectively. The phenolic profiles determined by UHPLC-ESI/QTOF-MS showed that cannabisin C, hydroxycinnamic and protocatechuic acids were the most abundant phenolic compounds in both hemp flours. Among the amino acids, isoleucine, glutamine, tyrosine, proline, and lysine were the most abundant in raw materials and pasta samples. Although the hemp seeds were previously subjected to oil extraction, hemp flours retain about 8% of oil, and the fatty acids present in the largest amount were linoleic acid and α-linolenic acid. Characterization of the minerals showed that the concentration of macro and trace elements increased according to fortification percentage. Sensory evaluation and cooking quality indicated that the best performance in terms of process production and consumer acceptance was obtained using Hemp 2 at 7.5%. Hemp supplementation could be a potential option for producing high-quality, nutritionally rich, low-cost pasta with good color and functionality.

It is well-accepted that the endogenous antioxidant protection system progressively decays in elderly people, and that the oxidative stress contributes to different neurodegenerative disorders such as Alzheimer’s Diseases (AD). The lower incidence of AD in countries which feature the Mediterranean Diet was associated to the high consumption of extra virgin olive oil and its polyphenolic fraction, in particular hydroxytyrosol. The protective role of these bio-phenols against oxidative stress, suggested that we combine their antioxidant/free radical scavenging activity with donepezil, an active ingredient which has just been approved for the treatment of AD. Different synthetic strategies were tested to conjugate the two different synthons in good yields. Additionally, a nitro-hydroxytyrosol derivative was synthesized to extend the application to other neurodegeneration inflammatory models. Then, their bioactivity was measured in different chemical and biological tests on a human neuroblastoma cell line (SHSY-5Y). Remarkable results on cell viability and the regulation of the redox state of cells were obtained. All hybrids showed negligible cell death under 1 μM and are stable and non toxic. Reactive oxygen species (ROS) measurements showed that the nitro-hybrid was the more effective one at reducing the ROS amount to physiological values. Then, in light of the bio-metal hypothesis of diverse neurodegenerative disorders, we tested these new compounds on the chelation properties of redox-active metals. The nitro-hybrid was able to chelate all of the tested metal cations, suggesting that we propose it as potential lead compound for a new class of neuroprotective antioxidant agents.

Inulin is considered a dietary fiber and represents a noteworthy ingredient for food biofortification due to its health effects and its neutral taste. The aim of the work was the evaluation of the quality of pasta produced using whole-meal flours of two ancient Sicilian landraces (Senatore Cappelli-CAP and Timilia—TIM) fortified with two types of inulin (long-chain topinambur inulin IT and low-chain chicory inulin IC), at two different levels of substitution (2 and 4%) to evaluate its possible effect on α-amylase inhibition. The color indices L* and a* were mainly influenced by cultivars, while IT improved the sensory attributes, mainly the elasticity sensation, and influenced less the other sensory attributes: adhesiveness, color, odor, taste, and Over Quality Score for both landraces. The cooking quality was linked mainly to the landrace used, due to the very different gluten matrix of CAP and TIM. IC and IT showed promising α-Amy inhibitory activity with comparable IC50 values of 0.45 ± 0.04 and 0.50 ± 0.06 mg/mL. The enrichment of spaghetti with inulin with an inhibitory effect on α-amylase determined the hypoglycemic properties of pasta, thus lowering the corresponding IC50 value.

The benzimidazole ring of the heterocyclic pharmacophores is one of the most widespread and studied systems in nature. The benzimidazole derivative synthesis study is a crucial point for the development of a clinically available benzimidazole-based drug. Here, we report a simple microwave assisted method for the synthesis of 1,2-disubstituted benzimidazoles. The combination of the molar ratio of N-phenyl-o-phenylenediamine:benzaldehyde (1:1) using microwave irradiation and only 1% mol of Er(OTf)3 provides an efficient and environmental mild access to a diversity of benzimidazoles under solvent-free conditions. The proposed method allows for the obtainment of the desired products in a short time and with very high selectivity.

Natural compounds have historically had a wide application in nutrition. Recently, a fundamental role has been identified for essential oils extracted from aromatic plants for their nutritional, antimicrobial, and antioxidant properties, and as food preservatives. In the present study, essential oils (EOs) from ten aromatic plants grown in Calabria (Italy), used routinely to impart aroma and taste to food, were evaluated for their antibacterial activity. This activity was investigated against Escherichia coli strain JM109, and its derived antibiotic-resistant cells selected by growing the strain at low concentrations of ampicillin, ciprofloxacin, and gentamicin by measuring the minimum inhibitory concentration (MIC) and the minimum bactericidal concentration (MBC). Although all the essential oils showed bactericidal activity, those from Clinopodium nepeta, Origanum vulgare, and Foeniculum vulgare displayed the greatest inhibitory effects on the bacterial growth of all cell lines. It is plausible that the antibacterial activity is mediated by epigenetic modifications since the tested essential oils induce methylation both at adenine and cytosine residues in the genomes of most cell lines. This study contributes to a further characterization of the properties of essential oils by shedding new light on the molecular mechanisms that mediate these properties.

Paclitaxel (PTX) is one of the most successful antineoplastic drugs and is widely used for the treatment of many forms of advanced and refractory cancer. Unfortunately, various drawbacks including non-selective cytotoxicity, poor water solubility and low bioavailability limit its clinical use. The aim of this study was to characterize a novel colloidal system made up of the natural protein zein, that would be able to efficiently retain the anticancer compound and increase its in vitro pharmacological effects. In fact, zein has promising characteristics that render it a potential material to be used in drug delivery application. The influences of temperature, pH and serum incubation on the stability of these particles, entrapment efficiency of PTX and in vitro toxicity on different cancer cell lines were evaluated. The nanosystems containing PTX demonstrated suitable storage stability, and were not destabilized by temperatures of up to 50 °C, pH alterations, the freeze-drying process or serum proteins. The encapsulation of PTX did not destabilize the structure of the zein nanoparticles and a suitable drug entrapment efficiency resulted. PTX-loaded zein nanoparticles showed an increased toxicity on different cancer cell lines with respect to the free drug, confirming its potential application in preclinical and clinical investigations.

The worldwide increased difficulty to counteract gastrointestinal nematode (GIN) infection in sheep, due to progressing anthelmintic resistance, has led to the evaluation of other alternative helminth control options, mainly from plants. The anthelmintic efficacy of an aqueous Punica granatum macerate was evaluated in sheep naturally infected by GIN in southern Italy. The macerate was chemically characterized by chromatographic analysis coupled with high-resolution mass spectrometry (LC/HRMS) and an aliquot was concentrated to obtain a dry extract. A part was characterized, the remaining washed with methanol to obtain an insoluble residue and methanol phase. In the methanol fraction, the quantitatively predominant gallic acid was purified to obtain the pure molecule. The three fractions thus obtained were used for in vitro studies (i.e., egg hatch test) to verify anthelmintic efficacy. For this purpose, fecal samples were collected from sheep naturally infected by GINs. Fractions were diluted in H2O/DMSO 0.5% at 1.00, 0.5, 0.25, 0.125, 0.05, and 0.005 mg/mL concentrations. Thiabendazole (0.25 and 0.5 mg/mL) and deionized water were used as positive and negative controls, respectively. Egg hatch test results indicated that all fractions caused a significant (p < 0.05) egg hatch inhibition within 48 h of exposure highlighting a high (>82%) efficacy in vitro at all tested doses. Maximal egg hatching inhibition effect was exhibited by the methanol fraction (99.3% and 89.3% at 1 and 0.005 mg/mL concentrations), followed by the insoluble residue and gallic acid (94.7% and 85.3% and 94.0% and 82.7% at 1 and 0.005 mg/mL, respectively). The current study validated the anthelmintic potential of traditional P. granatum macerate against GIN infection in sheep, thus highlighting the role of gallic acid as principal component and justifying a need to undertake further in vivo studies on these ethno-veterinary remedies.

The use of toxic solvents, high energy consumption, the production of waste and the application of traditional processes that do not follow the principles of green chemistry are problems for the pharmaceutical industry. The organic synthesis of chemical structures that represent the starting point for obtaining active pharmacological compounds, such as benzimidazole derivatives, has become a focal point in chemistry. Benzimidazole derivatives have found very strong applications in medicine. Their synthesis is often based on methods that are not convenient and not very respectful of the environment. A simple montmorillonite K10 (MK10) catalyzed method for the synthesis of benzimidazole derivatives has been developed. The use of MK10 for heterogeneous catalysis provides various advantages: the reaction yields are decidedly high, the work-up procedures of the reaction are easy and suitable, there is an increase in selectivity and the possibility of recycling the catalyst without waste formation is demonstrated. The reactions were carried out in solvent-free conditions and in a short reaction time using inexpensive and environmentally friendly heterogeneous catalysis. It has been shown that the reaction process is applicable in the industrial field.

In this new century, sustainable development challenges chemical sciences to develop new and clean technological processes. The agri-food industry produces significant quantities of waste, raising significant economic and environmental concerns. Food waste valorization using environmentally friendly procedures is of increasing importance. This study describes the use of several Natural Deep Eutectic Solvents (NADESs) for the microwave-assisted extraction (MAE) of valuable bioactive phenolic compounds from olive oil processing wastes. The extracted samples were characterized by liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOF/MS) analysis and the quantification of the phenolic compounds was performed by HPLC analysis. The obtained data were compared with those obtained using water as the solvent in the same extraction conditions. The extraction process is nontoxic, simple and selective and meets most of the criteria to be considered as a sustainable process, with the solvents arising directly from nature.

A simple and eco-friendly montmorillonite K10 (MK10)-catalyzed method for the synthesis of cyclopentenone derivatives from biomass-produced furfural has been developed. The versatility of this protocol is that the reactions were performed under solvent-free conditions and in a short reaction time under heterogeneous catalysis. Montmorillonite K10 is mostly explored as a heterogeneous catalyst since it is inexpensive and environmentally friendly.