Recent advancements in analytical strategies have enabled the efficient extraction and characterization of bioactive compounds from agri-food bio-residues, emphasizing green chemistry and circular economy principles. This review highlights the valorization of several agri-food bio-residues for the extraction of high-value-added bioactive compounds, particularly polyphenols, tocopherols, carotenoids, and fatty acids, as a biorefinery approach. To this end, the adoption of environmentally friendly extraction technologies is essential to improve performance, reduce energy consumption, and minimize costs. This study therefore examines emerging methodologies such as supercritical fluid extraction, pressurized liquid extraction, pulsed electric fields, and matrix solid-phase dispersion, highlighting their advantages and limitations. Additionally, the chemical characterization of these bioactive compounds is explored through spectrophotometric and high-resolution chromatographic techniques, crucial for their accurate identification and quantification. This is complemented by an analysis of bioactivity assays evaluating antioxidant, antimicrobial, anticancer, neuroprotective, and anti-inflammatory properties, with a focus on their applications in the food, pharmaceutical, and cosmetic industries. However, the analytical control of toxic compounds, such as alkaloids, in these bio-residues is undoubtedly needed. Ultimately, this approach not only promotes sustainability but also contributes to the development of eco-friendly solutions in various industries.

Alzheimer’s disease (AD) is the most serious and prevalent neurodegenerative disorder still without cure. Since its aetiology is diverse, recent research on anti-AD drugs has been focused on multi-target compounds. In this work, seven novel hybrids (RIV–BIM) conjugating the active moiety of the drug rivastigmine (RIV) with 2 isomeric hydroxyphenylbenzimidazole (BIM) units were developed and studied. While RIV assures the inhibition of cholinesterases, BIM provides further appropriate properties, such as inhibition of amyloid β-peptide (Aβ) aggregation, antioxidation and metal chelation. The evaluated biological properties of these hybrids included antioxidant activity; inhibition of acetylcholinesterase (AChE), butyrylcholinesterase (BChE) and Aβ₄₂ aggregation; as well as promotion of cell viability and neuroprotection. All the compounds are better inhibitors of AChE than rivastigmine (IC₅₀ = 32.1 µM), but compounds of series 5 are better inhibitors of BChE (IC₅₀ = 0.9−1.7 µM) than those of series 4. Series 5 also showed good capacity to inhibit self- (42.1−58.7%) and Cu(II)-induced (40.3−60.8%) Aβ aggregation and also to narrow (22.4−42.6%) amyloid fibrils, the relevant compounds being 5b and 5d. Some of these compounds can also prevent the toxicity induced in SH-SY5Y cells by Aβ₄₂ and oxidative stress. Therefore, RIV–BIM hybrids seem to be potential drug candidates for AD with multi-target abilities.

Obtaining polyphenols from horticultural waste is an emerging trend that enables the valorization of resources and the recovery of value-added compounds. However, a pivotal point in the exploitation of these natural extracts is the assessment of their chemical stability. Hence, this study evaluates the effect of temperature storage (20 and −20 °C) and drying methods on the phenolic composition and antioxidant activity of clementine and lemon peel extracts, applying HPLC-DAD-MS, spectrophotometric methods, and chemometric tools. Vacuum-drying treatment at 60 °C proved to be rather suitable for retaining the highest antioxidant activity and the hesperidin, ferulic, and coumaric contents in clementine peel extracts. Lemon extracts showed an increase in phenolic acids after oven-drying at 40 °C, while hesperidin and rutin were sustained better at 60 °C. Hydroethanolic extracts stored for 90 days preserved antioxidant activity and showed an increase in the total phenolic and flavonoid contents in lemon peels, unlike in clementine peels. Additionally, more than 50% of the initial concentration was maintained up to 51 days, highlighting a half-life time of 71 days for hesperidin in lemon peels. Temperature was not significant in the preservation of the polyphenols evaluated, except for in rutin and gallic acid, thus, the extracts could be kept at 20 °C.