Molecules doi: 10.3390/molecules31111836

Authors: Luisa Mattoli Andrea Lugli Michela Burico Giada Fodaroni Denise Decarli Mattia Gianni Anna Maidecchi Giulia Antonini Silvia Tondi Anna Gaetano Valentina Fiordelli Rita Pagiotti Jacopo Lucci Claudio Buttarini Stefano Garetto Raffaele Saladino Donatella Pietrella Valentina Mercati Emiliano Giovagnoni

Populus nigra buds contain resinous exudates rich in flavonoids, phenolic acids, terpenoids and other bioactive constituents. These exudates are the main botanical source of European Poplar-type propolis. Since hive-collected propolis shows strong botanical, geographical and hive contaminant variability, P. nigra bud resin exudate represents an attractive, standardizable and reproducible alternative for obtaining natural-complex ingredients. This study investigates the compositional relationship between Propolgemma® standardized P. nigra buds (PBHE) and European propolis (PHE) hydroalcoholic extracts through integrated analytical approaches and evaluates the functional bioactivity of PBHE and a related oral spray formulation (Propolgemma® spray forte, PBHE-SF). Untargeted metabolomic fingerprinting revealed clear clustering of P. nigra bud exudate with European propolis, demonstrating high compositional similarity. Targeted analyses confirmed that PBHE belongs to the poplar-type propolis family, while retaining additional bud-derived constituents such as salicylates, lignins and tannins, typical of bud tissue and largely absent from hive-collected propolis. Functionally, PBHE showed concentration-dependent antioxidant activity and significant inhibition of Streptococcus pyogenes biofilm at sub-MIC levels. PBHE, incorporated into a patented oral spray formulation (PBHE-SF), demonstrated strong mucoadhesion, high resistance to salivary wash-off, retention of antioxidant flavonoids on epithelial substrates and a mechanical barrier effect, reducing LPS-induced IL-6 release by 39%. It also showed dispersion of pre-formed S. pyogenes biofilms. PBHE emerges as a reproducible, plant-derived, bee-independent alternative to European propolis. Its chemical consistency, functional reliability, independence from bee foraging and from hive-derived contaminants improve the therapeutic potential on mucosal protection in medical device formulations and the suitability for scalable, controlled and industrially sustainable production.

Molecules doi: 10.3390/molecules31111837

Authors: Patrycja Gazda Paweł Glibowski

Metabolic disorders such as obesity, type 2 diabetes, and lipid disorders are major health challenges worldwide. There is increasing interest in the role of food-derived antioxidants in the context of metabolic disorders due to their documented antioxidant activity. Antioxidants such as flavonoids and polyphenols neutralize reactive oxygen species and reduce oxidative stress, which can affect cell function and metabolic processes. Anthocyanins, curcumin, and resveratrol exhibit physiological and pharmacological properties such as antioxidant, anti-inflammatory, anti-cancer, anti-obesity, and anti-diabetic effects. The main aim of this systematic review is to comprehensively evaluate and synthesize the current scientific evidence on the role of anthocyanins, curcumin, and resveratrol in the prevention and management of metabolic disorders, with a focus on obesity, type 2 diabetes, and dyslipidemia. Databases such as PubMed and Embase were searched, and the final selection included 105 studies that met the inclusion criteria. The analyzed studies demonstrated that anthocyanin supplementation (up to 320 mg/day) was associated with reductions in inflammatory markers such as IL-6 and TNF-α, improvements in HDL cholesterol, and modest reductions in HbA1c (~0.3–0.5%). Curcumin supplementation was associated with decreases in body weight (up to 0.82 kg), BMI (up to 0.30 kg/m2), triglycerides, total cholesterol, and fasting glucose levels. Resveratrol showed mixed but potentially beneficial effects on insulin sensitivity, oxidative stress markers, and lipid metabolism, although the clinical outcomes remained inconsistent across studies. These findings suggest that the antioxidant effects of anthocyanins, curcumin, and resveratrol may be related to their ability to suppress oxidative stress and inflammatory processes, thereby contributing to improvements in glucose and lipid metabolism. The conclusions from this analysis may contribute to a better understanding of the role of antioxidants in the management of metabolic health and indicate directions for future research in this area.

Molecules doi: 10.3390/molecules31111834

Authors: Adrian-Dan Rășinar Isidora Radulov Adina Berbecea Silvia Pătruică

Bee venom variability is driven by environmental and nutritional factors, yet their integrated effects remain poorly understood. This study provides a novel, comprehensive assessment combining dietary treatments with real-time environmental monitoring to evaluate their joint influence on the physico-chemical properties, total amino acid, mineral composition, and heavy metal content of Apis mellifera venom. A total of 32 samples collected between April and July 2025 were analyzed under both artificial feeding and natural foraging conditions. Moisture ranged from 11.2% to 19.2%, while pH remained stable (5.6–6.25). Total amino acids varied between 344.0 and 409.5 mg/g, with maximum values during the acacia period (>400 mg/g). Potassium was the dominant macroelement (3.19–11.37 mg/g), followed by Ca (0.80–3.68 mg/g) and P (0.31–1.84 mg/g). Microelements such as Fe (0.11–0.98 mg/g) and Mn (1.19–8.85 µg/g) showed pronounced seasonal variability. Lead reached up to 36.18 µg/g during natural foraging, while Cd (0.30–3.97 µg/g) was mainly associated with artificial feeding. By integrating nutritional and microclimatic determinants, this study demonstrates that floral origin and seasonal dynamics are the primary drivers of venom quality, while supplementation exerts secondary effects, and highlights the potential of bee venom as a sensitive bioindicator of environmental exposure.

Molecules doi: 10.3390/molecules31111835

Authors: Zitong Sang Haolin Han Fangfang Qi Guoqiang Pan Guanghui Zhang Shaolong Qiu Yan Wei Zhenzhen Zhang Hengjia Zhang Jinxing Xia

Tomato yellow leaf curl virus (TYLCV) is a major plant pathogen that spreads worldwide through persistent circulative transmission by Bemisia tabaci. During transmission, TYLCV crosses several physiological barriers in the insect vector, evading immune defenses and altering host metabolic pathways to facilitate viral accumulation. Polyamines, essential for maintaining nucleic acid stability and promoting cellular processes, are known to play a critical role in viral accumulation. However, their role in TYLCV accumulation within B. tabaci is not well understood. Here, we demonstrate that TYLCV infection leads to significant alterations in polyamine levels in B. tabaci, with polyamine availability positively affecting viral DNA accumulation. Polyamine availability leads to higher viral loads and suppresses the expression of immune and MAPK signaling genes. These findings provide new insights into virus–vector and metabolic interactions underlying viral persistence in insect vectors.

Molecules doi: 10.3390/molecules31111833

Authors: Achilleas Kechagias Andreas Giannakas Panagiotis Stathopoulos Maria Xenaki Areti A. Leontiou Anna Kopsacheili Nikolaos Chalmpes Emmanuel P. Giannelis Constantinos E. Salmas Charalampos Proestos Aris E. Giannakas

Olive leaves are an abundant agro-industrial by-product rich in oleuropein, yet they remain largely underutilized. The objective of this study is to a) develop a green microwave-assisted extraction (MAE) method for an oleuropein-rich extract, b) encapsulate it into edible natural zeolite to form OLE@NZ nanohybrids, and, c) evaluate their application in fortified salt and active gelatin films. MAE using only water at 96 °C for 5 min yielded a dry extract with 25.4% (w/w) oleuropein and a total phenolic content of 781 mg GAE/100 mL. The extract was successfully adsorbed onto clinoptilolite-type zeolite and the resulting nanohybrids showed strong antioxidant activity (EC50,DPPH = 2.74 mg, TPC = 426 mg GAE/g). A fortified salt containing 5% w/w OLE@NZ fully preserved the nanohybrid’s antioxidant activity. Extruded gelatin films incorporating 5–15% OLE@NZ exhibited a concentration-dependent increase in antioxidant activity (up to 14-fold higher than the blank film), together with a 5- to 7-fold enhancement, while maintaining good mechanical properties. The total phenolic content of the films correlated linearly with nanohybrid loading, with phenolic recovery of 68% both at 5 and 10% loading and 58% at 15%). Overall, these findings demonstrate that MAE is a rapid, and environ-mentally friendly approach for obtaining oleuropein-rich olive leaf extract (OLE), while OLE@NZ nanohybrids provide effective antioxidant additives for functional salt formulations and active gelatin films, supporting a circular bioeconomy strategy.

Molecules doi: 10.3390/molecules31111832

Authors: Sicheng Jin Yongan Meng Dongtian Miao Chun Shi Jing Yang Zhengjun Shi Haiyan Yang

Efficient pretreatment is essential for improving the conversion of lignocellulose into fermentable sugars and bioethanol. In this study, choline chloride–monoethanolamine (ChCl-MEA)-based solvent systems containing H2O2, NaHCO3, Na2S, or ethylene glycol were prepared and applied for the pretreatment of Dendrocalamus brandisii. Among the tested systems, ChCl-MEA-Na2S showed the best overall pretreatment performance, achieving 92.8 ± 2.3% delignification and 86.1 ± 1.7% cellulose retention. It also effectively disrupted lignin–carbohydrate associations, reduced lignin shielding and generated a more accessible cellulose-rich substrate for bioconversion. In the following separation enzymatic hydrolysis and fermentation, 92.2 ± 2.2% cellulose in substrate was converted to glucose, and 17.49 ± 0.7 g/L ethanol was obtained via the fermentation of enzymatic hydrolysate. Taking the bioconversion of substrate into consideration, the ChCl-MEA-H2O2 and ChCl-MEA-Na2S were recovered for full component utilization. Especially, the carbon dots produced from the degradation compounds in ChCl-MEA-H2O2 DESs had favorable antioxidation and antibacterial performance due to the oxygen-containing group caused by oxidation of H2O2.

Molecules doi: 10.3390/molecules31111831

Authors: Svetlana A. Kondrashova Shamil K. Latypov

The comparative analysis of calculated and experimental one-bond 31P-31P indirect nuclear spin–spin couplings for a wide range of structures, including P-P bonds, has shown that, on the whole, it is possible to estimate 1JPP fairly accurately using even modest levels of theory. However, in order to reduce systematic errors, it is necessary to carry out a linear correction procedure specific to different groups of compounds. Certain difficulties may arise only for diphosphanes (R1R2P–PR1R2) that are in solution in fast (in NMR time scale) exchange of conformers with close populations. In practice, a relatively simple PBE0/6-31G(d)//PBE0/6-31G(d) combination is sufficient for calculating the 1JPP with practically reliable accuracy. The efficiency of the proposed protocol is demonstrated using the example of more subtle structural features—the isomeric structure. The proposed approach allowed for the absolute sign of 1JPP in a number of cases where it is unknown experimentally.

Molecules doi: 10.3390/molecules31111830

Authors: Abdul Hafeez Gyanendra Sharma Romain Milotskyi Hao Wang Akihiro Shinku Naoki Wada Kenji Takahashi

In this study, a green technique of mechanochemistry was used to prepare superabsorbent polymers (SAPs) from soybean waste (Okara) and bio-based bifunctional itaconic acid (ItA) in a solventless melt-reactive esterification reaction using reactive extruder. SAPs were produced by reaction of ItA with Okara at 120 °C with and/or without the use of crosslinker N,N′-methylenebis(acrylamide) (MBA) in the presence or absence of free radical initiator, potassium peroxodisulfate (KPS). By varying the amounts of ItA and Okara, the effect of MBA and KPS was investigated on water absorption. The esterification of Okara with ItA was confirmed by attenuated total reflectance–Fourier-transform infrared (ATR-FTIR) spectroscopic measurements, while the structural characterization was done using X-ray diffraction, thermal gravimetric analysis, and scanning electron microscopy. Among the twelve SAPs formulations, the highest water absorption of 35.6 g/g of SAP was shown by SAP prepared from Okara/ItA in a ratio of 1 g/3.5 g and crosslinked with 0.5 wt% MBA. All the SAPs showed moderate centrifuge water retention (CWR) capabilities which show their potential for application in sustainable agriculture.

Molecules doi: 10.3390/molecules31111829

Authors: Zhen Sun Junran Wang Jietao Guan Yaoda Mei Wenyu Song Haixu Wang Weiwei Luo Xiang Cai

The development of high-performance cathode materials represents a crucial strategy for enhancing the overall electrochemical performance of aqueous alkaline zinc batteries. The rational design of electrode microstructure and chemical composition can synergistically boost the electrochemical reaction activity, ion/electron transport kinetics, and structural stability. In this work, a composite cathode material, FLG@NixS6/Co4S3/Ni-Co(OH)2, was successfully synthesized via an electrochemical codeposition method. The engineered architecture offers abundant electrochemically active sites, well-defined ion diffusion pathways, and continuous electron conduction networks. Moreover, the strong interaction among the constituent phases effectively regulates and accelerates the redox reaction kinetics. When integrated into an aqueous alkaline zinc battery, the device attains a high specific capacity of 385 mAh g−1 at 2 A g−1, excellent rate capability (287 mAh g−1 at 80 A g−1), a gravimetric energy density of 590 Wh kg−1, a power density of 128.57 kW kg−1, and remarkable cycling stability, with 100% capacity retention maintained after 20,000 cycles. Overall, this study proposes a scalable and rational composite strategy for designing high-performance electrode materials for next-generation electrochemical energy storage systems.

Molecules doi: 10.3390/molecules31111828

Authors: Weronika Magdalena Jabłońska Urszula Guzik Danuta Wojcieszyńska

The increasing presence of pharmaceutical compounds in aquatic environments poses a significant challenge for wastewater treatment systems worldwide. Among these emerging contaminants, bicyclic non-steroidal anti-inflammatory drugs (NSAIDs) are particularly concerning due to their high consumption, partial metabolism, and long-lasting persistence in wastewater. This review was prepared critically based on popular databases such as PubMed and the Google Scholar website, and using the modern Nested Knowledge platform. The bibliometric analysis was performed using the VosViewer program with the keywords co-occurrence method. The review aims to systematically compile and synthesize current knowledge on the impact of bicyclic non-steroidal anti-inflammatory drugs (NSAIDs) on biological wastewater treatment systems, with particular emphasis on activated sludge. It discusses how these compounds influence microbial community composition, metabolic activity, sludge structure, and overall treatment performance. Furthermore, the distribution of these contaminants in the environment and their degradation efficiency were analyzed. By integrating evidence from both laboratory and industrial studies, this article provides a comprehensive perspective on the environmental risks posed by bicyclic NSAIDs. Our findings also underscore the urgent need for systematic monitoring and adaptive management to mitigate the ecological impact of these widely used pharmaceuticals in the future.

Molecules doi: 10.3390/molecules31111827

Authors: Roko Šantić Marko Kumrić Lovre Martinović Marino Vilović Iris Jerončić Tomić Ivan Cvitković Joško Božić

High-phenolic extra-virgin olive oil (EVOO) is a chemically dynamic bioactive matrix in which cultivar, ripening stage, processing, storage, and digestion shape the final profile of phenolic alcohols and secoiridoids. In inflammatory bowel disease (IBD), chronic intestinal inflammation is associated with barrier dysfunction, dysbiosis, systemic immune activation, endothelial injury, platelet hyperreactivity, and increased cardiovascular risk. This narrative review evaluates whether EVOO phenolics may intersect the gut–endothelium–platelet axis linking IBD to vascular and thromboinflammatory complications. The review focuses on hydroxytyrosol, tyrosol, oleuropein- and ligstroside-derived secoiridoids, oleocanthal, and oleacein, with emphasis on their biosynthetic origin, processing-driven transformations, bioavailability, metabolism, and biological targets. Current evidence supports plausible effects on epithelial barrier integrity, TLR4/NF-κB signalling, Nrf2-mediated antioxidant defence, oxidised LDL formation, endothelial activation, and platelet-related pathways. Nevertheless, direct clinical evidence in IBD patients remains limited, and most cardiovascular-relevant findings are extrapolated from non-IBD human trials, animal studies, or in vitro models. Chemically characterised, biomarker-anchored intervention trials are needed before high-phenolic EVOO can be considered a validated strategy for modifying cardiovascular risk in IBD.

Molecules doi: 10.3390/molecules31111826

Authors: Gabrielle D. Pereira Igor F. de Souza Luana Floriano Osmar D. Prestes Renato Zanella

The increasing occurrence of pesticides in aquatic environments has raised concern due to their potential impact on human health and ecosystems. In this context, the development of sensitive, reliable, and environmentally sustainable analytical methods is essential for monitoring these contaminants. Therefore, the aim of this study was to develop and validate a miniaturized dispersive solid-phase extraction (DµSPE) method for the determination of current-use multiclass pesticides in water samples using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Initially, a simple and rapid sample preparation procedure was developed, in which different experimental variables were evaluated to obtain suitable extraction efficiency. The validated method has a quantification limit of 0.01 µg L−1 and was applied to the determination of pesticides in surface water from different regions in Rio Grande do Sul State, Brazil. In addition, the environmental sustainability of the method was evaluated using the AGREEprep tool, allowing a quantitative and visual assessment of its compliance with the principles of Green Analytical Chemistry. The results demonstrated that the proposed method provides adequate analytical performance for the determination of 28 compounds in water matrices while offering a simple sample preparation procedure with reduced solvent consumption and waste generation.

Molecules doi: 10.3390/molecules31111825

Authors: Federica Armeli Beatrice Mengoni Martina Menin Gregorio Martínez-Sánchez Mauro Martinelli Maurizio Maggiorotti Rita Businaro

In this Reply, we address the criticisms raised by Franzini, Valdenassi, and Chirumbolo concerning our study on the effects of ozonized saline solution (O3SS) on microglial polarization and endothelial responses in vitro. We clarify that the primary aim of the original work was mechanistic, relying on rigorously controlled cellular models that are universally recognized as essential preclinical tools in translational medicine. We reaffirm the validity of our experimental approach, including the preparation and characterization of O3SS based on empirically validated methodologies, direct ozone quantification, and standardized protocols consistent with the existing literature and clinical practice. Concerns regarding ozone chemistry, dose relevance, and hypochlorite formation are addressed through analytical validation, biological threshold considerations, and the use of certified assays. We further justify the choice of BV2 microglia and HUVEC cells as established and widely used models for investigating inflammatory and vascular pathways under reproducible conditions. Statistical analyses, gene expression interpretation, and the absence of comparative pharmacological agents are discussed in the context of the study’s focused objectives. Finally, we place our findings within the established framework of ozone as an indirect pro-oxidant that elicits adaptive redox signaling (“oxidative eustress”), emphasizing the translational relevance of in vitro systems for elucidating early mechanistic events. Overall, we maintain that our study provides a robust, balanced, and evidence-based contribution to the understanding of ozone-derived redox biology.

Molecules doi: 10.3390/molecules31111824

Authors: Nurcan Berber Özge Nur Türkeri Faika Başoğlu Kubra Çıkrıkcı Adem Ergün Nahit Gencer

A new series of isoxazole-fused thiazole–oxazole derivatives (11a–n) was rationally designed and synthesised with the aim of developing potent carbonic anhydrase (CA) I and II inhibitors. The synthesis was achieved in five steps starting from 4-bromoacetophenone, involving key intermediates such as hydroxylamine hydrochloride, hydrazine hydrate, thioisocyanate, and various phenacyl bromide derivatives, using ethanol, triethylamine, tetrahydrofuran (THF), and dimethylformamide (DMF) as solvents. The synthetic route included the formation of a β-ketoester, isoxazole ester, hydrazine adduct, thiourea derivative, and, ultimately, a thiazole ring. The structures of the final compounds were confirmed by 1H-NMR, 13C-NMR, IR spectroscopy, and elemental analysis. All compounds were examined as inhibitors of human carbonic anhydrase (hCA) I and II, and all of them inhibited hCA I and hCA II. Kinetic investigation results revealed that these compounds inhibited hCA I and hCA II in a non-competitive manner. To further explore the molecular basis of their inhibitory activity, in silico studies, including molecular docking and 300 ns molecular dynamics (MD) simulations, were carried out against both CA I and CA II isoforms. These simulations provided detailed insights into the dynamic behaviour, stability, and key binding interactions of the compounds within the enzyme active sites, supporting their potential as promising carbonic anhydrase inhibitors.

Molecules doi: 10.3390/molecules31111822

Authors: Alisa K. Pautova

Neuroscience is a rapidly advancing field; however, a comprehensive understanding of brain function at the molecular, cellular, and systems levels remains incomplete. Neurological and psychiatric disorders represent a major global health burden, highlighting the need for improved diagnostic and therapeutic strategies. Cerebrospinal fluid (CSF) is one of the most informative biofluids for investigating central nervous system (CNS) pathology due to its close biochemical relationship with brain tissue. Recent advances in neurometabolomics, defined as the comprehensive analysis of small-molecule metabolites in CSF, have been driven by the development of highly sensitive and informative mass spectrometry-based techniques. These approaches enable the identification of disease-associated metabolic signatures. This review summarizes current chromatography–mass spectrometry-based methods used in both untargeted and targeted CSF metabolomics, with particular emphasis on their analytical performance, reproducibility, and limitations. Special attention is given to method standardization and validation, as well as to the identification of reliable metabolic biomarkers for the diagnosis and monitoring of neurological disorders, including neurodegenerative, psychiatric, oncological, and neuroinflammatory diseases.

Molecules doi: 10.3390/molecules31111823

Authors: Zin Zin Ei Bodee Nutho Boonchoo Sritularak Pithi Chanvorachote Preedakorn Chunhacha

Background: T-cell acute lymphoblastic leukemia (T-ALL) remains a challenging malignancy with limited targeted therapies. Natural phenanthrene derivatives represent a promising source of antileukemic agents. Objective: We screened a library of natural phenanthrene-type compounds to identify cytotoxic leads in Jurkat T-ALL cells and investigated the mechanisms underlying their activity, including potential synergy with the proteasome inhibitor bortezomib (BTZ). Methods: Jurkat cells were treated with thirteen natural compounds at 10 and 20 µM for 48 h; cell viability was assessed by WST-1 cell viability assay. Dose–response curves were generated to calculate IC50 values. Apoptosis was evaluated by Hoechst 33342/PI staining and Annexin V/PI flow cytometry. Synergy with BTZ was analyzed using a fixed-ratio combination index (CI) approach and IC50 shift analysis. ER stress signaling was characterized by Western blotting, quantitative RT-PCR of UPR genes (GRP78, ATF6), and immunoprecipitation of GRP78 followed by ubiquitin immunoblotting. Results: Among the compounds screened, Cypripedin showed the most potent cytotoxicity with an IC50 of 6.52 µM. It induced a dose-dependent increase in apoptosis. Combination with BTZ yielded a CI < 0.5 and reduced BTZ IC50 from 3.43 to 1.88 ng/mL. Cypripedin activated the unfolded protein response (UPR), modulated key ER stress markers including GRP78, p-PERK, p-eIF2α, p-JNK, and ATF6, downregulated UPR gene transcripts, and promoted GRP78 ubiquitination. Molecular docking predicted strong binding of Cypripedin to the GRP78 ATPase domain (Vina score −7.630 kcal/mol), supporting its mechanism of action. Conclusion: Cypripedin induces apoptosis in Jurkat T-ALL cells, synergizes with BTZ, and modulates ER stress through GRP78 ubiquitination. These findings support its further development as a potential T-ALL therapeutic.

Molecules doi: 10.3390/molecules31111821

Authors: Jabulile H. Xulu Vuyelwa J. Tembu Sharon Moeno Bienvenu Tsakem Vuyisile S. Thibane Bwalya A. Witika Xavier Siwe Siwe Noundou

The rising incidence of viral infections demands the creation of innovative, biocompatible antiviral drugs with broad-spectrum effectiveness. This study combines the green synthesis, optimization, and characterization of silver nanoparticles (AgNPs) utilizing Dacryodes edulis (D. edulis) extract, assessing their antiviral, and antimicrobial characteristics. AgNPs were synthesized through the bio-reduction of silver nitrate with D. edulis water extract as a reducing, capping and stabilizing agent. The synthesis was refined through a Design of Experiments methodology. The characterization techniques, UV-Vis, Fourier-transform infrared, transmission electron microscopy, and dynamic light scattering, validated the successful synthesis of AgNPs with an average size of 101.56 ± 28.22 nm (TEM) and 156 ± 0.81 nm (DLS), a polydispersity index of 0.34, and a zeta potential of −22 mV. High-resolution liquid chromatography–tandem mass spectrometry analysis identified some bioactive compounds which enhance the antimicrobial and antiviral properties of the samples. Enzyme kinetics experiments revealed substantial inhibitory efficacy against the SARS-CoV-2 papain-like protease (PL-pro), with AgNPs exhibiting a lower IC50 (0.271 ± 0.051 mg/mL) than the D. edulis extract (0.337 ± 0.043 mg/mL). The AgNPs exhibited MIC of 0.063 mg/mL for E. coli, 0.125 mg/mL for S. aureus and 0.08 mg/mL for S. pyrogens. The corresponding MBC values were 0.125 mg/mL, 0.25 mg/mL and 0.31 mg/mL, respectively. The fungal strains C. glabrata and C. albicans displayed MIC of 0.63 mg/mL and 0.31 mg/mL, respectively, and MBC values of 0.63 mg/mL and 0.31 mg/mL, respectively. This study underscores the potential of D. edulis-derived AgNPs as a cost-efficient, environmentally sustainable, and highly bioactive antibacterial and antiviral nanomaterial, facilitating the advancement of nanotechnology-based therapies for viral infections.

Molecules doi: 10.3390/molecules31111820

Authors: Qibo Deng Zhihui Wang Jiajia Ji Minsi Xie Qiaozhen Tong Kunlai Sun Qinghua Peng Zhiying Yuan

Lilium lancifolium Thunb. is an important economic crop widely cultivated and traded across Asia and has significant pharmacological activity. Despite decades of research on their chemical composition, the spatial distribution patterns of characteristic secondary metabolites within the bulbs remain poorly understood. In this study, we used matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) technology to characterize and spatially visualize multiple metabolites within the bulb for the first time. Additionally, ultra-high-performance liquid chromatography-Orbitrap Exploris mass spectrometry (UHPLC-OE-MS) was used to obtain comprehensive metabolite information from the bulbs. Using spatial metabolomics, we successfully identified nine steroidal saponins, three phenolic acid glycerides, and six other metabolites. Subsequently, we analyzed the spatial distribution of steroidal saponins and phenolic acid glycerides, which are key bioactive components. The analysis revealed that most of the steroidal saponins and phenolic acid glycerides, such as deacylbrownioside and regaloside A, exhibited a similar distribution pattern, mainly being enriched in the outer regions (A2, B2) and basal regions (B1, B2) on an individual scale. Further metabolomic and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway enrichment analyses indicated that 11 substances detected in the bulbs, including diosgenin, phenylalanine, and acetyl-CoA, were jointly associated with 39 metabolic pathways, including “phenylpropanoid biosynthesis” and “terpenoid backbone biosynthesis”. Based on the above findings, we propose biosynthetic pathways and accumulation patterns of steroidal saponins and phenolic acid glycerides in bulbs. This study provides a basis for precise resource utilization of L. lancifolium bulbs and a methodology to elucidate the biosynthesis of plant metabolites.

Molecules doi: 10.3390/molecules31111819

Authors: Alejandra Romero-Padilla Luís M. G. Castro Manuela Pintado María Emilia Brassesco

This study evaluates the influence of harvesting methods and seasonal variability on the physicochemical and antioxidant properties of Tetragonisca fiebrigi honey produced in the tropical dry forest of Bolivia. Despite the growing interest in stingless bee honey, studies addressing the combined effects of seasonality and collection practices in this region remain scarce. Honey samples were collected during winter and spring using three approaches: conventional, optimized (based on good manufacturing practices), and direct racking from natural nests. Physicochemical parameters (pH 4.60–6.15; moisture 28-34%; water activity 0.69–0.75) and sugar composition (glucose 10.60–29.03 g/100 g; fructose 9.01–21.97 g/100 g; sucrose 0.70–3.23 g/100 g) showed variability primarily associated with season rather than harvesting method. Bioactive compounds exhibited a marked seasonal effect, with higher total phenolic content (up to 11.03 mg GAE/100 g), flavonoids (up to 23.08 mg QE/100 g), and antioxidant capacity (DPPH up to 1.33 mol TE/100 g; ORAC up to 25.93 mol TE/100 g) in spring samples. Multivariate analysis (PCA) revealed that honey variability is structured along bioactive and physicochemical axes, with samples obtained using the optimized method showing reduced dispersion and greater compositional consistency. These results indicate that while seasonality governs the compositional and functional properties of T. fiebrigi honey, improved harvesting practices contribute to reducing variability and enhancing product standardization. This study provides one of the first comprehensive datasets on Bolivian stingless bee honey and highlights its potential as a functional food, supporting the development of species-specific quality criteria and sustainable meliponiculture in tropical dry forest ecosystems.

Molecules doi: 10.3390/molecules31111818

Authors: Yue Gao Cheng Ma Xuan Qi Hao Yan Changbao Wang Junfeng Zhang

Lost circulation in oil-based drilling fluids (OBDFs) under high-temperature conditions remains a significant challenge in deep and ultra-deep drilling. In this study, a high-temperature-resistant composite lost circulation material (LCM) was developed based on a synergistic strategy combining rigid bridging–consolidation and flexible embedding–filling. Rigid self-consolidating particles were prepared by coating skeleton materials with modified thermosetting resin, while flexible oil-absorbing resin was synthesized via suspension polymerization. The materials exhibited excellent lipophilicity, thermal stability, and structural integrity at 150 °C, with oil absorption capacity up to 3.43 g/g. The optimized composite LCM showed superior plugging performance, achieving compressive strengths above 11 MPa in white oil and 5 MPa in base mud at 150 °C. Effective sealing of 1–3 mm pore structures was obtained with leakage volumes below 10 mL, and fractured formations could be successfully consolidated. Mechanistically, rigid particles provide structural bridging, flexible resin enables pore filling via swelling, and modified resin(thermosetting resin chemically modified to achieve self-consolidation) enhances consolidation and micro-pore sealing, resulting in a dense and high-strength plugging layer. This work provides a promising approach for designing high-performance LCMs for OBDFs in high-temperature drilling environments.

Molecules doi: 10.3390/molecules31111817

Authors: Subin Lee Yerim Kim Jeongeun Kim Kwang Suk Lim Hyun-Ouk Kim

Targeted drug delivery remains difficult because multiple biological barriers interfere with the stable transport of therapeutics to the site of action. Polymeric nanocarriers have gained broad attention as delivery platforms since their composition and surface properties can be adjusted to improve circulation behavior and cellular delivery. This review discusses the major biological barriers involved in targeted drug delivery and describes how polymeric nanocarriers are engineered to overcome them. Major carrier types, including polymeric nanoparticles and micelles, are considered with emphasis on their physicochemical and interfacial features. Particular attention is given to surface engineering and stimuli-responsive design as key strategies for barrier transport and controlled cargo release. The review also highlights representative applications in anticancer, gene, protein, and vaccine delivery, together with translational issues such as biocompatibility, stability, reproducibility, scale-up, and regulatory acceptance.

Molecules doi: 10.3390/molecules31111816

Authors: Sanyuan Qiao Luoqi Cui Li Cai Zhenzhong Fan

ASP flooding wastewater contains crude oil, suspended solids, anionic polymers and surfactants, with high viscosity, high zeta potential, difficult demulsification, flocculation and slow separation and sedimentation. In order to solve the problem of wastewater treatment of ASP flooding in oil fields, a magnetic branched core was prepared from ethyl silicate (TEOS), nano Fe3O4 and aminopropyl triethoxysilane (APTES), and then reacted with polyamine and methyl acrylate to synthesize the magnetic hyperbranched molecule FSNMN with demulsification ability. Using acrylamide (AM), acryloxyethyl trimethylammonium chloride (DAC) and maleic anhydride (MA) as raw materials, cationic polymer long chain (CAMHA) with flocculating properties was synthesized and grafted with hyperbranched molecules. The demulsification flocculation ability of the product regarding ASP flooding wastewater was evaluated, and the demulsification flocculation mechanism was summarized. The results showed that the average molecular weight of 3-FSNMN4-C was 4.7 million, the cationic degree was 20.5%, and the saturation magnetization was 20 EMU/g. The removal rate of oil and suspended solids was 93.82% and 91.95% respectively when the simulated sewage was treated by magnetic field for 30 min. Magnetic hyperbranched star chain polymer provides a solution to the serious ecological environment problems caused by ASP flooding.

Molecules doi: 10.3390/molecules31111815

Authors: Jing Huang Xinyan Yu He Zhao Fenying Kong Yong Dai

In this study, bis-1,10-phenanthroline (Biphen) was synthesized via a hydrogen transfer-mediated coupling reaction in a single step. The resulting compound was demonstrated, for the first time, to function as a selective fluorescent probe for Ni2+ ions. The presence of Ni2+ at a 2:1 molar ratio of Biphen to Ni2+ results in complete fluorescence quenching, with a detection limit of 4.34 × 10−9 M in aqueous medium. Fluorescence is restored upon the introduction of a suitable chelating agent, producing an “on-off-on” fluorescence switching response. Furthermore, fluorescence co-localization studies demonstrate that Biphen functions as a mitochondria-targeted fluorescent probe with excellent cell membrane permeability, enabling rapid, reversible imaging and ultratrace detection of Ni2+ in mitochondria of live cells. Overall, this work demonstrates highly selective ultratrace detection of Ni2+ in both aqueous and biological environments, providing a promising platform for mitochondrial imaging and potential diagnostic applications.

Molecules doi: 10.3390/molecules31111814

Authors: Anwuli E. Odieka Ayodeji O. Oriola Gugulethu M. Miya Pallab Kar Opeoluwa O. Oyedeji Mavuto M. Gondwe Yiseyon S. Hosu Thami Madliwa Adebola O. Oyedeji

Cannabis sativa L. is a medicinal plant cultivated globally due to its remarkable historical and scientific relevance. Through the consumption of its flowers, also referred to as inflorescences, which contain a high content of cannabinoids, terpenes and polyphenols, the therapeutic properties of C. sativa can be harnessed. This study therefore aimed to determine the chemical profile, antioxidant and anti-inflammatory activities of the essential oils (EOs) obtained from the fresh and dried flowers of two C. sativa cultivars, Lifter and Cherrywine, grown in Komga, South Africa, to assess which cultivar has greater biological potential. The chemical profiles of the hydro-distilled EOs were analyzed by gas chromatography–mass spectrometry (GC-MS), while the in vitro antioxidant and anti-inflammatory activity of the EOs was analyzed using the DPPH and EAD methods, respectively. The identified constituents from the EOs were molecularly docked against NOX2 and NIK (NF-κB-inducing kinase) protein, which are implicated in oxidative stress. The afforded EOs were yellow (pale and bright yellow) in color with a sweet to mildly sweet aroma description. A total of 51 constituents were identified in both fresh and dry oils from the Lifter cultivar, while the Cherrywine cultivar contained a total of 44 constituents. Eighteen compounds, were found to be the main chemical constituents consistent in the flower EOs of both cultivars, notably, caryophyllene (10.71–19.96%), levo-β-pinene (1.37–13.21%), humulene (5.88–9.77%), caryophyllene oxide (4.32–7.49%), D-limonene (1.40–5.48%), α-pinene (2.22–5.22%), nerolidol (0.63–4.97%), cis-β-ocimene (0.22–4.37%), linalool (1.12–4.28%), selina-3,7(11)-diene (0.15–4.23%), humulene-1,2-epoxide (1.23–3.32%), guaiol (0.17–2.60%), (+)-β-selinene (1.20–2.51%), trans-α-bergamotene (0.68–2.37%), β-ocimene (0.90–2.27%), fenchol exo- (0.15–1.27), terpineol (0.14–1.38%) and α-terpineol (0.19–0.75%). The fresh Lifter flower oil (LFO) showed 50% inhibition at 100 μg/mL, with an IC50 of 69.50 ± 4.05 µg/mL against DPPH, suggesting moderate to low radical scavenging activity. The maximum percentage inhibition response of DLFO, CFO and DCFO remained below 50% at all concentrations. The antioxidant activity of fresh LFO may be attributed to its overall chemical composition. The flower oils showed in vitro inhibition of protein denaturation; however, the high standard deviation relative to the mean IC50 values limited the ability to rank the samples’ potencies. Further in silico studies on the putative constituents in the Lifter and Cherrywine cultivars revealed β-bisabolene and α-curcumene as potential molecular targets, with binding energy scores of −7.7 and −7.9 kcal/mol, respectively. Thus, the study findings highlight the promising biological importance of C. sativa inflorescences in the management of oxidative stress-related conditions. Further studies may investigate the influence of environmental growing conditions on their chemical composition, total ROS analysis, pharmacokinetic properties, and in vivo efficacy against oxidative damage to DNA, proteins and lipids. Evaluating the toxicity of the flower EOs is also recommended.

Molecules doi: 10.3390/molecules31111812

Authors: Chenyu Jiang Muhammad Sajjad Kaibing Zhou

The fallen Camellia vietnamensis fruits caused by typhoons are usually collected by the farmers to be processed into oil in order to decrease the loss of the disaster. Then, this report investigates the difference in the yield, quality, and antioxidant activity of the seed oil between the fallen fruits caused by the typhoons and the normally harvested fruits. The yield of seed oil from fallen fruits caused by typhoons (HCA) was significantly lower than that of normally harvested fruits (HCB). The physicochemical properties of HCA showed signs of quality deterioration. HCA seemed to optimize the fatty acid composition. HCA exhibited stronger DPPH· radical scavenging, ABTS·+ inhibitory, and ferric ion-reducing activities. Thirty-four volatile compounds were identified in both samples. HCA showed higher levels of antioxidant-rich volatiles. Overall, this investigation demonstrates that the fallen fruits caused by typhoons lead to significant seed oil yield losses and measurable quality deterioration, thereby offering clear, evidence-based insights to support more effective typhoon disaster mitigation strategies.

Molecules doi: 10.3390/molecules31111813

Authors: Guoying Wang Ying Su Jianglei Yu Ruihong Li Shangrong Ma Xiuli Niu Gaofeng Shi

In the original publication [...]

Molecules doi: 10.3390/molecules31111809

Authors: You Luo Zhuo Li Jing Xie

Inspired by natural porphyrin-containing enzymatic active sites, metalloporphyrins have become important platforms for oxygen reduction reaction (ORR) catalysis because of their well-defined structures and tunable coordination environments. Recently, breaking the N4-coordination environment of cobalt porphyrins by inverting one pyrrolic unit to generate N3C1-site, i.e., N-confused porphyrin, has emerged as an effective strategy to promote their electro-catalyzing ORR capability. Herein, we reviewed recent progress in N-confused cobalt porphyrin in catalyzing ORR, with special emphasis on the influence of the catalyst’s architecture. We first summarized the general ORR mechanism on metalloporphyrins and the computational methods commonly used for mechanistic studies. Then, for comparison, the more common modification strategies like meso- and β-position substitution, axial coordination, and dinuclear design were reviewed for cobalt porphyrin-based catalysts. The main part reviewed the N-confused cobalt porphyrins with three different architectures, i.e., molecular, framework, and supported heterogeneous molecular form, highlighting their synthesis, characterization, electrocatalytic ORR behavior, and mechanistic interpretation from both experimental and theoretical perspectives. It summarizes the current understanding of why CoN3C1 systems outperform the original CoN4 porphyrin systems. The architecture of catalysts was found to affect the selectivity and mechanisms of ORR, along with the discussion of pH. The effects of N-confused strategy were compared to other modification strategies. Finally, we proposed possible directions for integrated catalyst design and mechanism studies.

Molecules doi: 10.3390/molecules31111811

Authors: Shenshen Li Wei Liu Jiaojiao Zheng Lingyu Ren Changhao Zhou Qiao Wu Zhilong Ai

Thyroid cancer (TC) is an endocrine malignant tumor with the fastest-growing incidence worldwide. It has complex pathological types and significant heterogeneity, with great differences in clinical prognosis among different subtypes. Among them, aggressive subtypes, such as radioiodine-refractory (RAI-R) TC and anaplastic thyroid cancer (ATC), have become a major challenge in current clinical diagnosis and treatment, due to limited treatment options and high risks of recurrence and metastasis. Tumor metabolic reprogramming is one of the characteristics of cancer, among which the Warburg effect plays a driving role. As a rate-limiting enzyme in the glycolytic pathway, pyruvate kinase M2 (PKM2), with its unique functional plasticity, has become a linchpin of glycolytic metabolism and malignant phenotypes of tumor cells. This article will systematically review the functional regulatory mechanisms of PKM2, its specific role in TC, and explore the targeted therapeutic strategies and research prospects of TC with PKM2, providing a new theoretical basis and potential plans for the clinical diagnosis and treatment.

Molecules doi: 10.3390/molecules31111810

Authors: Weifeng Liu Xiaran Miao Shiwen Tao Ji Li Jianzhong Ma Jinjun Yang Hui Li

The non-isothermal crystallization behavior of CF/PEEK composites during the cooling stage of processing significantly influences their final properties. However, the effect of PEEK melt fluidity on the crystallization kinetics and crystal morphology of CF/PEEK composites under varying cooling rates remains to be elucidated. This study employed differential scanning calorimetry (DSC) combined with crystallization kinetic models including Avrami and Mo equations to analyze the non-isothermal crystallization process, while wide-angle X-ray scattering (WAXS) characterized the crystal morphology. The results indicate that with increasing PEEK melt fluidity, the crystallinity of CF/PEEK composites rose from 22.2% to 25.93% at a cooling rate of 5 °C/min, accompanied by an enhanced crystallization rate. Mechanical testing revealed that the mechanical properties improved with increasing fluidity: the tensile and flexural strengths increased from 264.8 MPa and 413.3 MPa for CF/PEEK20 to 299.1 MPa and 476.5 MPa for CF/PEEK146, respectively. Furthermore, as the PEEK melt fluidity increased, the dominant factor governing crystallization behavior shifted from chain structural stability to molecular chain mobility, and ultimately to nucleation capability.

Molecules doi: 10.3390/molecules31111808

Authors: Ali Osman Abdel-Rahaman M. Merwad Azza H. Mohamed Mahmoud Sitohy

The journal retracts the article titled “Foliar Spray with Pepsin-and Papain-Whey Protein Hydrolysates Promotes the Productivity of Pea Plants Cultivated in Clay Loam Soil” [...]

Molecules doi: 10.3390/molecules31111807

Authors: Justus Wambua Mukavi Monica Cal Marcel Kaiser Pascal Mäser Njogu M. Kimani Leonidah Kerubo Omosa Thomas J. Schmidt

In the original publication [...]

Molecules doi: 10.3390/molecules31111806

Authors: Thanh Sang Vo Thi Ngoc My Vo Hoang Dung Nguyen Dai-Nghiep Ngo Quang Vinh Nguyen Dai-Hung Ngo

This study aimed to investigate the anti-allergic potential of the ethyl acetate fraction (EtOAc) from Phyllanthus amarus using an ovalbumin (OVA)-induced allergic mouse model and in vitro RBL-2H3 mast cell assays. The EtOAc fraction was characterized by high total phenolic and flavonoid contents, reaching 261 ± 18 mg GAE/g EtOAc fraction and 86 ± 7 mg QE/g EtOAc fraction, respectively. It was found that EtOAc fraction significantly reduced histamine release up to 43.3% and suppressed reactive oxygen species (ROS) production from FcɛRI-mediated mast cell activation at a concentration treatment of 200 µg/mL. Furthermore, EtOAc fraction decreased interleukin-4 (IL-4) and tumor necrosis factor-alpha (TNF-α) release up to 94.2 pg/mL and 195.6 pg/mL, respectively. In the OVA-induced allergic mouse model, EtOAc fraction treatment markedly lowered sneezing frequency and serum IgE and histamine levels by approximately 50% at a dose treatment of 50 mg/kg. In addition, histopathological analysis revealed that the EtOAc fraction significantly alleviated inflammatory cell infiltration, particularly eosinophils, in lung tissue. Accordingly, the results highlight the potential of EtOAc fraction from P. amarus as a natural candidate for managing allergic diseases.

Molecules doi: 10.3390/molecules31111805

Authors: Jesús M. Martín-Marroquín Dolores Hidalgo

Ammonia is a key chemical for fertilizers, industrial processes, and emerging energy applications, yet its conventional production via the Haber–Bosch process is associated with high energy demand and significant greenhouse gas emissions. In this context, electrochemical routes for ammonia synthesis have attracted increasing attention as a potential sustainable alternative, enabling nitrogen conversion under milder conditions and using renewable electricity. This review examines recent advances in electrochemical ammonia production, focusing on nitrogen reduction mechanisms, catalyst development, and electrochemical system design. The main reaction pathways for nitrogen activation are analyzed, together with the role of electrocatalysts in determining activity and selectivity. Progress in catalyst engineering, electrolyte optimization, and reactor configuration is discussed, with particular emphasis on strategies to mitigate competing reactions such as hydrogen evolution. In addition, alternative approaches based on nitrate reduction are considered due to their promising performance and potential integration with wastewater treatment. Unlike many recent reviews primarily focused on catalyst development or individual reaction pathways, this review provides an integrated perspective encompassing nitrogen reduction, nitrate reduction, electrolyte engineering, reactor architectures, and techno-economic considerations, thereby highlighting the interdependence between materials design, reaction environment, and system-level integration for scalable electrochemical ammonia synthesis.

Molecules doi: 10.3390/molecules31111804

Authors: Carmela Protano Arianna Antonucci Maria Luisa Astolfi

The determination of soluble elemental contaminants in tattoo inks is challenged by the lack of standardized extraction procedures, limiting the comparability of analytical results and the assessment of exposure-relevant fractions under the European REACH framework. In this study, artificial sweat extraction was applied as a mild and physiologically relevant approach to evaluate elements potentially released from tattoo inks under sweat-simulated skin-contact conditions. Seventy-eight commercial tattoo inks of different colors were extracted with artificial sweat at 37 °C for 1 h and analyzed by inductively coupled plasma mass spectrometry. Optimization of collision/reaction cell conditions, dilution strategy, and internal standard correction effectively reduced matrix-related interferences caused by the high salt and chloride content of artificial sweat, ensuring reliable quantification. Matrix-matched calibration was required due to significant signal suppression for several analytes. Method accuracy and precision, assessed using NIST 1643f and spiked samples, were generally satisfactory. Elemental release showed marked color-dependent trends, particularly for Cu, Zn, Ba, Al, Ga, Si, Sr, and Zr, reflecting differences in pigment composition and formulation. Soluble Ba, Cu, and Zn remained below EU regulatory limits. While total digestion remains essential for complete characterization, the proposed methodology provides a simple and transferable tool for exposure-oriented assessment of potentially bioaccessible elements in tattoo inks.

Molecules doi: 10.3390/molecules31111802

Authors: Aleksandra Wilczyńska Aleksandra Wójcicka Andrzej Taube Mateusz Łakomski Tomasz N. Kołtunowicz

This paper presents the results of the preparation and electrical characterization of Ru–Si–O thin-film nanocomposites deposited by magnetron sputtering (pDC) with varying oxygen content ranging from 0% to 50%. Measurements were conducted over a wide frequency range of 50 Hz–5 MHz and temperatures of 20–373 K. Conductivity analysis revealed that DC conduction occurs at low frequencies (≤103 Hz), while an increase in conductivity associated with electron tunneling mechanisms is observed at higher frequencies. The determined charge transport activation energies range from 3 × 10−4 eV for the oxygen-free sample to 6 × 10−2 eV for the high-oxygen samples, indicating a significant effect of composition on the conduction mechanisms. In samples containing 30% and 50% oxygen, two characteristic frequency ranges for the activation of transport processes were observed (e.g., ~102–103 Hz and 104–106 Hz), suggesting the coexistence of multiple tunneling mechanisms. Phase angle analysis revealed a transition from values near –90° at 151 K to values near 0° at 333 K, characteristic of parallel RC systems. The minimum dielectric loss tangent occurs in the range of 103–105 Hz, corresponding to Maxwell–Wagner relaxation. The dispersion coefficient α reaches maximums in two frequency ranges, decreasing with increasing oxygen content. EDS analysis showed a decrease in Ru content from ~24.9 at.% (0% O2) to ~0.7 at.% (50% O2) and an increase in oxygen content to ~78 at.% at 10% O2. The results confirm the transition from metallic conduction to tunneling and hopping mechanisms with increasing oxidation state of the structure.

Molecules doi: 10.3390/molecules31111803

Authors: Antonella Angelini Carlo Pastore

The catalytic isomerization of glucose to fructose is a pivotal step in the valorisation of lignocellulosic biomass. In this study, polyaluminium chloride (PAC), a low-cost, industrially available material characterised by polynuclear aluminium–oxo species, is investigated for the first time as an alternative catalyst for this transformation. The catalytic performance of PAC was systematically investigated by varying the temperature (70–130 °C), solvent (pure water, H2O:MeOH 1:1 or 4:1) and reaction time (30–120 min). A fructose yield of up to 55% with a selectivity of 85% was obtained by using PAC at 120 °C in H2O:MeOH 1:1 for 120 min, confirming its effectiveness in promoting glucose isomerization to fructose. Mechanistic insights and quantitative monitoring were achieved using benchtop NMR spectroscopy. 27Al-NMR of PAC in aqueous solution exhibits two main signals at 1.12 ppm (attributed to the hexacoordinated Al complex) and at 63.3 ppm (associated with a tetrahedral Al centre typical of the Al13 Keggin-type cluster). With the increase in temperature, as well as by changing the reaction media from pure aqueous to a mixed aquo-alcoholic system, new Al species were generated that are more reactive than the starting AlCl3∙6H2O and PAC. Overall, this work demonstrates that PAC represents a viable, scalable, and more sustainable alternative to conventional aluminium-based catalysts, offering a promising route toward more efficient biomass conversion processes.

Molecules doi: 10.3390/molecules31111801

Authors: Natalina Makieieva Michał Jewgiński Artur Małolepszy Teobald Kupka

Cathinone and its synthetic derivatives are among the most popular drugs worldwide. However, the literature provides data on the medicinal and cytotoxic potential of some of these compounds. These data are extremely limited due to the need to obtain additional permits for laboratory studies. Consequently, the therapeutic potential of cathinones may not have been fully explored. Furthermore, the literature provides data on the reduction or reversal of undesirable biological properties of drugs encapsulated in a bio-compatible carrier and administered through targeted therapy. The current study presents preliminary theoretical and experimental tests for further research on target cathinone–graphene–oxide complexes. A non-psychotropic cathinone model—o-fluorophenylacetic acid—was used. The NMR properties (chemical shifts, spin–spin coupling constants, and T1 relaxation times) of graphene oxide–F-derivative complexes were measured at an acidic and neutral pH. To analyze the structure and stability of the possible complexes in different environments, molecular modelling was performed with simplified graphene oxide models using density functional theory. Experimental data were compared with theoretical values, and the most stable structures that may account for the observed spectral properties of the studied complexes were presented. The obtained data indicate a stronger tendency towards the formation and stabilization of GO-2-fluorophenylacetic acid complexes in a neutral environment.

Molecules doi: 10.3390/molecules31111800

Authors: Marian Czauderna Małgorzata Białek Wiktoria Wojtak Agnieszka Białek Valeriia Fesenko

Background: An original pre-column derivatisation strategy combining liquid chromatography, supported by gas chromatography, was developed for the determination of malondialdehyde (MDA), formaldehyde (FA), and 4-hydroxynonenal (4-HNE) in selected plant oils and model edible animal tissues (i.e., muscle, adipose tissue, liver, and brain). Methods: In oils, direct derivatisation with 2,4-dinitrophenylhydrazine (DNPH) was applied to quantify the target aldehydes (as hydrazones) without prior saponification. In the analysed animal tissue samples, MDA and FA were released by saponification and subsequently derivatised with DNPH, whereas 4-HNE was extracted from these samples and subsequently derivatised with DNPH. Derivatised aldehydes were quantified using C18 ultra-high performance liquid chromatography (C18-UHPLC) with photodiode array detection (DAD) under binary-gradient elution conditions, supported by gas chromatography (GC) with flame ionisation detection (FID). Results: The combination of the original binary gradient elution programme, selective DAD, and a high-performance C18 column (150 mm, 1.6 µm particle size) resulted in excellent baseline stability, good linearity, and satisfactory repeatability and specificity in the determination of MDA, FA, and 4-HNE. C18-UHPLC–DAD enabled satisfactory separation of MDA, FA and 4-HNE hydrazones from endogenous matrix components in solutions of processed oils and animal tissues, while the addition of acetonitrile to these sample solutions further reduced background interference. C18-UPLC-DAD provided satisfactory symmetrical peak shapes, peak purities, and recoveries of MDA, FA, and 4-HNE in analysed plant oils and ovine tissues, compared with GC–FID. Compared with GC–FID, C18-UHPLC-DAD provided superior resolution of derivatised aldehydes in matrices of analysed biological samples. Conclusions: The determination of lipid peroxidation biomarkers in oils and animal tissues using our novel C18-UHPLC-DAD method may contribute to the optimisation of breeding practices, helping to minimise animal stress and enhance the health-promoting properties of food products.

Molecules doi: 10.3390/molecules31111799

Authors: Zeyuan Li Zhenzhen Liu Xiangping Lin Mengyuan Ge Nannan Wu Xinquan Wang Yuteng Zhou Shuchun Wu Wei Ding Peipei Qi

The excessive use of herbicides in agricultural fields has emerged as a critical environmental concern. This study innovatively synthesized a ZIF-8@TPPa composite through a solvothermal method for the efficient removal of herbicides from aqueous environment. The material exhibited remarkable adsorption capacities for butachlor (232.56 mg/g), anilofos (188.68 mg/g), and pendimethalin (285.71 mg/g), along with excellent acid–base stability (pH 3–9), strong anti-ion interference capability, and good reusability (adsorption efficiency >80% after five cycles). The adsorption processes were well-described by the two isotherm models and the pseudo-second-order model, indicating that the dominant mechanism is a synergistic effect between monolayer chemical adsorption and multilayer physical adsorption, primarily driven by π-π stacking, hydrogen bonding, and coordination. The material maintained outstanding adsorption efficiency (>85%) in real water samples (tap water, seawater, and river water). This study not only provides a sustainable and effective strategy for herbicide remediation from aqueous environment but also expands the practical applications of MOF@COF in aqueous environment.

Molecules doi: 10.3390/molecules31111793

Authors: Xinchuan Huang David W. Schwenke

High-accuracy potential energy surface (PES) and rovibrational energy levels are essential for computational IR line lists used in (exo)planetary atmospheric spectroscopic analysis and modeling. We present a new 14N216O PES refinement achieving 0.001–0.002 cm−1 statistical accuracy for Evib ≤ 7000 cm−1 and Jmax = 88–100, relative to complete experiment-based rovibrational energy levels in RITZ, MARVEL, HITRAN2020, and NOSL-296 datasets. Building upon the high-quality ab initio Comp-I PES, the resulting D2n (and D2nB) PES outperform the Ames B1b PES, the UCL TYM PES, and the UCL 2025 PES series in both energy-resolved and J-resolved comparisons, exhibiting the smallest mean residuals and scatter below Evib = 8000 cm−1, as well as the highest fractions of |δ| < 0.0010 cm−1 and |δ| < 0.0005 cm−1. Robust analysis identified only seven outliers among the UCL-2025 reference level set; all remaining levels are retained to ensure resilient statistics. The D2n PES also shows stable IR intensities with the G10K dipole moment surface and reasonably consistent isotopologue accuracy. Analysis of J-resolved σrms highlights the critical role of reference-dataset accuracy and internal consistency. We discuss factors enabling (sub-)0.002 cm−1 accuracy and prospects for extending similar accuracy to higher energies, additional isotopologues, and other molecules.

Molecules doi: 10.3390/molecules31111798

Authors: Zaixiang Lou Xinyan Cui Beiqi Wu Hongxin Wang Nattaya Konsue Sook Wah Chan Bing Kang

Developing a Pueraria lobata compound beverage is of great significance for enhancing the utilization value of Pueraria lobata resources. However, its flavor balance, physical stability, and quality changes during storage require further investigation. This study aimed to develop a high-quality Pueraria lobata compound beverage and establish a reliable shelf-life prediction model. The optimal formulation was determined using orthogonal design and multi-index evaluation, including extract stock solution, mogroside, citric acid, and a composite stabilizer consisting of xanthan gum (XG) and sodium carboxymethyl cellulose (CMC-Na). GC-MS analysis identified multiple volatile compounds collectively forming the characteristic flavor profile. During storage, physicochemical properties, sensory quality, and active component contents changed to varying extents, with deterioration significantly accelerated at higher temperatures. Among the quality indicators, Zeta potential was selected as the most suitable predictor because it showed a strong correlation with sensory scores and fitted the first-order kinetic model well. Based on the established Arrhenius-based prediction model, the predicted shelf-lives of the Pueraria lobata compound beverage at 4 °C, 27 °C, and 37 °C were 193, 104, and 82 days, respectively. These findings provide a solid theoretical basis for formulation design, stability improvement, and shelf-life evaluation of functional Pueraria lobata beverages.

Molecules doi: 10.3390/molecules31111797

Authors: Larisa Adela Udriştioiu Marius Enăchescu Alexia Ecaterina Cârstea George Cristian Curcă Mihaela-Monica Popa Mihai Andrei

Teeth may retain forensic value after chemical exposure, yet the effects of commercially available corrosive agents remain insufficiently characterized. This study evaluated short-term alteration patterns in human teeth exposed to household acidic and alkaline products available on the Romanian market. Five extracted mandibular third molars were analyzed, including four experimental teeth and one control. Each experimental tooth was fully immersed for 48 h in a different agent: hydrochloric acid descaler, sodium hypochlorite bleach, mixed hydrochloric/sulfuric acid descaler, or sodium hydroxide. Morphometric changes, mass, and pH were monitored serially, while stereomicroscopy, SEM-EDX, and hard tissue ground sections were used for structural and compositional assessment. Acid-exposed teeth showed the greatest damage, with major mass loss in the hydrochloric acid and mixed-acid samples, enamel loss, and marked microstructural disruption. The mixed-acid specimen exhibited the most severe collapse and near-complete calcium/phosphorus depletion. Sodium hypochlorite produced mainly superficial and root-level alterations with relative preservation of gross morphology, whereas sodium hydroxide caused minimal dimensional change and a calcium-rich adherent surface deposit. These findings show that household corrosives produce distinct, forensically recognizable dental alteration patterns within 48 h and support an integrated pattern-recognition approach in suspected chemical concealment scenarios.

Molecules doi: 10.3390/molecules31111794

Authors: Ying Guo Xi Qin Jing Zhang Hua Bi Shuting Hou Youxue Ding Dening Pei Xiang Li Yue Pan Xiaoliang Sun Chenggang Liang

Currently, the most commonly used methods for detecting Mycoplasma are the culture method and the indicator cell culture method. However, both approaches exhibit low sensitivity and are incapable of detecting low-concentration contamination. In addition, the detection period may extend up to 28 days, which is unsuitable for rapid screening and may delay timely contamination control measures. To address these limitations, a Mycoplasma detection method based on nucleic acid amplification technology (NAT) was developed following a comparative analysis of gene sequences from various Mycoplasma species. The method was validated with respect to its detection performance and its applicability to biological product samples. DNA was extracted from Mycoplasma-contaminated samples using a magnetic bead-based nucleic acid extraction method. Universal primers were designed based on the highly conserved 16S rRNA gene sequence of Mycoplasma, and amplification was performed using multiplex quantitative PCR (qPCR) with fluorescent probes. The limit of detection (LOD) was established based on statistics of 24 replicates. Method specificity and robustness were evaluated according to the guidelines set by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH Q2), while sample applicability was assessed in accordance with the European Pharmacopoeia (EP) <2.6.7>. The NAT-based Mycoplasma detection method enabled rapid, qualitative identification of Mycoplasma contamination. The validated LOD was 10 CFU/mL, and the method met predefined requirements for sensitivity, specificity, and robustness. To assess applicability, real biological product samples, including monoclonal antibodies, antibody fusion proteins, bispecific antibodies, and trispecific antibodies, were spiked with 10 CFU/mL of standard Mycoplasma strains. All spiked samples tested positive. These findings confirm that the NAT-based Mycoplasma detection method is suitable for process control and product release testing in the production of biological products.

Molecules doi: 10.3390/molecules31111796

Authors: Federica Carnemolla Sandeep Kumar Singh Leonardo Ceccherini Niccolò Taddei Monica Bucciantini Manuela Leri

Chemotherapy-induced cognitive impairment (CICI), often referred to as “chemobrain,” is a common and sometimes persistent consequence of cancer treatment, characterized by deficits in memory, attention, executive function, and processing speed; it disproportionately affects older adults and women, suggesting a role for aging- and sex-related biological factors, including estrogen depletion. This work examines the potential of dietary phenolic compounds as multi-target modulators of mechanisms underlying CICI. A narrative synthesis of preclinical and clinical evidence was conducted, focusing on major phenolic subclasses (flavonoids, phenolic acids, stilbenes, lignans, and secoiridoids) and their effects on pathways implicated in chemotherapy-related neurotoxicity. The reviewed data indicate that phenolic compounds can influence redox balance, neuroinflammatory responses, mitochondrial function, synaptic plasticity, and estrogen-related signaling, with effects that appear to be structure-dependent; however, evidence remains heterogeneous and largely derived from experimental models rather than studies in humans. Overall, the current findings suggest that selected phenolic compounds could mitigate vulnerability to CICI, particularly in higher risk groups such as older individuals and women with low estrogen levels. These compounds represent promising and safe adjunctive strategies, although further well-designed clinical studies are needed to confirm their efficacy and clarify the underlying mechanisms.

Molecules doi: 10.3390/molecules31111795

Authors: Meruyert D. Dauletova Almagul K. Umbetova Aisulu Zh. Kabdraisova Rizvangul S. Iminova Gauhar Sh. Burasheva Yuliya A. Litvinenko Nazym S. Yelibayeva Natalya V. Kurbatova Dmitriy Yu. Korul’kin Nailya A. Ibragimova Gulnar O. Bugubaeva Murat R. Zhumabayev

Atraphaxis virgata and Atraphaxis pyrifolia are xerophytic species of the Polygonaceae family that remain insufficiently characterized from pharmacognostic, phytochemical, and toxicological perspectives. This study provides an integrated evaluation of both species through anatomical authentication, sequential extraction of CO2-extracted residual biomass, GC–MS and LC–MS metabolite profiling, and acute oral toxicity assessment. Anatomical analysis revealed shared xeromorphic traits, including cuticular protection, dorsiventral mesophyll organization, structured vascular bundles, and calcium oxalate druses. It also identified species-specific differences in leaf thickness, mesophyll arrangement, vascular architecture, and druse morphology. GC–MS analysis showed distinct chemical profiles: A. virgata displayed a concentrated profile dominated by acetophenone- and benzofuran-related constituents, whereas A. pyrifolia showed a broader spectrum of carbohydrate-derived, phenolic-related, and oxygenated constituents. LC–MS analysis supported the tentative annotation of diverse polyphenolic classes, including flavonoids, phenolic acids, coumarins, and phenylpropanoid derivatives. Acute oral toxicity testing showed no mortality at doses up to 2000 mg/kg, supporting a low acute oral toxicity classification under the tested conditions. However, histological examination revealed mild to moderate dose-dependent alterations in liver and kidney tissues at higher doses. The novelty of this work lies in linking diagnostic anatomical traits, species-specific metabolite patterns, residual biomass valorization, and preliminary safety evidence within a single comparative framework. These findings provide a basis for pharmacognostic authentication, phytochemical standardization, and future bioactivity-guided evaluation of Atraphaxis species.

Molecules doi: 10.3390/molecules31111792

Authors: Jailane de Souza Aquino Alana Natalícia Vasconcelos de Araújo Januse Míllia Dantas de Araújo Luana Clementino Santos Jordania Candice Costa Silva Kamila Sabino Batista Lucas Rannier Ribeiro Antonino Carvalho

Acerola (Malpighia emarginata DC.) is one of the richest natural sources of vitamin C and an important source of phenolic compounds, carotenoids, and bioactive polysaccharides. Although the fruit can be consumed fresh, it is more commonly processed into juices and frozen pulp, generating substantial amounts of by-products (pomace, peels, and seeds), corresponding to approximately 20–60% of the fruit biomass, with high phytochemical content. These fractions represent underutilized sources of bioactive compounds. This narrative review, supported by a structured literature search, integrates evidence on the phytochemical composition of acerola pulp and its by-products and relates these profiles to biological effects in experimental and human studies, focusing on compound characterization, composition–function relationships, and underlying mechanisms. Key compounds, including ascorbic acid, hydroxycinnamic acids, flavonoids, and polysaccharides, are associated with the modulation of redox homeostasis, inflammatory signaling, and lipid metabolism, particularly under high-fat dietary conditions. Human evidence remains limited but suggests matrix-dependent effects on vitamin C bioavailability and selected cardiometabolic markers. Overall, the evidence is constrained by methodological heterogeneity, limited clinical data, and insufficient characterization of bioactive fractions. Future research should prioritize detailed phytochemical profiling, dose–response relationships, bioavailability assessment, and well-controlled clinical trials incorporating molecular biomarkers, supporting the development of acerola-derived matrices as functional and bioactive-rich ingredients.

Molecules doi: 10.3390/molecules31111791

Authors: Kételin Vitória Matias Mario Augusto Izidoro Fernando Barbosa Bruno Alves Rocha Victor Silva da Fonsêca Fulvio Alexandre Scorza Frederick Wasinski Valeria de Cassia Gonçalves Rozana Mesquita Ciconelli Andresa Aparecida Berretta Josef Finsterer Carla Alessandra Scorza

Parkinson’s disease (PD) is characterized by progressive nigrostriatal degeneration and striatal dysfunction, yet its metabolic remodeling remains incompletely defined. Here, untargeted GC–MS metabolomics was used to investigate the effects of standardized Brazilian green propolis on the striatal metabolic profile in the 6-hydroxydopamine (6-OHDA) rat model. Discriminant metabolites, including suberic acid, gluconic acid, heptadecane, and tartaric acid, distinguished experimental groups, capturing key features of the metabolic response to dopaminergic injury and treatment. Suberic acid emerged as a prominently modulated metabolite, potentially linked to alterations in lipid catabolism associated with mitochondrial–peroxisomal pathways. Propolis treatment attenuated the elevation of suberic acid, accompanied by a reduction in gluconic acid levels, suggesting a metabolic profile linked to pathways involved in redox balance and glucose handling. Given previous reports identifying heptadecane as a hydrocarbon constituent of volatile propolis fractions, complementary GC-Q-TOF analyses demonstrated that heptadecane was absent from the administered extract, despite its consistent association with propolis-treated groups. Metabolic changes were accompanied by attenuation of nigrostriatal dopaminergic neurodegeneration and improved motor performance. Together, these findings delineate a striatal metabolic signature associated with Brazilian green propolis and identify suberic acid as a key metabolite linked to neuroprotection in experimental Parkinsonism.

Molecules doi: 10.3390/molecules31111790

Authors: Qin-Feng Qu Qing-Ping Zhang Yi Yu

Lactobacillus species are widely used in various food products, including conventional food products, dairy products, and health food products. To achieve the desired functional properties, manufacturers commonly incorporate two or more distinct Lactobacillus species during production. In this study, a multiplex PCR detection method was developed for four Lactobacillus species commonly used in food based on TaqMan real-time fluorescent PCR technology, enabling the efficient and rapid identification of multiple Lactobacillus strains in food matrices. The research team selected and validated four representative species—Lactobacillus rhamnosus, Lactobacillus plantarum, Lactobacillus acidophilus, and Lactobacillus paracasei—as targets for the multiplex PCR assay, designing specific primer–probe combinations for each. The accuracy and reliability of the detection method were rigorously evaluated through a series of validation experiments, including the assessment of primer–probe specificity, optimization of fluorescent signal labeling chemistries, determination of the limits of detection for individual strains, evaluation of the method’s repeatability, and analysis of commercial food samples. The results demonstrated that the selected primer–probe sets exhibited no cross-reactivity in the multiplex system and specifically amplified their target Lactobacillus species, with no amplification observed for non-target strains. The established method achieved a minimum LOD for L. acidophilus of 102 CFU/g and showed high repeatability across replicates. Furthermore, the successful detection of labeled Lactobacillus strains in commercial products confirmed the method’s practical applicability. Therefore, the developed multiplex real-time PCR assay provides a reliable, sensitive, and high-throughput tool for the simultaneous detection of multiple Lactobacillus species in complex food products and holds potential for application in quality control, product authentication, and regulatory compliance monitoring.

Molecules doi: 10.3390/molecules31111789

Authors: Anna Ignaczak Łukasz Woźniak Mariola Kozłowska Hanna Kowalska

The aim of the study was to investigate the effect of enriching carrot slices by NFC (not from concentrate) juices from chokeberry (CH), sea buckthorn (SB), cherry (CHE) and carrot (CA) before microwave-vacuum (MVD) and freeze-drying (FD) carrot on the physicochemical and thermal properties. While water activity (AW) was not dependent on enrichment treatment but only on drying method, NFC juices significantly enriched carrot slices with biocomponents. Freeze-dried samples, as a reference, had significantly lower AW than those dried by the MVD method. Both FD and MVD-dried samples had comparable polyphenol content and DPPH antioxidant activity (AA), but the MVD-dried samples exhibited higher ABTS antioxidant activity. Carrot enrichment in chokeberry and cherry juices resulted in up to six and 10 times higher TPC than in the raw material. In addition, samples enriched in these juices and dried with FD proved to be the most stable in terms of water state and glass transition temperature (61.4 and 69.6 °C) and water activity (approx. 0.10). In FTIR analysis, all samples exhibited similar spectral shapes, indicating similar chemical composition and functional group composition. Only in the spectral region below 900 cm−1 were unique molecular vibrations induced by various organic compounds present. Enriching carrot in juices and MVD can lead to increased hardness (Fmax and breaking work), although this is associated with increased crispness, resulting from the microstructure with a large number of small pores, especially in MVD samples enriched with cherry, chokeberry, and carrot juices, with scores of 8.0–8.4 In this respect, the average crispness rating of the MVD samples (7.2) exceeded that of the FD samples (6.8). If there is a requirement for crunchiness in the future production of dried vegetables as snacks, changes in hardness should be prioritized, along with color and biocomponent content.

Molecules doi: 10.3390/molecules31111787

Authors: Xue-Ping Kong Xue-Qing Zhong Hong-Ling Yan Zhuo-Zheng Xu Jia-Xu Qin Jing Yang Qing-Li He Qun-Fei Zhao

Fraxinus chinensis Roxb. (Qinpi), a traditional Chinese medicinal plant, accumulates abundant coumarins that contribute to its anti-inflammatory and other bioactivities. However, the enzymatic basis for coumarin structural diversification in this species remains largely unexplored. Here, through transcriptome-wide identification of the 2-oxoglutarate-dependent dioxygenase (2OGD) family in F. chinensis, followed by phylogenetic analysis, heterologous expression, and in vitro enzyme assays, we identified FcDOH2, a member of the DOXC31 subfamily, which exhibits substrate-dependent bifunctionality, catalyzing the C6-O-demethylation of scopoletin (3) to esculetin (2) and the C8-hydroxylation of umbelliferone (1) to daphnetin (6). Using AlphaFold3-based structural modeling, molecular docking, and alanine scanning mutagenesis, we revealed that residues R155 and R221 are essential for both activities through stabilizing hydrogen bonds, whereas residue F312 acts as a functional switch, being critical for demethylation but negatively regulating hydroxylation. These findings uncover a rare bifunctional 2OGD with substrate-dependent catalytic plasticity, providing mechanistic insights into coumarin diversification in medicinal plants and a structural basis for future enzyme engineering.

Molecules doi: 10.3390/molecules31111788

Authors: Flor Ximena Cadena-Aponte Sofiane El Barkaoui Patricia Plaza-Bolaños Ana Agüera Rossella Annelio Cristina De Ceglie Subhoshmita Mondal Giuseppe Bagnuolo Giuseppe Mascolo Claudio Di Iaconi

The performance of a sequencing batch biofilter granular reactor (SBBGR), followed by a dual media granular activated carbon (GAC) column, was evaluated in terms of its ability to remove selected per- and polyfluoroalkyl substances (PFAS) from landfill leachate. The results show that the SBBGR achieved an overall reduction of 51%, with the preferential removal of long-chain PFAS, while short-chain PFAS were only partially removed. Subsequent GAC treatment exhibited compound-specific breakthrough behavior, which was governed by chain length. Short-chain PFAS (e.g., perfluorobutanoic acid) exhibited rapid bed volumes at 50% breakthrough (BV50 ≈ 88), whereas long-chain PFAS (e.g., perfluorooctanoic acid and perfluorooctanesulfonic acid) were substantially more retained (BV50 ≈ 446 and 361, respectively), with perfluorohexanesulfonic acid and perfluorodecanoic acid failing to reach BV50 within the monitored period. Mass balance analysis showed that the hybrid GAC column captured ~73% of the influent PFAS mass. This resulted in >80–95% retention of long-chain PFAS and <40% retention of short-chain PFAS. Although long-chain PFAS were preferentially adsorbed, mobile short-chain species dominated residual effluent loads. These findings highlight the need for optimized contact times or dual-media strategies to control the breakthrough of short-chain PFAS.

Molecules doi: 10.3390/molecules31111786

Authors: Pimchanok Satapoomin Thiplada Juntranon Siriporn Sripinyowanich

Phyllanthus emblica L. is a nutraceutically important medicinal plant; however, the relationship between genetic variation and bioactive potential remains poorly understood. This study integrates genome-wide SNP analysis, phytochemical profiling, and functional bioassays to investigate cross-scale differentiation among fourteen cultivars. Genotyping-by-sequencing (GBS) identified 5644 high-quality SNPs from an initial dataset of 9018 SNPs, revealing moderate but structured genomic divergence (0.0275–0.0845). Phytochemical analysis of five commercial cultivars demonstrated significant variation (p < 0.05) in total phenolic content (6.58–15.53 mg GAE/gDW) and tannin content (284.52–333.81 mg TAE/gDW). Functional assays revealed strong anti-obesity potential, with crude extracts exhibiting superior α-glucosidase inhibition (up to 98.75%), while tannin-enriched extracts showed enhanced pancreatic lipase inhibition (up to 46.26%). Importantly, enzyme inhibition did not correlate directly with total phenolic or tannin content, indicating compound-specific bioactivity. LC-MS/QTOF analysis identified flavonoids (e.g., quercetin and kaempferol), phenolic acids, and other candidate metabolites potentially associated with enzyme inhibitory activity. These findings demonstrate a non-proportional association among genomic variation, metabolite composition, and functional bioactivity, suggesting that bioactivity may be influenced more strongly by compound-specific metabolite composition than by genome-wide similarity alone.

Molecules doi: 10.3390/molecules31111785

Authors: Akif Emre Kavak Enes Dertli

In recent times, the importance given to versatile functional nutrition has increased, escalating interest in fermented foods and their potential health benefits. Fermentation is an ancient method frequently used to develop functional and bioactive products. Fermented microalgae and their biomass are important sustainable biotechnological resources for increasing the nutritional value, healthiness, and functionality of foods and for producing high-value-added bioactive compounds. The fermentation of microalgae encompasses the conversion of carbohydrates into sugar or organic substances by a range of microorganisms, particularly lactic acid bacteria (LAB). The fermentation process can activate numerous beneficial mechanisms by enhancing the bioavailability of bioactive compounds in microalgae. Lactic acid bacteria are widely used in food fermentation due to their safety and metabolic versatility. Their ability to produce organic acids, enzymes, and bioactive metabolites makes them suitable for modifying microalgal biomass. This review aims to provide a detailed and critical evaluation of fermented microalgae, including health effects, functional enhancements, bioactivities, and industrial applications.

Molecules doi: 10.3390/molecules31111784

Authors: Svetlana G. Roman Salavat R. Nabiev Anastasia M. Kochurova Galina V. Kopylova Julia Y. Antonets Sergey Y. Kleymenov Valeriya V. Mikhaylova Daniil V. Shchepkin Alexander M. Matyushenko Victoria V. Nefedova

Tropomyosins (Tpm) are the family of actin-binding proteins encoded by four genes in humans. Missense mutations in the TPM1 gene associated with cardiomyopathies have been studied in the sarcomeric isoform Tpm1.1. The cardiomyopathy-causing mutations E40K and E54K are located in exon 2b of the TPM1 gene and may be expressed in non-muscle cytoplasmic Tpm isoforms, including Tpm1.7, which is associated with early tissue development. In the present work, we investigate the effects of mutations E40K and E54K on the properties of Tpm1.7. The E40K and E54K mutations caused destabilization of the Tpm1.7 molecule at the N- and C-termini parts. Neither mutation affected the Tpm1.7 affinity for filamentous actin (F-actin). The bending stiffness of F-actin/Tpm1.7 E40K filaments was lower compared to F-actin/Tpm1.7 WT (wild-type). The interplay of Tpm1.7 and motor proteins was studied in an in vitro motility assay with skeletal myosin. Tpm1.7 WT reduced the sliding velocity of F-actin by half; the velocity of F-actin with Tpm1.7 E54K did not differ from that of bare F-actin; and Tpm1.7 E40K decreased the F-actin velocity by approximately threefold. While Tpm1.7 E40K did not affect the protective effect of Tpm1.7 against F-actin severing by cofilin-1, the E54K mutation enhanced protection against cofilin-1. Thus, cardiomyopathic mutations in the TPM1 gene can affect the properties of non-muscle Tpm isoforms, which indicates that this should be taken into account when studying the molecular mechanisms of the pathogenesis of these diseases.

Molecules doi: 10.3390/molecules31111783

Authors: Fatih Göger Mehmet Tekin Gülmira Özek Süleyman Yur Mevlüt Akdağ Temel Özek

Verbascum species have long been recognized for their medicinal properties; however, detailed studies on the endemic species Verbascum wiedemannianum Fisch. & C.A. Mey. remain limited. The purpose of this study is to evaluate the antioxidant and anti-tyrosinase activities of essential oil (EO) and methanol extract (ME) derived from V. wiedemannianum, an endemic species from Türkiye. The EO was obtained by hydrodistillation, and its chemical composition was characterized using GC-FID and GC/MS. The principal constituents of the EO were palmitic acid (27.3%), myristic acid (11.9%), 1-octadecanol (13.0%), and pentacosane (6.6%). LC-MS/MS analysis of the ME identified luteolin and chrysoeriol derivatives as the predominant compounds. The antioxidant potential of both the EO and ME was evaluated using three assay systems based on electron transfer reactions: the Folin–Ciocalteu reagent, the Trolox equivalent antioxidant capacity assay, and the cupric ion (Cu2+) reducing antioxidant capacity assay. The potential skin care effects of the EO and ME were further evaluated using a tyrosinase inhibition assay. Across all the assays, the ME consistently showed notable activities, whereas the activity of the EO was less clearly defined. These findings indicate that the ME of V. wiedemannianum contains bioactive compounds with potential applications in natural antioxidant and skin care formulations. Further studies are warranted to clarify its therapeutic uses.

Molecules doi: 10.3390/molecules31111781

Authors: Kai He Hu Li Han Sun Ning Li Tong Wang Jian-Dong Jiang Zong-Gen Peng

The bark of Myrica rubra (Lour.) Siebold & Zucc (M. rubra) is a natural remedy widely used in China and other Asian countries to treat tissue and bone injuries, burns, scalds, gastrointestinal ulcers, and diarrhea. Myricanol is an important ingredient in the bark of M. rubra. This review summarizes articles published over the past 26 years on the pharmacological effects and mechanisms of action of myricanol, aiming to advance research and applications of myricanol. Evidence shows that myricanol has multiple bioactive properties, including antioxidant, anticancer, anti-inflammatory, antimicrobial, antidiabetic, and antihyperlipidemic effects. Myricanol improves metabolic abnormalities in mice by activating the AMPK/SIRT1/PGC-1α signaling pathway. It also demonstrates significant anticancer, antioxidant, and anti-inflammatory actions, primarily by regulating Caspase and BCL-2 family proteins, inhibiting iNOS expression, scavenging free radicals, and interacting with Peroxiredoxin 5. Therefore, myricanol shows great potential for the treatment of cancer, metabolic abnormalities, and inflammatory bowel disease. Further research is needed to improve its bioavailability, confirm its pharmacological effects and mechanisms in vivo, and explore its pharmacokinetic properties and safety.

Molecules doi: 10.3390/molecules31111782

Authors: Anastasiya Shesterkina Valeriya Myakota Petr Pribytkov Sergey Dunaev Gennady Kapustin Igor Mishin Natalya Gordeeva Leonid Kustov Alexander Kustov

1-Methylnaphthalene and the products of hydrogenation exhibit a high hydrogen storage capacity (6.6 wt.%), which makes them extremely promising as liquid organic hydrogen carriers. In this work, effective monometallic catalysts, 15Ni/Al2O3, 15Ni/Al2O3-SiO2, and 15Ni/Sib-ox, were synthesized and first investigated for hydrogenation of 1-methylnaphthalene to 1-methyldecalins. The prepared catalysts were characterized using a set of physicochemical analysis methods: SEM-EDX, TEM, XRD, N2 adsorption–desorption, FTIR and UV-vis-DRS. The catalytic activity of the samples in the hydrogenation reaction of 1-methylnaphthalene (100 min, 4 MPa, 240 °C) was studied in comparison to the traditional catalyst of hydrogenation, Ni Raney. The 15%Ni/Sib-ox catalyst showed a 100% conversion and high selectivity of 85.2% with respect to the target product 1-methyldecalins, while in the presence of Ni Raney, a selectivity of 74.3% was achieved with complete conversion of the substrate.

Molecules doi: 10.3390/molecules31111780

Authors: Xiaohui Cai Jun Men Qingwu Yang Yili Hu Zhixian Qiao

A derivatisation-free HPLC–MS/MS method was developed and validated for the simultaneous quantification of selenium- and sulphur-containing amino acids in soybean leaves, and applied to a 3 × 3 factorial hydroponic experiment probing selenium–sulphur metabolic interactions. The method resolves five biologically informative analytes (Cys2, SeCys2, MeSeCys, Met, SeMet) within 1.5 min through multiple reaction monitoring (MRM). Ultrasound-assisted extraction (UAE) of the free fraction was jointly optimised for both analyte classes by the response-surface methodology; enzymatic hydrolysis of the extraction residue recovered the protein-bound fraction on the same platform. Limits of detection ranged from 0.036 to 0.556 µg L−1, intra-day relative standard deviations were below 5%, and spike recoveries fell between 92.3 and 117.4%. Free SeAA and SAA pools were negatively correlated across the nine treatments (R2 = 0.83), consistent with competitive Se–S assimilation, whereas bound pools were positively correlated (R2 = 0.89), reflecting proportional protein-level incorporation. A regime of 1–5 mM of sulphate with 20 µM of selenite yielded the highest bound organo-Se with near-normal growth, providing leaf-level evidence that may inform future seed-focused studies aimed at Se-enriched soy-protein ingredient development.

Molecules doi: 10.3390/molecules31111779

Authors: Jing Shi Xiang Li Shuo-Jiang Song Li Feng

Heavy metal pollution from coal gangue severely degrades mine soil structure and threatens landscape ecological stability. Particularly, γ-polyglutamic acid (γ-PGA), a green biopolymer, offers potential applications for pollution remediation while supporting ecological restoration. To evaluate γ-PGA’s efficacy in immobilizing Pb, Cd, and Zn in gangue-based soil and clarify its regulatory mechanism for landscape-friendly remediation, soil samples from a 3-year-weathered gangue hill in the Liupanshui mining area were subjected to indoor leaching experiments with different γ-PGA doses, combined with material characterization and Density Functional Theory (DFT) simulations. The results showed that the optimal γ-PGA dose was 6 g/kg, achieving 93.25% Pb immobilization and reducing Cd/Zn migration risk by over 30%; γ-PGA acted via carboxyl-amide dual-site chelation and hydrogen-bonded agglomeration, forming stable aggregates that inhibited metal migration. DFT calculations confirmed strong chelation for Cu2+ (−59.54 kcal/mol, BSSE-corrected: −57.23 kcal/mol), while Pb2+ and Cd2+ showed weaker binding (−8.32 kcal/mol and −5.67 kcal/mol, BSSE-corrected: −6.15 kcal/mol and −3.89 kcal/mol, respectively), indicating multi-pathway immobilization mechanisms. This study provides a theoretical basis for applying γ-PGA in mine landscape ecological restoration.

Molecules doi: 10.3390/molecules31111778

Authors: Fanghua Mao Bowen Wang Zhengwang Chen Yin-Long Lai Huanfeng Jiang Jianxiao Li

3,6-Dihydro-2H-pyran heterocyclic framework is one of the currently developed heterocyclic building blocks in both pharmaceutical chemistry and organic synthesis, but with significant challenges. To overcome these challenges, herein, we report a robust synthetic methodology of palladium-catalyzed carboetherification of alkenes with alkynols for accessing polyfunctionalized 3,6-dihydro-2H-pyrans under aerobic oxidative conditions. In particular, this synthetic approach features excellent functional group compatibility, mild reaction conditions, and good step- and atom-economy. Additionally, an array of functional groups such as halogen group, ester, nitrile, aldehyde, phenoxy, and aromatic heterocycles were nicely tolerated, affording the synthetically challenging 2H-pyran derivatives in moderate-to-good yields. Notably, the practicability of this protocol is further verified by gram-scale synthesis and the late-stage diversification of pharmaceuticals and biologically active molecules.

Molecules doi: 10.3390/molecules31111777

Authors: Rajib K. Sarker Jennifer M. Murphy R. Michael van Dam

Fluorine-18 is often considered an ideal positron emitter owing to its excellent chemical, physiological, and nuclear properties. Consequently, the development of rapid, simple, and reliable 18F-labeling strategies remains critically important for synthesizing new radiopharmaceuticals for PET molecular imaging. A common approach involves the synthesis of 18F-labeled prosthetic groups that subsequently undergo bioconjugation with peptides or other biomolecules to generate 18F-labeled imaging probes. However, conventional synthetic methods for these prosthetic groups are often lengthy, require large quantities of precursor and solvent, and typically rely on elevated reaction temperatures. Herein, we report a droplet-based microscale synthetic methodology for the preparation of the [18F]FVSB prosthetic group that minimizes precursor and solvent usage, proceeds rapidly, and operates at relatively low temperatures. Conditions were optimized using a platform for performing droplet reactions in parallel, enabling high-throughput study of multiple reaction parameters within a short period of time. Additionally, we introduce a simple micro-cartridge purification technique that affords purified [18F]FVSB in small volumes. Furthermore, we describe an efficient bioconjugation that requires substantially lower reagent amounts than the previously reported macroscale method. The microscale process we report could facilitate wider use of this 18F-labeling strategy and can be extended to label other thiol-bearing peptides or biomolecules.

Molecules doi: 10.3390/molecules31111776

Authors: Micheal Arockiaraj J. Celin Fiona S. Ruth Julie Kavitha Arul Jeya Shalini Krishnan Balasubramanian

In the original publication [...]

Molecules doi: 10.3390/molecules31101775

Authors: Yutao Zhang Jiawei Bi Tiancheng Yuan Shenpeng Xia Minzhen Bao

A lightweight and high-efficiency microwave-absorbing material was developed via an in situ solvothermal pyrolysis strategy by anchoring sphere-like Fe3O4 nanostructures onto bamboo-derived porous carbon (BPC). The resulting composites preserve the intrinsic anisotropic honeycomb architecture of bamboo while introducing uniformly distributed magnetic nanoparticles, enabling synergistic dielectric–magnetic loss. Electromagnetic parameters, alongside impedance matching, were successfully modulated through the optimization of precursor concentrations. Of the evaluated materials, BPC-0.9 stood out for its intense attenuation, recording an RLmin of −45.17 dB at a 1.8 mm thickness. Furthermore, a significant effective absorption bandwidth of 6.65 GHz was attained by the BPC-0.6 sample at only 2.2 mm. Several factors contribute to the boosted efficiency, starting with conductive and interfacial polarization losses paired with multiple scattering events. Furthermore, magnetic loss components, encompassing eddy current effects as well as natural and exchange resonances, play a pivotal role in optimizing the material’s response. Furthermore, radar cross-section (RCS) modeling reveals a substantial reduction of 19.9 dB·m2, verifying the material’s viability for real-world stealth technologies. Our findings offer a straightforward methodology for fabricating magnetic carbon structures from biomass with adjustable dielectric responses, underscoring their potential in high-performance energy conversion and low-density microwave absorption.

Molecules doi: 10.3390/molecules31101774

Authors: Asma Kisalaei Vali Rasooli Sharabiani Ahmad Banakar Ebrahim Taghinezhad Mariusz Szymanek Agata Dziwulska-Hunek

This research aimed to develop a rapid, non-destructive, and accurate method for detecting adulteration in turmeric using Visible–Near-Infrared (UV/Vis and NIR) spectroscopy combined with machine learning algorithms. Spectral data from the samples were collected and analyzed in two ranges: 170–870 nm (UV/Vis) and 900–2170 nm (NIR). Four supervised learning algorithms, including Support Vector Machine (SVM), Linear Discriminant Analysis (LDA), the Multilayer Perceptron (MLP) neural network, and Decision Tree, were evaluated for modeling. To quantitatively assess model performance, we employed not only the accuracy metric but also complementary performance indicators including precision, recall, and the F1-score to provide a more comprehensive evaluation of classification effectiveness. The models developed in the 900–2170 nm spectral range demonstrated highly significant performance, with most models achieving 100% accuracy on the independent test set. To reduce data dimensionality and enhance computational efficiency, a hybrid feature selection method combining SVM with five algorithms—League Championship Algorithm (LCA), Genetic Algorithm (GA), Particle Swarm Optimization (PSO), Ant Colony Optimization (ACO), and Imperialist Competitive Algorithm (ICA)—was employed. Upon evaluation of each method, the SVM-LCA was selected as the optimal feature selection technique. This algorithm successfully extracted the most effective wavelengths with the highest correlation and lowest error, which maintained or improved the accuracy of the classification models. This study confirms the high potential of UV/Vis and NIR spectroscopy as rapid, non-destructive, and precise tools for detecting adulteration in turmeric. The findings can pave the way for the development of intelligent quality control systems in the food and pharmaceutical industries, playing a crucial role in ensuring consumer health and safety.

Molecules doi: 10.3390/molecules31101773

Authors: Sujin Lee Mei Zheng Kang Kim Kwang-Hoon Chun

NAD+ plays crucial roles in various biological processe and its aberrant regulation has been suggested to be critical in the pathogenesis of diverse diseases. Intracellular NAD+ is synthesized largely from nicotinamide mononucleotide (NMN), which is the product of reaction catalyzed by nicotinamide phosphoribosyltransferase (NAMPT). Thus, the development of specific inhibitors targeting NAMPT has been suggested as a promising treatment strategy. In this study, we developed a pharmacophore-based QSAR model to discover novel NAMPT inhibitors based on diverse structural features. By virtual screening using the conformation model, we could identify eight novel active analogs having distinct pharmacophores. The biological activity of these candidates on cell viability were further examined. Our study proves the efficiency of our novel screening model and demonstrates its usefulness in the application of drug discovery process.

Molecules doi: 10.3390/molecules31101772

Authors: Prawpan Inpota Nathawut Choengchan

This work presents, for the first time, a novel cross injection analysis (CIA) system for the simultaneous multi-determination of key biomarkers associated with diabetic nephropathy—namely, albumin, creatinine, and glucose—within a single analytical run. Unlike conventional flow-based techniques that rely on sequential measurements, the proposed CIA platform integrates multiple analytical pathways into a unified design, enabling one-shot multi-analyte analysis without the need for complex separation units or injection valves. The system employs peristaltic pumps and a rectangular platform with orthogonal flow channels, allowing concurrent aspiration and efficient transport of reaction products to compact detectors. Albumin determination was based on ion-association with tetrabromophenolphthalein ethyl ester. Creatinine was measured using the Jaffé reaction. Glucose was colorimetrically detected via its reaction with 3,5-dinitrosalicylic acid. The developed CIA provides enhanced sensitivity through its pre-mixing effect, enabling reliable quantification of trace analytes. Excellent analytical performance was achieved, including wide linear ranges (r2 > 0.99), good precision (RSD < 7%), and rapid analysis (5 min). The method was validated against established reference methods, showing no significant differences, and successfully applied to urine with satisfactory recoveries (84.8–107.3%). Importantly, the proposed system adheres to green chemistry by minimizing reagent consumption and waste generation, offering a sustainable approach for multi-parameter clinical analysis.

Molecules doi: 10.3390/molecules31101771

Authors: Stefano Econdi Sholpan Nazarkulova Stefano Marchesi Chiara Bisio Mukhambetkali Burkitbayev Matteo Guidotti

Iron-exchanged bentonites derived from a natural montmorillonite-rich clay (Taganskoe deposit, Kazakhstan) were prepared through a simple aqueous ion-exchange route using Fe(II) or Fe(III) inorganic salt precursors, yielding final Fe contents of ca. 5–7 wt.%, while preserving the smectite layered framework. A mild thermal treatment under air was applied to tune iron coordination without triggering major structural collapse. The resulting materials were characterized by ED-XRF, PXRD, FE-SEM/EDX, DLS/ζ-potential and DR UV–Vis–NIR spectroscopy, revealing predominantly exchanged Fe species with a limited fraction of surface iron-oxide clusters, whose contribution increases after activation. Structure–reactivity relationships were probed under mild conditions in liquid-phase ethyl acetate using dimethyl methylphosphonate (DMMP) and 2-chloroethyl ethyl sulfide (2-CEES) as organophosphorus and organosulfur hazardous chemicals and chemical warfare agent simulants, respectively. Fe(III)-bentonite enabled very fast DMMP removal (ca. 93% within 0.5 h) with a remarkable improved performance with respect to Fe(II)-bentonite and the pristine mineral clay. For 2-CEES, the presence of H2O2 markedly enhanced oxidation on Fe-containing clays, reaching quantitative abatement within 24 h (up to >90%), with strong retention of oxidized sulfur products by the clay matrix. These results highlight Fe-exchanged natural bentonites as robust, cheap and multifunctional adsorption/catalytic solids for decontamination and water-treatment applications.

Molecules doi: 10.3390/molecules31101770

Authors: Sandra Borges Tânia C. F. Ribas André Almeida Manuela Pintado

The rising global demand for protein-rich food has intensified interest in alternative and sustainable protein sources. Insects, particularly black soldier fly (BSF) larvae, represent promising substrates due to their high nutritional content and potential for valorization into functional ingredients. This study investigated the impact of pre-hydrolysis treatments on the efficiency of enzymatic hydrolysis using alcalase to enhance protein solubilization and bioactive peptide production. Pre-treatments included organic acids (propionic and acetic acid) and a pressure-thermal method. Results indicated that BSF larvae responded differently to the evaluated pre-treatment strategies. Notably, the pressure-thermal treatment combined with enzymatic hydrolysis increased soluble protein content by approximately 30% and antioxidant activity by approximately 20%, suggesting enhanced release of bioactive peptides. Although organic acid treatments increased protein solubility, they did not improve the degree of hydrolysis or antioxidant activity. These findings highlight the potential of pressure-thermal pre-treatment to improve the efficiency of protein extraction from insect biomass and support the integration of such approaches into food bioprocessing strategies aimed at developing novel, high-value protein ingredients.

Molecules doi: 10.3390/molecules31101769

Authors: Natalia Pachura-Hanusek Kamila Lewandowska Anna Burek Antoni Szumny Aleksandra Tabiś Sylwia Banaszkiewicz Jacek Bania Robert Kupczyński

Conifer-derived essential oils have gained attention as versatile natural additives with potential applications in animal production, including influencing microbial processes and supporting environmental sustainability. This study aimed to characterize the chemical composition of selected conifer essential oils (EOs), evaluate their antimicrobial activity against rumen microorganisms in vitro, and assess the effects of Pinus sylvestris essential oil on rumen fermentation and methane production under in vitro and in vivo conditions. EOs from Thuja occidentalis, Cupressus sempervirens, Juniperus communis, Picea mariana, Pinus sylvestris, and Pinus pinaster were analyzed by GC–MS, and their inhibitory activity against selected rumen bacteria was determined by MIC and IC50 assays. Based on these results, P. sylvestris oil was selected for fermentation experiments. Ninety-two volatile compounds were identified, with monoterpenes as the dominant constituents and α-pinene as the major compound in P. sylvestris oil. In vitro, P. sylvestris oil influenced fermentation in a dose-dependent manner without affecting ruminal pH. In vivo, ruminal pH, ammonia-related parameters, and total VFA concentration were not significantly affected by treatment, whereas several variables showed a significant effect of time. Temporal changes in VFA profiles suggested a transient adaptation of ruminal fermentation. Methane concentration was significantly (p < 0.01) reduced by Pinus sylvestris essential oil supplementation, with a decrease of approximately 28.7% after 14 days. These findings indicate that P. sylvestris EOs may serve as a promising natural modulator of rumen fermentation, although further studies are needed to optimize dosage and confirm long-term effects.

Molecules doi: 10.3390/molecules31101768

Authors: Sara Maia Helena Ferreira Maria Beatriz P. P. Oliveira Rita C. Alves

Coffee is among the most widely consumed beverages globally being cultivated in nearly 80 countries. Its processing generates large quantities of by-products, including mucilage, pulp/husks, silverskin, parchment, and spent coffee grounds. Although traditionally treated as waste, these residues are increasingly recognized as valuable resources rich in bioactive compounds exhibiting antioxidant, antimicrobial, and health-promoting properties. This review explores the antimicrobial potential of coffee by-products, with particular emphasis on their chemical composition and mechanisms of action. Compounds such as caffeine, chlorogenic acids, polyphenols, and melanoidins have demonstrated inhibitory effects against a broad spectrum of bacteria, including both Gram-positive and Gram-negative bacteria. Many of these compounds, which originate from plant’s defensive system or result from Maillard reactions, are known to disrupt microbial membranes, inhibit DNA repair, and interfere with pathogen metabolism. However, the available literature on their antimicrobial effectiveness remains limited. In the context of the rising worldwide concern over antimicrobial resistance, coffee by-products represent a sustainable and promising source of novel antimicrobial agents. Their valorization may support advances in food preservation, pharmaceutical innovation, and waste management practices, contributing to the implementation of a circular economy framework in the coffee industry while promoting environmental, economic, and social sustainability.

Molecules doi: 10.3390/molecules31101767

Authors: Jakub Garbarek Julia Karolina Markiel Wojciech Rzepka Kamil Glazik Magdalena Pitek Karolina Szewczyk-Golec Beata Kukulska-Pawluczuk Natalia Soja-Kukieła Alina Woźniak Jarosław Nuszkiewicz

Acute ischemic stroke (AIS) is associated with redox imbalance; however, the early temporal changes in enzymatic and non-enzymatic antioxidant responses are poorly understood. The aim of this study was to evaluate changes in selected oxidative stress markers during the early phase of AIS. The study was designed as a longitudinal within-subject analysis, with each patient serving as their own reference between day 1 and day 8. A total of 48 patients (mean age 69.31 ± 1.59 years; 56.3% male; mean body mass index (BMI) 27.05 ± 0.61 kg/m2), predominantly presenting with mild to moderate stroke severity, were enrolled in a prospective observational study. The cohort was characterized by a high prevalence of hypertension (87.5%), dyslipidemia (45.8%), and diabetes or prediabetes (45.9%). Blood samples were collected on day 1 and day 8 after stroke onset. Depending on the distribution of paired differences, either the paired Student’s t-test or Wilcoxon signed-rank test was applied. A significant increase in superoxide dismutase (SOD) activity was observed (1932.73 vs. 2086.55 U/g Hb, p = 0.032), whereas catalase (CAT; 403.19 vs. 415.30 × 103 U/g Hb, p = 0.444) and glutathione peroxidase (GPx; 24.70 vs. 24.40 U/g Hb, p = 0.477) showed no significant changes. Similarly, malondialdehyde (MDA) levels remained stable in both erythrocytes (182.96 vs. 187.15 nmol/g Hb, p = 0.838) and plasma (0.41 vs. 0.41 nmol/mL, p = 0.922). In contrast, melatonin (59.65 vs. 55.49 pg/mL, p = 0.042) and 25-hydroxyvitamin D (25(OH)D; 19.31 vs. 16.52 ng/mL, p < 0.001) concentrations significantly decreased. These findings suggest that the early phase of AIS may be associated with a selective and potentially maladaptive antioxidant response, involving increased SOD activity alongside depletion of systemic modulators, which may contribute to persistent redox imbalance.

Molecules doi: 10.3390/molecules31101766

Authors: Guohang Zhuang Liuye Mo Iemasa Yao

p-Methoxy-m-nitrobenzoic acid (MNBA) serves as a valuable chemical intermediate across numerous domains. Nevertheless, the synthesis of MNBA through non-catalytic oxidation processes invariably results in the production of environmentally polluting substances. In this study, we report an environmentally benign catalytic oxidation system for the synthesis of MNBA using water as a solvent. Based on the two-step TEMPO/KBr/NaOCl/NaClO2 system, which achieved a 91.4% yield at 70 °C, we have devised a simplified one-step procedure employing the TEMPO/KBr/NaClO2 system. This less energy-intensive input method yields 90.1% MNBA at 60 °C. Systematic optimization has revealed that temperature, time, and oxidant quantity are critical parameters. Furthermore, acidic conditions have been found to reduce yields due to the decomposition of NaClO2. The aqueous-phase approach completely avoids organic solvents and facilitates product isolation. A synergistic catalytic mechanism involving N-oxoammonium intermediates is proposed. This work establishes a sustainable strategy for preparing multifunctional aromatic carboxylic acids, addressing key challenges in both ecological impact and industrial scalability for fine chemical production.

Molecules doi: 10.3390/molecules31101765

Authors: Fatin Aqilah Mohd Nasir Nur Rabiatul Amierah Mohd Ariff Zulaikha Mohd Kamal Muhammad Adnan Iqbal Maria Khalid Faisal Jamil Vikneswari Perumal Puvana Devi Selvarajoo Tavamani Balan Sharon Fatinathan

Erythrosine B (ER) dye is widely used and increasingly detected in wastewater, necessitating effective removal. This study compares chitosan beads (CB) and chemically crosslinked beads, namely chitosan–tripolyphosphate (CT) and chitosan–sulphite (CS), for ER removal via batch adsorption studies. Characterisation confirmed successful crosslinking of the modified beads. Under optimised conditions, CB, CT, and CS achieved removal efficiencies of 75.27%, 91.69%, and 98.73%, respectively, at an initial concentration of 100 mg/L within 50–60 min. Kinetic analysis suggested that the rate-controlling step was not solely governed by intraparticle diffusion but also involved physisorption and chemisorption. While the Langmuir isotherm adequately described the adsorption process of CB and CT, with maximum adsorption capacities of 71.80 mg/g and 89.33 mg/g, respectively, a better fit was observed for the Freundlich and Redlich–Peterson isotherms, indicating multilayer adsorption. In contrast, CS showed moderate agreement with all isotherms, suggesting a complex removal process. CS demonstrated the highest adsorption capacity, with 120.30 mg/g, highlighting sodium metabisulphite (SM) as a promising crosslinking agent for improved dye removal. Density functional theory (DFT) analysis proposed that at the molecular level, interactions between the ionised oxygenated groups of ER and protonated amine groups of chitosan facilitated the adsorption process.

Molecules doi: 10.3390/molecules31101764

Authors: Jianyang Song Peng Xu Zhiheng Wei Huimin Yao Aohan Wang Changfeng Xu Yawei Zhu Rongrong Wang Xinfang Yuan

Ammonium nitrogen pollution presents a significant challenge in wastewater treatment. Traditional activated sludge processes often suffer from limitations such as low efficiency and high energy consumption when treating high-ammonium nitrogen wastewater. This study utilized previously screened high-efficiency heterotrophic nitrification aerobic denitrification (HN-AD) bacterial strains (Pseudomonas alcaliphila and Paracoccus versutus) synergistically with microalgae to construct an immobilized bacteria algae symbiotic system (IBAS). The nitrogen removal performance and microbial community response of the system were investigated under different nitrogen sources, carbon to nitrogen (C/N) ratios, and light intensities. Results demonstrated that the system achieved a removal rate of over 95% for nitrite and nitrate. Under conditions of C/N = 15 and high light intensity (335.36 μmol/(m2 · s)), the removal rates of NH4+-N, TN, and COD exceeded 90% without nitrite accumulation. Microbial community analysis revealed that high C/N conditions significantly enriched HN-AD functional bacteria (such as Acinetobacter) in the Pseudomonadota phylum and Gammaproteobacteria class. High light intensity promoted the proliferation of microalgae (Chlorella and Halochlorella), enhanced algal bacterial interaction, and improved system stability. This study elucidated the nitrogen removal mechanism of the IBAS under multi-factor regulation, providing a theoretical foundation and demonstrating application potential for low-carbon and high-efficiency wastewater treatment technologies.

Molecules doi: 10.3390/molecules31101763

Authors: Muhammad Farhan Qadir Somavia Ameen Rida Fatima Nadim Ullah Gamal A. Shazly Abu Summama Sadavi Bilal Mehwish Nazar Anoosha Sajjad Tawaf Ali Shah Yukun Yang

The journal retracts the article titled “Synthesis and Characterization of Metal Particles Using Malic Acid-Derived Polyamides, Polyhydrazides, and Hydrazides” [...]

Molecules doi: 10.3390/molecules31101762

Authors: Saulo Victor e Silva María Celeste Gallia Cristian Sillagana Verdezoto Leonardo Bajda Ana Ferrari Gabriel Araujo-Silva Jefferson Romáryo Duarte da Luz Maria das Graças Almeida Luisa Quesada Romero

This study investigated the influence of solvent composition on the extraction efficiency and selectivity of phenolic compounds from the Amazonian fruits açaí (Euterpe oleracea) and bacaba (Oenocarpus bacaba). Six choline chloride-based natural deep eutectic solvents (NaDES), combined with different hydrogen bond donors (glycerol, 1,2-propanediol, citric acid, lactic acid, oxalic acid, and urea), were compared with acidified methanol. Extracts were evaluated for total phenolic content (TPC), total flavonoid content (TFC), and antioxidant capacity using FRAP, DPPH, and ORAC assays. In açaí, methanol exhibited the highest TPC and reducing capacity, whereas acid-based NaDESs enhanced phenolic recovery in a matrix-dependent manner. In bacaba, choline chloride–citric acid enhanced total phenolic recovery compared to methanol, highlighting matrix-dependent solvent performance. Differences among FRAP, DPPH, and ORAC responses reflected variations in phenolic composition rather than total concentration alone. HPLC-DAD analysis revealed solvent-selective enrichment of anthocyanins, chlorogenic acid, flavan-3-ols, and rutin, particularly with acid-based NaDES formulations. Molecular docking provided complementary mechanistic insight by indicating favorable interactions between major phenolics and polyphenol oxidase. Overall, the results indicate that choline chloride-based NaDESs can function as tunable extraction systems capable of modulating phenolic profiles in a matrix-dependent manner, representing promising alternatives to conventional organic solvents for phenolic recovery from Amazonian fruits.

Molecules doi: 10.3390/molecules31101760

Authors: Tayssir Hamieh Mouhamad Rachini Soumaya Hamieh Mohammad Mahdi Assaf Zeinab Hamie Khaled Chawraba Thibault Roques-Carmes Joumana Toufaily

A comprehensive thermodynamic and molecular-level investigation of adsorption on MgY and NH4Y zeolites is presented using inverse gas chromatography at infinite dilution (IGC-ID), combined with a Hamaker-based formalism and an extended five-parameter Lewis acid–base model. The study introduces a unified framework that integrates dispersive, polar, and donor–acceptor interactions while explicitly accounting for temperature-dependent intermolecular geometry. The results demonstrate that the London dispersive free energy exhibits a highly linear temperature dependence (R2 > 0.999), while the corresponding surface energy decreases linearly with temperature (e.g., γsdT=−0.297T+189.48 mJ·m−2 for MgY), reflecting the progressive weakening of dispersion forces. Simultaneously, the intermolecular separation distance follows a linear relation r(T)=r0+αeffT, with αeff values on the order of (2–3) × 10−3 Å·K−1 for MgY, enabling the determination of intrinsic contact distances r0 at 0 K, varying between 4.00 Å and 6.60 Å. A major finding is that the molecular surface area of adsorbed probes is not constant but follows a quadratic temperature dependence with excellent accuracy (R2 > 0.999), establishing adsorption cross-section as a thermodynamic variable. The comparison between MgY and NH4Y reveals two distinct adsorption regimes: MgY exhibits a structured and strongly dispersive interaction field associated with Mg2+ cations, whereas NH4Y displays enhanced polarity, stronger specific interactions, and greater molecular flexibility driven by hydrogen bonding and protonic effects. Thermodynamic analysis of Lewis acid–base interactions shows that classical linear models are insufficient. Statistical evaluation (R2 ≈ 0.986, minimum AIC/BIC, lowest RMSE) demonstrates that the five-parameter Hamieh model provides the most accurate and physically meaningful description, capturing nonlinear donor–acceptor interactions and amphoteric coupling effects. Overall, this work establishes a novel thermodynamic methodology that quantitatively links macroscopic surface energetics to microscopic interaction parameters, providing new insight into adsorption mechanisms and a robust framework for the rational design of porous materials in catalysis, separation, and energy applications.

Molecules doi: 10.3390/molecules31101761

Authors: Joanna Horoszkiewicz Ewa Jajor Marek Korbas Jakub Danielewicz Jan Bocianowski Marzena Mikos-Szymańska Tomasz Szymczak Jagoda Kucharska Monika Kobiałka Marcin Podleśny

Plant extracts and microbiological supernatants were subjected to qualitative and compositional analyses to characterize their bioactive profiles and assess their potential agricultural applications. The garlic (Allium sativum) extract was rich in allicin and selected free amino acids, contained betulin as the dominant triterpene, and displayed a favorable elemental profile with high levels of potassium, phosphorus, sulfur, calcium, and magnesium, with no detectable heavy metals. Detectable amounts of B-group vitamins and vitamin E isoforms were also identified. Qualitative phytochemical screening confirmed the presence of saponins and flavonoids in the garlic extract. The Jerusalem artichoke (Helianthus tuberosus) extract exhibited a significantly higher total phenolic content compared to the garlic extract, with qualitative analysis confirming the presence of saponins, tannins, and flavonoids, suggesting a broader spectrum of bioactive compounds. The two bacterial supernatants were characterized by HPLC analysis and differed in their metabolic profiles: the Enterobacter sp. fermentation broth contained glycerol, 2,3-butanediol, and acetic acid, while the Paenibacillus sp. supernatant additionally contained lactic acid, ethanol, and succinic acid, reflecting distinct fermentation pathways. The in vitro and greenhouse studies aimed to evaluate biological preparations for controlling wheat diseases caused by fungi of the Fusarium genus as well as diseases affecting the stem base. Plant extracts (garlic—Allium sativum, Jerusalem artichoke—Helianthus tuberosus) and supernatants (fermentation broths) obtained with the Paenibacillus and Enterobacter bacteria were tested at three concentrations. In laboratory experiments, the degree of inhibition of the growth of the mycelium of the tested fungal species was determined, while in greenhouse studies, the effectiveness in limiting the development of stem base diseases and the impact of the applied biopreparations on plant growth were evaluated. Among the plant extracts, H. tuberosus demonstrated superior antifungal activity, achieving up to 100% inhibition of R. cerealis mycelial growth at 10% concentration and reducing disease severity by 34.3% compared to the untreated control under greenhouse conditions. Paenibacillus sp. supernatant demonstrated strong in vitro antifungal activity. The results indicate that H. tuberosus extract represents a promising candidate for further field evaluation as a component of sustainable wheat protection programs.

Molecules doi: 10.3390/molecules31101746

Authors: Jordana Georgin Younes Dehmani Noureddine El Messoaudi Dison S. P. Franco

This paper systematically reviews losartan, a hypertension pharmaceutical compound that is one of many newly identified emerging contaminants in water. Worldwide use of pharmaceuticals continues to grow, and losartan has been identified as a contaminant that frequently accumulates in aquatic systems as a result of this global increase in use. The paper presents systematic reviews on the environmental occurrence, physicochemical characteristics, analytical methods of detection, and remediation techniques associated with losartan contamination. Losartan is often detected at levels of ng L−1–µg L−1 in wastewater systems, surface water and marine ecosystems, very effectively demonstrating the inadequacies of existing conventional wastewater treatment facilities, which are typically capable of removing only 20–70% of the contamination, with this variability largely attributed to differences in hydraulic/solids retention times, operational conditions, influent organic load, and the limited microbial acclimatization to recalcitrant pharmaceutical compounds. Emerging remediation technologies demonstrate the potential for removal efficiencies of >90% include hybrid systems, advanced electrochemical processes, new improved adsorption systems, and novel material for adsorption. However, there are still considerable barriers to progress, including excessive energy use, high operating costs, and perhaps most concerning, potentially toxic transition products generated by partial degradation. Furthermore, the literature review identified key literature gaps: lack of specific regulations, absence of full-scale studies, and inconsistencies in by-product toxicity assessments. The conclusion of this review is that to achieve worldwide water security and sustainability of aquatic resources, effective mitigation of the environmental risks associated with losartan requires combined approaches comprising innovative technologies, comprehensive ecotoxicological investigations, and improved collaboration between scientists, policymakers, and industry.

Molecules doi: 10.3390/molecules31101759

Authors: Xiaoyun Xia Xiandong Du Zhifeng Chen Sisi Yu Chaojie Wang

Triple-negative breast cancer (TNBC) is a clinically aggressive malignancy with extremely limited effective targeted therapies. Natural products are promising alternatives for anticancer drug discovery, whereas integrated computational approaches serve as efficient tools for novel lead identification. Herein, four novel spiro-polycyclic sesquiterpene [4+2] trimers (Inubritantrimers A–D) and eight synthetic derivatives from Inula britannica L. were investigated via DFT calculations at the ωB97xD/6-311++G(2d,p) level (for geometric, electronic, spectral, and reactivity parameters), network pharmacology, molecular docking against seven core breast cancer-related targets, 500 ns all-atom molecular dynamics (MD) simulation, and MM/PBSA analysis. The results showed that the endo-type cycloaddition products had superior structural stability, with all reactions thermodynamically spontaneous (ΔG < 0). Compound 11 exhibited the most potent and balanced binding activity, with a docking free energy of −13.45 kcal/mol to MTOR; MD and MM/PBSA confirmed stable complex formation (total binding free energy −21.13 kcal/mol), driven predominantly by hydrophobic interactions. This study first established a comprehensive stereochemistry–electronic structure–property–activity relationship for this rare sesquiterpene trimer class and identified compound 11 as a promising MTOR-targeted TNBC lead. It provided a theoretical basis for developing high-efficiency, low-toxicity natural anticancer agents.

Molecules doi: 10.3390/molecules31101757

Authors: Ganga Reddy Velma Srinivasa Reddy Telukutla Jayaram Vankudoth Ajmer Singh Grewal Steven Privér Poornachandra Yedla Ravikumar Akunuri Donald Wlodkowic Srihari Pabbaraja Suresh K. Bhargava Magdalena Plebanski Ahmed Kamal

Pharmacophore hybridization is a well-established strategy for developing novel anticancer agents with improved biological profiles. In this study, a new series of (E)-4-(4-acrylamidophenoxy)-N-methylpicolinamide derivatives has been rationally designed by hybridizing key structural features of sorafenib with cinnamide pharmacophores and subsequently synthesized. The antiproliferative activities of the synthesized compounds were evaluated against a panel of human cancer cell lines, including A549 (lung), DU-145 (prostate), SKOV3 (ovarian), and HepG2 (liver), along with non-cancerous Hek293T cells. In comparison with the standard drug sorafenib, most of the (E)-4-(4-acrylamidophenoxy)-N-methylpicolinamides demonstrated significant antiproliferative activity, with specificity toward the HepG2 (liver cancer) cell line, and no effect on the noncancerous cells (Hek293T). Among them, compound 5f, the derivative containing a trifluoromethyl-substituted cinnamoyl moiety was identified as the lead candidate, exhibiting an IC50 of 5.3 µM towards HepG2 (liver) cancer cells, comparable to the reference drug sorafenib. Enzyme inhibition studies showed that compound 5f inhibited both b-Raf and VEGFR-2 with IC50 values of 1.45 and 0.37 µM, respectively. Furthermore, compound 5f suppressed angiogenesis in vitro and in vivo, as evidenced by the tube formation assay using HUVECs and in transgenic zebrafish Tg(fli1a:EGFP) models, respectively. Mechanistic studies indicated that compound 5f induced apoptosis in HepG2 cells through mitochondrial membrane depolarization and increased ROS generation. Molecular docking studies supported experimental findings and showed that 5f can interact with catalytically active residues via hydrogen-bonding interactions. Overall, these results highlight the potential of compound 5f as a promising dual target therapeutic lead with dual direct anticancer and antiangiogenic properties.

Molecules doi: 10.3390/molecules31101758

Authors: Corina Carranca Filipe Pedra Gustavo Brunetto Joana Barata

The degradation of mulch materials in perennial cropping systems is governed by both polymer properties and environmental conditions. Their relative influence under field conditions remains unclear. To our knowledge, this study is one of the first to integrate mass loss measurements, polymer characterization, and soil microclimatic assessment under field conditions. A one-year field experiment was conducted under irrigated Mediterranean conditions to compare the degradation of Kraft® paper and polybutylene adipate terephthalate (PBAT)-based (Kritifil®) mulch with polypropylene (PP) geotextile fabric and polyethylene (PE) mulch in randomized blocks, with three replicates. Mass loss was quantified in situ using mesh bags, while soil moisture, temperature, and electrical conductivity (EC) were monitored monthly to characterize microclimatic and edaphic conditions underlying mulch treatments. Polymer changes were assessed by ATR-FTIR analysis of field-exposed mulch fragments. Kraft® paper degraded rapidly (≈72% mass loss), consistent with moisture-driven biological processes and susceptibility to hydrolysis. In contrast, PBAT-based mulch showed limited degradation (≈3.5%) despite favourable conditions, suggesting constraints in enzymatic activity. No mass loss was observed for PE- and PP-based mulch. ATR-FTIR analysis indicated minimal structural changes in PBAT, PP, and PE, reflecting their high stability. Overall, polymer composition and inherent (bio)degradability, rather than soil thermal time, were the main drivers of mulch (bio)degradation under Mediterranean conditions.

Molecules doi: 10.3390/molecules31101754

Authors: Noufal Komby Abdulla Elham A. Alzahrani Ghaida H. Munshi Abeer Mohammed AL-Balawi Salwa D. Al-Malwi Naha Meslet Alsebaii Sumbul Hafeez Seungdae Oh Saif Ali Chaudhry

In this study, manganese ferrite was grown on the surface of a low-cost powder substrate of a guava leaf using the co-precipitation method. The resulting material was characterized using various spectroscopic and microscopic techniques. The composite was formed through the electrostatic and non-electrostatic interactions between the manganese ferrite nanoparticles, and the functional groups present on the guava leaf substrate; consequently, a high content of functional groups was observed in the synthesized composite through the Fourier transform infrared spectroscopy. The average size of the nanoparticles grown on the guava leaf substrate was determined to be between 3 and 5 nanometers. The synthesized composite material was utilized for adsorption applications, employing Methylene blue dye as a model adsorbate. Methylene blue was removed from the aqueous solutions under various conditions—including variations in the pH, contact time, temperature, and concentration. Under optimal conditions, it was observed that an adsorbent dosage of 2 g L−1 was capable of removing approximately 99% of the dye from a 10 mg L−1 dye solution at pH 7. The dye removal efficiency (%) decreased with the increasing temperature, indicating an exothermic process; this was further confirmed by the thermodynamic parameter analysis (specifically, the change in enthalpy, or ΔH), which yielded a negative value. Gibbs Free Energy (ΔG) also yielded a negative value, signifying the feasibility and spontaneity of the adsorption process. In this study, the adsorption process followed the Freundlich isotherm model, with the value of ‘n’ falling between 1 and 10, which is indicative of heterogeneous adsorption. The adsorption kinetics were determined to follow a pseudo-second-order model, and the overall rate-limiting step of the process was identified as intraparticle diffusion. To assess the sustainability and stability of the adsorbent, regeneration and reusability experiments were conducted. The results revealed that the modified guava leaf performed effectively for up to five cycles, achieving an adsorption efficiency of approximately 24% after the final cycle. Thus, the developed adsorbent proved to be an effective material for the removal of Methylene blue dye.

Molecules doi: 10.3390/molecules31101749

Authors: Anna Sadowska Daria Włosek-Pawełas Halina Car

Medicinal mushrooms have become an important component of modern dietary supplementation and functional nutrition due to their diverse biological activities and long-standing use in traditional medicine. Among the most widely studied and utilized species are Ganoderma lucidum, Lentinula edodes, Grifola frondosa, Cordyceps militaris, Cordyceps sinensis, Trametes versicolor, and Inonotus obliquus. Their therapeutic potential is associated with a wide range of biologically active constituents, including polysaccharides, triterpenoids, phenolic compounds, and other secondary metabolites. Experimental and clinical studies indicate that extracts derived from these species may support immune function, modulate inflammatory responses, and exhibit antioxidant, antimicrobial, and anticancer properties. In addition to extensive in vitro and in vivo investigations, a growing number of clinical studies have evaluated the safety and potential therapeutic benefits of medicinal mushroom preparations in humans. In recent years, increasing attention has been directed toward their incorporation into nutraceutical formulations and functional foods aimed at supporting health and preventing chronic diseases. Advances in cultivation technologies and extraction methods have also contributed to improved availability and standardization of mushroom-derived products. This review provides a comprehensive overview of selected medicinal mushroom species commonly used in dietary supplements, focusing on their bioactive constituents, reported biological activities, and potential applications in contemporary medicine.

Molecules doi: 10.3390/molecules31101755

Authors: Fan Qiu Cunbao Ling Shaoyue Wang Siyuan Chen Liping Liu Xuan Wang Yuping Chen

Mulberrofuran A (MFA), a natural product originally isolated from the root bark of Morus alba L. (Sang-Bai-Pi), is a structurally distinctive mulberry-derived 2-arylbenzofuran bearing a prenyl-related side chain. Although MFA has attracted attention because of its phytochemical uniqueness and reported biological relevance, the available evidence specific to MFA remains limited and fragmented. In addition, pharmacological interpretations are often complicated by the frequent use of indirect evidence derived from structurally related mulberrofuran analogues, other arylbenzofurans, or complex Morus extracts. This review critically summarizes current knowledge on the chemistry, occurrence, and biological relevance of MFA, while explicitly distinguishing direct MFA-specific evidence from indirect and contextual evidence. Available studies suggest that MFA may be associated with antimicrobial activity and modulation of arachidonic acid-related inflammatory pathways, whereas its putative roles in metabolic regulation, cardiovascular protection, antiviral activity, antioxidant effects, and anticancer relevance are currently supported mainly by structurally related compounds or broader mulberry literature rather than robust MFA-specific validation. We further discuss the limitations of the current evidence base, including methodological heterogeneity, incomplete statistical reporting, the lack of pharmacokinetic and toxicity data, and the absence of clinical validation. Rather than establishing MFA as a confirmed therapeutic agent, the available literature supports its consideration as an emerging natural product candidate that warrants rigorous chemical, pharmacological, and translational investigation.

Molecules doi: 10.3390/molecules31101756

Authors: Igor V. Nechaev Alexey V. Krisilov Vladislav E. Chernov Marina G. Holyavka

Dimetallofullerenes are obtained in synthesis in parallel to monometallofullerenes, but they are less studied because their yields are considerably lower. In this work, DFT modeling of Gd2@C82 endohedral metallofullerene (EMF) has been performed. A total of 32 isomers of Gd2@C82 have been established, the most stable of which form the C2v(9)-C82 structure. The similarity of the infrared (IR) spectra of the ground and excited states of C2v(9)-C82 is here established.

Molecules doi: 10.3390/molecules31101753

Authors: Zhiyi Yu Xuehan Yang Bin Sun Yuhan Jiang Yanfei Shi Meishuang Zhang Siwei Zhang Fengying Guan

Non-coding RNAs are pivotal regulators of metabolic disease pathogenesis, yet the role of microRNA-27a (miR-27a) in obesity-associated hepatic steatosis remains incompletely characterized. This study examined the functional contribution and molecular mechanism of miR-27a in regulating hepatocyte mitochondrial homeostasis and lipid metabolism. Utilizing in vivo mouse models, including low-fat diet controls, high-fat diet (HFD)-induced obesity, and gain- and loss-of-function approaches, miR-27a was found to be markedly upregulated in the serum and liver of obese mice, correlating with disrupted glucose and lipid homeostasis as well as hepatic steatosis. Mechanistically, miR-27a overexpression recapitulated HFD-induced mitochondrial dysfunction, manifested by decreased mitochondrial biogenesis and elevated reactive oxygen species (ROS) production. Conversely, genetic silencing of miR-27a restored mitochondrial integrity and mitigated lipid accumulation. In vitro experiments using HepG2 cells confirmed that miR-27a directly suppresses nuclear factor erythroid 2-related factor 2 (NFE2L2), and NFE2L2 overexpression counteracted miR-27a-induced mitochondrial damage and steatosis. Collectively, these results demonstrate that miR-27a promotes hepatic steatosis by targeting NFE2L2, leading to mitochondrial impairment and oxidative stress, highlighting miR-27a as a potential biomarker and therapeutic target for obesity-associated liver metabolic disorders.

Molecules doi: 10.3390/molecules31101748

Authors: Patrycja Zawiślak Justyna Kapelewska Izabela Ryza Joanna Karpińska Urszula Kotowska

Conventional wastewater treatment systems cannot effectively eliminate micropollutants such as contaminants of emerging concern (CECs). These compounds, even at trace levels, are persistent or pseudo-persistent, bioaccumulative, and potentially harmful to ecosystems and human health. Advanced oxidation processes (AOPs), based on the in situ generation of highly reactive oxygen species, have emerged as promising solutions. Peroxyacetic acid (PAA) has gained attention due to its strong oxidizing capacity, broad antimicrobial activity, environmentally benign by-products, and compatibility with different activation methods. This review provides an updated and integrated synthesis of recent advances in PAA-based AOPs for the degradation of major CEC groups, including pharmaceuticals, personal care products, pesticides, and industrial chemicals, as well as for the oxidative modification of microplastics (MPs). The review discusses several strategies for PAA activation and critically discusses removal efficiency, underlying mechanisms, and current limitations, emphasizing the gap between pollutant transformation and complete mineralization. Furthermore, the article highlights a key research need, which is the assessment of the toxicity of transformation products and their validation under realistic conditions. Overall, this review provides insight into the potential and challenges of PAA-based AOPs for sustainable water treatment.

Molecules doi: 10.3390/molecules31101752

Authors: Kristina Mojsilović Rastko Vasilić Marko Dević Nenad Tadić

Plasma electrolytic oxidation (PEO) enables the fabrication of multifunctional oxide coatings with embedded active phases, offering a promising route for durable photocatalytic surfaces in water purification. This study examines how the electrical regime affects particle incorporation and photocatalytic performance. Coatings were produced under a 50% duty cycle in both unipolar mode and during the anodic part of the bipolar mode. A silicate-based electrolyte was modified with zeolites (Y and ZSM5), used in pristine form, Zn-loaded form, and combined with ZnO nanoparticles, to enhance catalytic activity. Photocatalytic performance was evaluated via methyl orange degradation under simulated solar irradiation for 6 h. The highest efficiency (~45%) was achieved with unipolar coatings containing Y zeolite and ZnO. In contrast, bipolar coatings with combined Y and ZnO showed lower efficiency (~35%). Although lower than typical powder photocatalysts, these results are notable since active phases are directly embedded in the coating, and both modes improve the photocatalytic activity by ~10% compared to the standard electrolyte. Microstructural analysis revealed that bipolar coatings were more compact, limiting access to active sites. Unipolar processing enabled better particle incorporation and a morphology more favorable for photocatalytic activity, making it the more effective regime for developing PEO-based photocatalytic coatings.

Molecules doi: 10.3390/molecules31101751

Authors: Wenyu Liu Defa Liu Bin Sun Xingpeng Liu Pengfei Gao Xiao Lin Guowei Zhou

The reasonable structural design and interfacial modification of heterojunction photocatalysts for accelerated charge separation and boosting photocatalytic activity remains a crucial challenge in solar-driven water splitting for H2 production. Herein, a hierarchical structured In2S3/Ti3C2/TiO2 ternary heterojunction was effectively constructed through a facile hydrothermal method integrated with a self-assembly strategy, in which Ti3C2 and TiO2 were loaded on the surface of hierarchical In2S3 microspheres assembled from nanosheets. In the photocatalytic system, the in situ electron paramagnetic resonance verifies that the photogenerated charge transfer between In2S3 and TiO2 obeys a typical S-scheme mechanism. Meanwhile, the introduction of Ti3C2 MXene as a conductive cocatalyst further promotes the separation and transfer of photogenerated charge through the formation of a Schottky junction, thus remarkably boosting the photocatalytic performance. Under simulated sunlight irradiation, the In2S3/Ti3C2/TiO2 ternary heterojunction exhibits a superior H2 production rate compared to pure TiO2 and In2S3. Moreover, the ternary heterojunction also displays outstanding stability after five consecutive cycling tests. This work highlights the synergistic integration of an S-scheme and Schottky junction in a ternary heterostructure for efficient charge separation, providing a feasible strategy for designing high-performance photocatalysts toward solar-driven H2 production.

Molecules doi: 10.3390/molecules31101750

Authors: Toktam Mohammadi-Moghaddam Hamid Bakhshabadi Afsaneh Morshedi Seyed Mehdi Hosseini Marcos E. Valdes

In industrial soybean lecithin production, process variables such as temperature, water content, agitation, and processing time play a critical role in determining the final product quality. Despite their importance, the combined effects of these parameters under industrial-scale conditions have not been sufficiently quantified. Therefore, this study systematically evaluated the influence of processing temperature (70–80 °C) and water content (1.5–3% w/w of oil) on key quality attributes, including lecithin moisture content, purity, acidy number, and peroxide value, as well as soybean oil acidity and insoluble fine substances. A response surface methodology (RSM) approach was applied to model the relationships between variables and to identify optimal processing conditions. The results indicate that an increasing temperature reduces lecithin moisture content, likely due to enhanced water evaporation and improved phase separation, while simultaneously increasing peroxide value and oil acidity (p < 0.05), possibly because of accelerated lipid oxidation and hydrolysis. Lecithin purity improved up to 75 °C, indicating more efficient separation, but decreased at higher temperatures, suggesting thermal degradation or emulsification effects. Similarly, increasing water content led to higher moisture, peroxide value, and acidy numberin lecithin, as well as increased acidity and insoluble fine substances in soybean oil (p < 0.05), which can be attributed to excessive hydration promoting emulsion stability and entrainment of oil-phase impurities into the lecithin fraction. Process optimization indicated that a water content of 1.5% and a temperature of 73.93 °C yielded the highest overall product quality, with a desirability value of 0.874.

Molecules doi: 10.3390/molecules31101747

Authors: Mohamed Brahmi Sara Moumnassi Adem Gharsallaoui

Interactions between resveratrol and biological or carrier systems play a key role in determining its bioavailability, stability, and delivery performance. These interactions involve proteins, lipids, cyclodextrins, nucleic acids, polysaccharides, and other formulation matrices, and are governed by noncovalent forces such as hydrogen bonding, hydrophobic interactions, π–π stacking, and desolvation effects. This review examines how complementary spectroscopic, calorimetric, structural, and computational techniques are used to characterize resveratrol interactions. Fluorescence, UV–visible spectroscopy, circular dichroism, FTIR, NMR, ITC, DSC, X-ray diffraction, molecular docking, and molecular dynamics simulations are discussed according to their contribution to binding analysis, conformational assessment, thermodynamic interpretation, structural organization, and complex stability. By integrating these approaches, this review provides a technique-oriented framework for understanding resveratrol binding and guiding the development of more stable resveratrol-based carrier systems and bioactive formulations.

Molecules doi: 10.3390/molecules31101745

Authors: Songkai Qiu Ruihao Li Yu Zhang Hanbing Zheng Yuqun Zou Zhuowei Cheng

Bioelectrochemical systems (BESs) for nitrogen removal, which integrate electrochemical processes with biological nitrogen removal technologies, is a sustainable and energy-efficient alternative to conventional biological nitrogen removal methods. However, the practical application of BESs for nitrogen removal remains limited due to technical challenges, and existing reviews have not provided an integrated analysis that systematically links mechanistic understanding, operational optimization, and engineering-scale challenges across multiple BES configurations. Therefore, the mechanisms and performance of main nitrogen removal pathways in BESs are critically summarized and compared within a unified framework. Low nitrogen removal rate and long-term instability are identified as the main challenges. Furthermore, the links between nitrogen removing performance and the key operational parameters, including substrate concentration, applied voltage, electrode materials and microbial interactions are systematically analyzed to reveal their influences and optimization opportunities. Finally, based on this integrated analysis, alternatives are proposed to improve the nitrogen removal rates and stability of BESs for nitrogen removal.

Molecules doi: 10.3390/molecules31101744

Authors: Fugui Cai Jie Ren Yuqing Yao Hanying Li

Using the gel-grown method to control the morphology of crystals attracts extensive attention. Potassium dihydrogen phosphate (KDP) is a nonlinear optical crystal with a high laser damage threshold. Here, we studied the crystallization of KDP in silica gel. The kebab-like KDP crystals (multiple KDP crystals aligning along a straight line) were prepared in the silica gel. In situ observation revealed that the kebab-like crystals were obtained through secondary nucleations on preformed needle-like crystals. Further investigation revealed that the hydroxyl groups on the gel network have an important influence on the formation of kebab-like KDP crystals. The hydroxyl groups on the gel networks can form hydrogen bonds with the phosphoric acid group of the KDP crystal and hinder the growth of the prismatic KDP faces, which leads to the preformation of needle-like crystals. Additionally, the influence of the acetic acid concentration and antisolvent on morphology was also studied.

Molecules doi: 10.3390/molecules31101743

Authors: Jiabin Sun Xinjian Song Yuan Zhang

Electrochemical sensors have emerged as promising tools for rapid pesticide screening in food and environmental samples because they combine simple instrumentation, fast response, portability, and compatibility with disposable electrodes. This review organizes recent progress through a cross-system framework linking pesticide class, interfacial electrochemical process, and material design. Carbon materials, metal–organic frameworks and their derivatives, metal nanoparticles, metal compounds, conducting polymers, MXene-based composites, and selected emerging materials are compared in terms of enrichment capability, charge-transfer regulation, catalytic amplification, recognition-layer integration, and suitability for real-sample analysis. Emphasis is placed on issues that are often under-discussed in performance-centered surveys, including matrix interference, electrode fouling, batch-to-batch reproducibility, storage stability, scalability, and cost-effectiveness. Representative examples show that the most useful advances arise not simply from lowering the limit of detection but from improving structure–function understanding and translating interfacial design into robust analytical performance. Future work should prioritize standardized fabrication and benchmarking protocols, in situ and operando identification of active sites and interface evolution, matrix-specific antifouling validation, multiresidue and metabolite analysis, and hybrid portable devices coupled with intelligent readout.

Molecules doi: 10.3390/molecules31101742

Authors: Maria-Ioanna Stavropoulou Antigoni Cheilari Konstantia Graikou Ioanna Chinou Nektarios Aligiannis

Propolis is a resinous bee product with a long history of medicinal use, valued for its antimicrobial, antioxidant and anti-inflammatory properties. Identification of its key bioactive constituents would enable chemical standardization and quality control of propolis-based products, once their activity is confirmed. In the current study we investigated a Greek propolis sample (PR09) belonging to a phenolic-rich type, dominated by flavonoids. After extraction and fractionation with Fast Centrifugal Chromatography (FCPC), the fractions were evaluated for their DPPH and collagenase inhibitory activity while their NMR metabolic profiles were recorded. NMR HeteroCovariance Approach (NMR-HetCA) analysis of PR09 propolis methanolic extract revealed the presence of 26 secondary metabolites: seven diterpenes, 13 flavonoids and six caffeic acid esters. All compounds were identified from NMR-HetCA and Statistical Total Correlation Spectroscopy (STOCSY) plots prior to their isolation. NMR-HetCA analysis indicated that caffeic acid derivatives were the most potent inhibitors of the DPPH free radical and collagenase. Additionally, galangin (11) and 3-O-methyl galangin (24) appeared to contribute considerably to the antioxidant activity, while together with pinocembrin (12), they all contributed to the extract’s collagenase inhibitory activity. In contrast, metabolites such as isocupressic acid (8), 13-epi-cupressic acid (18), pinostrobin (17) and chrysin (7) appeared not to contribute to the observed activities. Bioassays of selected metabolites confirmed the NMR-HetCA’s predictions, with caffeic acid phenethyl ether (1) exhibiting very high inhibition (92.54 ± 0.16%), and notable collagenase inhibition close to 50% (at 100 μg/mL). Overall, the findings demonstrate that NMR-HetCA enables rapid identification of bioactive compounds in propolis extracts and is proposed as a tool in accelerating the evaluation of propolis samples prior to laborious isolation procedures.

Molecules doi: 10.3390/molecules31101741

Authors: Keke Zhang Xiateng Qin Yan Zhao Rui Wang Changyong Li Suotang Jia

We report a comprehensive spectroscopic investigation of p-diethynylbenzene (pDEB) using two-color resonance-enhanced multiphoton ionization (REMPI) and mass-analyzed threshold ionization (MATI) spectroscopy, complemented by density functional theory (DFT) calculations. The S1 ← S0 electronic origin is observed at 34,255 ± 2 cm−1. The adiabatic ionization energy (IE) is determined to be 69,095 ± 5 cm−1 from two-color MATI spectra recorded via the S1 origin. Notably, a narrow peak is observed at 32 cm−1 above the IE in the two-color MATI spectrum, which is assigned to a one-color, two-photon accidental resonance arising from the near-resonant condition where the S1 ← S0 transition energy (34,255 cm−1) is close to half of the IE (69,099/2 = 34,549.5 cm−1). This observation is consistent with similar reports for p-chlorofluorobenzene and p-difluorobenzene. Franck–Condon simulations show good agreement with the experimental spectra. The present results provide a spectroscopic basis for identifying pDEB and distinguishing it from its ortho and meta isomers.

Molecules doi: 10.3390/molecules31101740

Authors: Cheng-Fu Huang Jia-Feng Chang Hui-Shan Yang Chih-Ping Hsu Chih-Cheng Lin

Extracted from Ganoderma lucidum mycelium, the developed β-1,3;1,6-glucan rich polysaccharides have the potential to be used during the industrial production of health food products due to their inhibition of metabolic syndrome, immunomodulatory and antitumor activities and other health benefits. Ganoderma active polysaccharides (GAP) have also been found to promote skin health, particularly due to their antioxidant and anti-aging properties. The present study investigates the skin-protective properties of polysaccharides purified from Ganoderma mycelium cultivated using stress-tolerance technology and a fully plant-based medium. The effects of the GAP are investigated in both in vitro and human studies. The results of the study indicate that the developed GAP effectively inhibit 32.4% of tyrosinase activity and 30.6% of melanin production in B16F10 cells. Furthermore, in scratch assays using NIH 3T3 cells, these GAP also promote cell migration and wound healing. In human studies, GAP demonstrated no potential for skin irritation while effectively reducing skin wrinkles, enhancing skin brightness, diminishing erythema, and increasing epidermal hydration. In hot-flux patch-induced erythema experiments, these GAP were found to be capable of alleviating erythema severity by up to 48%. The present study demonstrates that GAP, which can be produced industrially using innovative technologies and is rich in highly water-soluble β-1,3;1,6-glucan with a triple-helix structure, holds potential for application in the skincare industry.

Molecules doi: 10.3390/molecules31101739

Authors: So-Hyun Shin Jihyun Kim Hyungkyu Moon T. Sheshashena Reddy Myung-Seok Choi

Copper is an indispensable trace element for maintaining metabolic homeostasis; however, the dysregulation and subsequent accumulation of Cu2+ are critically linked to neurodegenerative pathologies, including Alzheimer’s disease in humans. Consequently, the development of robust analytical tools for Cu2+ monitoring is of paramount importance. Here, we report a 2,2′-dipicolylamine porphyrin (DPAP)-based fluorescent sensor designed for the precise detection of metal cations. Photophysical investigations reveal that DPAP operates via a rapid turn-off fluorescence mechanism, achieving high-performance sensing in the parts-per-million range. Notably, the probe demonstrates exceptional sensitivity with detection limits of 26.3 nM for Cu2+ and 34.8 nM for Ni2+. Interference studies demonstrated the selectivity of DPAP for Cu2+ over a diverse range of competing metal ions such as Na+, Ag+, Ni2+, Cr3+, Pb2+, Al3+, Fe2+, Cd2+, and Zn2+. These results indicate that DPAP is a sensitive and selective probe suitable for copper ion detection.

Molecules doi: 10.3390/molecules31101738

Authors: Süheyla Tongur Sefa Çetin

Wastewater containing high pollutant loads is discharged into the municipal sewerage system by industrial facilities operating within the industrial zones of Konya, Türkiye. Although regulations mandate that wastewater be treated to comply with specified discharge standards, some facilities lack pretreatment systems due to high capital and operational costs, while existing systems experience operational deficiencies. As a consequence, operational disruptions and increased environmental risks occur within the municipal sewerage system. Periodic sampling and inspection activities conducted by municipal authorities are becoming increasingly challenging for effective monitoring and evaluation as the number of facilities increases. In this study, a Geographic Information System (GIS)-based approach was developed to enhance monitoring effectiveness, and industrial wastewater quality data were analyzed using ArcGIS Pro 2.9 software (Esri, Redlands, CA, USA) to generate spatial pollution distribution maps. Samples were collected from five industrial facilities and four sewer junction points located in the Hacıyusufmescit, Emirgazi, and Fetih neighborhoods, where odor problems are frequently reported, during the 2022–2023 period. It was determined that COD (24,960 mg/L), BOD (2970 mg/L), and oil and grease (254 mg/L) concentrations significantly exceeded the regulatory discharge limits, particularly during the summer season. The results demonstrate that GIS-based monitoring systems constitute an effective tool for the early detection of pollution and odor-related problems at the urban scale, for the systematic management of control processes, and for the facilitation of evidence-based decision-making.