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Keywords = nuclear magnetic resonance spectroscopy (NMR)

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25 pages, 5668 KB  
Article
Synthesis, Characterization, and Magnetic Properties of Fe(BIP)3, a Novel Paramagnetic Relaxation Agent
by Federico Vavassori, Pietro Anzini, Marco Lamperti, Matteo Uboldi, Sandro Recchia, Giosuè Saibene, Veronica Remori, Roberto Tallarita, Benedict Josua Elvers, Carola Schulzke, Mauro Fasano, Andrea Penoni, Veronica Pettinato, Luca Nardo and Angelo Maspero
Pharmaceuticals 2026, 19(2), 221; https://doi.org/10.3390/ph19020221 - 27 Jan 2026
Viewed by 48
Abstract
Background/Objectives: First row transition metal ions have recently regained attention in coordination chemistry as alternatives to gadolinium-based paramagnetic contrast agents, motivated by emerging safety concerns associated with certain Gd3+-based contrast agents. In this study, we report the development of a [...] Read more.
Background/Objectives: First row transition metal ions have recently regained attention in coordination chemistry as alternatives to gadolinium-based paramagnetic contrast agents, motivated by emerging safety concerns associated with certain Gd3+-based contrast agents. In this study, we report the development of a novel homoleptic diketonate Fe3+ complex functionalized with biocompatible indole moieties. We investigate its potential as a paramagnetic relaxation agent by evaluating its ability to modulate the T1 and T2 relaxation times of water proton. Methods: Iron(III) tris-1,3-(1-methylindol-3-yl)propanedionate [Fe(BIP)3] was synthesized via a thermal method from bis(1-methylindol-3-yl)-1,3-propanedione (HBIP) using Fe(ClO4)3∙6 H2O as the metal source. The complex was characterized by UV-Vis, IR and NMR spectroscopy, differential scanning calorimetry–thermogravimetric analysis, and single-crystal X-ray diffraction. Fe(BIP)3 aggregation behavior in aqueous environment, including size and morphology of aggregates, was investigated using dynamic light scattering and scanning electron microscopy. Incorporation of the aggregates into phospholipid vesicles was evaluated by fluorescence resonance energy transfer and fluorescence correlation spectroscopy. The paramagnetic properties of monomeric Fe(BIP)3 were probed in solution by nuclear magnetic resonance recurring to the Evans bulk magnetization method. Results: The designed synthetic procedure successfully afforded Fe(BIP)3, which was fully characterized by UV-Vis and IR spectroscopy, as well as single-crystal X-ray diffraction. Aqueous solutions of Fe(BIP)3 spontaneously formed rice-grain-shaped nanoscale aggregates of hydrodynamic radius ≈ 30 nm. Incorporation of these aggregates into phospholipid vesicles enhanced their stability. The longitudinal r1 and transverse r2 relaxivities of Fe(BIP)3 aggregates were assessed to be 1.92 and 52.3 mM−1s−1, respectively, revealing their potential as paramagnetic relaxation agents. Conclusions: Fe(BIP)3 aggregates, stabilized through incorporation into phospholipid vesicles, demonstrate promising potential as novel paramagnetic relaxation agents in aqueous environments. Full article
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23 pages, 4386 KB  
Article
Could Insect Frass Be Used as a New Organic Fertilizer in Agriculture? Nutritional Composition, Nature of Organic Matter, Ecotoxicity, and Phytotoxicity of Insect Excrement Compared to Eisenia fetida Vermicompost
by Patricia Castillo, José Antonio Sáez-Tovar, Francisco Javier Andreu-Rodríguez, Héctor Estrada-Medina, Frutos Carlos Marhuenda-Egea, María Ángeles Bustamante, Anabel Martínez-Sánchez, Encarnación Martínez-Sabater, Luciano Orden, Pablo Barranco, María José López and Raúl Moral
Insects 2026, 17(2), 142; https://doi.org/10.3390/insects17020142 - 27 Jan 2026
Viewed by 80
Abstract
The expanding insect farming industry generates up to 67,000 tons of frass per year. Its potential use as fertilizer is promising, but has not yet been widely studied. This study aimed to characterize the chemical composition, organic matter structure, ecotoxicity, and phytotoxicity of [...] Read more.
The expanding insect farming industry generates up to 67,000 tons of frass per year. Its potential use as fertilizer is promising, but has not yet been widely studied. This study aimed to characterize the chemical composition, organic matter structure, ecotoxicity, and phytotoxicity of frass from four insect species in order to evaluate its potential as a fertilizer. We compared four types of insect frass (IF) (Tenebrio molitor, Galleria mellonella, Hermetia illucens, and Acheta domesticus) to Eisenia fetida vermicompost (EFV). We used physicochemical analyses (pH, electrical conductivity (EC), macro-micronutrients and dissolved organic carbon (DOC), spectroscopy (solid-state 13C nuclear magnetic resonance (NMR), and Fourier-transform infrared spectroscopy (FTIR)) and thermogravimetry/differential scanning calorimetry (TGA/DSC: R1, R2, Tmax), together with phytotoxicity (germination index, %GI) and ecotoxicity (toxicity units, TU) bioassays. Composition was species-dependent: A. domesticus showed the highest levels of nitrogen (N), phosphorus (P), and potassium (K); the concentration of DOC was higher in insect frass (IF) than in EFV, with the highest concentration found in IF of T. molitor. 13C NMR/FTIR profiles distinguished between frass (carbohydrates/proteins and chitin signals) and EFV (humified, oxidized matrix). Thermal stability followed: G. mellonella (R1 ≈ 0.88) ≥ A. domesticus (0.79) > H. illucens (0.73) > EFV (0.67) > T. molitor (0.50). In bioassays, T. molitor and A. domesticus exhibited phytotoxicity (%GI < 30), whereas G. mellonella and H. illucens did not. EFV exhibited the highest %GI. Dilution increased %GI in all materials, especially in T. molitor and A. domesticus, and reduced acute risk (TU). Frass is not a uniform input: its agronomic performance emerges from the interaction between EC (ionic stress), the availability of labile C (DOC, C/N and low-temperature exotherms), and structural stability (R1/R2 and aromaticity). In terms of formulation, IF can provide nutrients that mineralize rapidly, whereas EFV contributes stability. Controlling the inclusion and dilution of materials (e.g., limiting the amount of T. molitor in blends) and considering the mixing matrix helps to manage phytotoxicity and ecotoxicity, and realize the fertilizer value of the product. Full article
(This article belongs to the Section Role of Insects in Human Society)
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16 pages, 1700 KB  
Article
The Effects of Salicyluric Acid, the Main Metabolite of Aspirin, on Lipid Peroxidation Induced by Iron and Copper Ions in a Lipid Membrane Model
by Viktor A. Timoshnikov, Vladimir E. Koshman, Aleksandr A. Deriskiba, Nikolay E. Polyakov and George J. Kontoghiorghes
Int. J. Mol. Sci. 2026, 27(3), 1216; https://doi.org/10.3390/ijms27031216 - 26 Jan 2026
Viewed by 83
Abstract
Salicyluric acid (SUA), the main metabolite of aspirin and a natural product, is known for its ability to chelate iron and other metal ions. In particular, the chelation and increased excretion of iron by SUA may contribute to the aspirin-induced iron deficiency anemia [...] Read more.
Salicyluric acid (SUA), the main metabolite of aspirin and a natural product, is known for its ability to chelate iron and other metal ions. In particular, the chelation and increased excretion of iron by SUA may contribute to the aspirin-induced iron deficiency anemia observed in long-term aspirin users. The redox activity of iron and copper complexes of drugs and also drug metabolites, such as SUA, is an important parameter of their overall toxicity profile, including the induction of ferroptosis, which has been associated with many diseases. In this context, the effect of SUA on iron- and copper-induced lipid peroxidation and also its localization within a model lipid membrane have been investigated. A combination of physicochemical methods, including Nuclear Magnetic Resonance (1H NMR), molecular dynamics (MD), and Nuclear Overhauser Effect Spectroscopy (1H NOESY), has been used to demonstrate that SUA does not promote the peroxidation of linoleic acid micelles in the presence of Fe(II) or Cu(II) ions. NMR experiments revealed that SUA incorporates into the lipid bilayer, which stabilizes the ligands and inhibits its metal chelation ability in comparison to the control. NOESY experiments and MD simulations further showed that SUA localizes shallowly within the membrane, interacting primarily with the head group and upper acyl chain regions of lipids. These findings provide crucial insights into the membrane redox reactivity and other behavior of SUA, explaining its lack of pro-oxidant activity and also highlighting its complex role in the pharmacological and toxicological effects on iron metabolism in long-term aspirin users. Full article
(This article belongs to the Section Bioactives and Nutraceuticals)
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20 pages, 7768 KB  
Article
The Evolution Law of Molecular Structure of Vitrain and Durain During Low–Medium Coalification
by Yue Chen, Zan Liu, Huaichang Wang, Changjiang Ji, Liya Wang, Pengpeng Guan, Peilin Wang, Kai Ma and Liyuan Dang
Processes 2026, 14(3), 401; https://doi.org/10.3390/pr14030401 - 23 Jan 2026
Viewed by 139
Abstract
Molecular structural disparities between maceral components are intrinsic factors governing their reactivity and physicochemical behaviors during storage and transportation. To investigate the molecular structural differentiation between vitrain and durain in low- to medium-rank coals (Ro,max = 0.65–1.71%), this study selected samples [...] Read more.
Molecular structural disparities between maceral components are intrinsic factors governing their reactivity and physicochemical behaviors during storage and transportation. To investigate the molecular structural differentiation between vitrain and durain in low- to medium-rank coals (Ro,max = 0.65–1.71%), this study selected samples of long-flame coal and gas coal from the Huanglong Coalfield, coking coal from the Hedong Coalfield, and fat coal from the Weibei Coalfield. The microstructural variations in macroscopic coal components during coalification were analyzed using Fourier transform infrared spectroscopy (FTIR), 13C nuclear magnetic resonance (13C-NMR), and X-ray photoelectron spectroscopy (XPS). The results indicated that the aromatic structures of vitrain are predominantly trisubstituted, with their proportion consistently exceeding that in durain. In contrast, durain exhibits a progressive transition from trisubstituted to pentasubstituted aromatics with increasing coal rank, accompanied by higher aromaticity, condensation degree, and aromatic carbon content. The d002 size of the vitrain decreased from 3.82 to 3.47, while that of the durain decreased from 3.52 to 3.40. Both values showed a gradual decline, with the vitrain exhibiting a larger reduction than the durain. This indicates that the lateral extension of the microcrystalline structure in the durain is more developed, resulting in tighter molecular connections. 13C-NMR analysis further reveals that durain possesses higher falH/fal* and bridge carbon ratios (XBP), along with a lower faS/fa ratio, reflecting a greater degree of aromatic ring condensation. XPS analysis revealed that durain generally contains a higher oxygen-functional group content but lower C-C/C-H content compared to vitrain. Collectively, these findings confirm significant structural divergence between vitrain and durain during coalification, with durain exhibiting more developed aromaticity, structural condensation, and organizational order. Full article
(This article belongs to the Special Issue Phase Behavior Modeling in Unconventional Resources)
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24 pages, 6227 KB  
Article
Gadolinium-Doped Hydroxyapatite Nanoparticles Functionalized with Curcumin and Folic Acid: Structural Insights and Magnetic Behavior for Theranostic Applications
by Jéssica P. N. Marinho, Luísa A. F. Vieira, André F. Oliveira, Aloísio M. Garcia, Monica E. B. Guarin, João Batista S. Barbosa, Yan F. X. Ladeira, Adolfo H. M. Silva and Edésia M. B. de Sousa
Materials 2026, 19(3), 449; https://doi.org/10.3390/ma19030449 - 23 Jan 2026
Viewed by 136
Abstract
Gadolinium-doped hydroxyapatite nanoparticles (HapGd NPs) have emerged as promising multifunctional platforms for biomedical applications due to their unique combination of biocompatibility, structural tunability, and magnetic responsiveness. In this work, HapGd nanoparticles were synthesized using a microwave-assisted method and subsequently functionalized with curcumin and [...] Read more.
Gadolinium-doped hydroxyapatite nanoparticles (HapGd NPs) have emerged as promising multifunctional platforms for biomedical applications due to their unique combination of biocompatibility, structural tunability, and magnetic responsiveness. In this work, HapGd nanoparticles were synthesized using a microwave-assisted method and subsequently functionalized with curcumin and folic acid to enhance therapeutic efficiency and selective targeting. The synthesized nanostructures were characterized using various techniques, including X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometry (VSM), and relaxometry. Structural analyses revealed successful incorporation of Gd3+ ions into the Hap lattice, resulting in reduced unit cell volume and slight lattice distortion, while preserving the apatite crystalline framework. Surface functionalization with curcumin and folic acid was confirmed through spectroscopic characterization, demonstrating effective molecular attachment. Nuclear Magnetic Resonance (NMR) relaxation measurements indicated that Gd doping endowed paramagnetic behavior suitable for contrast enhancement in magnetic resonance imaging (MRI). Relaxometry studies revealed a strong linear correlation between 1/T1 and the Gd3+ concentration, especially in the functionalized samples, with performance comparable to the commercial contrast agent Omniscan™. The developed HapGd-based nanoplatform exhibits integrated diagnostic and therapeutic potential, providing a foundation for future research in biomedical applications. Full article
(This article belongs to the Special Issue Materials for Drug Delivery and Medical Engineering)
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24 pages, 1003 KB  
Review
Diagnostic Potential of Metabolomic and Proteomic Biomarkers in Cardiology—A Narrative Review
by Lazzat Zhussupbekova, Dinara Nurkina, Gyulnar Zhussupova, Aliya Smagulova, Venera Rakhmetova, Elmira Akhmedyarova, Aisha Darybayeva, Klara Kurmangaliyeva and Ilya Kukes
Biomedicines 2026, 14(2), 257; https://doi.org/10.3390/biomedicines14020257 - 23 Jan 2026
Viewed by 360
Abstract
Cardiovascular disease is a major cause of death worldwide and a global socio-economic problem. To date, there are numerous studies focused on finding new biomarkers of cardiovascular diseases. High-technological methods such as mass spectrometry (MS), high-performance liquid chromatography (HPLC), and nuclear magnetic resonance [...] Read more.
Cardiovascular disease is a major cause of death worldwide and a global socio-economic problem. To date, there are numerous studies focused on finding new biomarkers of cardiovascular diseases. High-technological methods such as mass spectrometry (MS), high-performance liquid chromatography (HPLC), and nuclear magnetic resonance (NMR) spectroscopy enable us to record thousands of metabolites of organs and tissues. Studying organisms at a molecular level contributes to an in-depth understanding of preclinical conditions of various diseases. Metabolomics reflects the dynamics of metabolism distribution, including environmental influences, allowing us to create a metabolic profile of the patient. The aim of this review was to analyze current data on metabolomic and proteomic biomarkers in the diagnosis of cardiovascular diseases. The search databases were used to select studies on the potential clinical and diagnostic application of proteomic and metabolomic markers in cardiology. The selected sources were subjected to qualitative and thematic analysis. All biomarkers were grouped according to the pathophysiological process (inflammation, blood coagulation and lipid metabolism disorders, myocardial necrosis, etc.). The association of changes in metabolomic and proteomic profiles with the activation of pathogenic processes in the cardiovascular system was demonstrated. The use of these multivariate markers, individually or in combination, will increase the accuracy of early diagnosis and the effectiveness of treatment. This article also highlights the limitations of the method and possible ways to solve them. Full article
(This article belongs to the Section Endocrinology and Metabolism Research)
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25 pages, 2766 KB  
Article
Design and Optimization of Pullulan-Isononanoate Films with Bioactive-Loaded Liposomes for Potential Biomedical Use
by Amjed A. Karkad, Aleksandar Marinković, Aleksandra Jovanović, Katarina Simić, Stefan Ivanović, Milena Milošević and Tamara Erceg
Polymers 2026, 18(2), 305; https://doi.org/10.3390/polym18020305 - 22 Jan 2026
Viewed by 160
Abstract
This study reports the synthesis and detailed characterization of pullulan-isononanoate (Pull-Iso), as well as the preparation and characterization of Pull-Iso films incorporating liposomes loaded with silibinin (SB) and smoke tree (Cotinus coggygria) extract (STExt), to explore the physicochemical and functional properties [...] Read more.
This study reports the synthesis and detailed characterization of pullulan-isononanoate (Pull-Iso), as well as the preparation and characterization of Pull-Iso films incorporating liposomes loaded with silibinin (SB) and smoke tree (Cotinus coggygria) extract (STExt), to explore the physicochemical and functional properties of pullulan-based biomaterials for potential biomedical applications. Pullulan was successfully esterified with isononanoic acid chloride, as confirmed by 1H and 13C NMR (Nuclear Magnetic Resonance) and Fourier Transform Infrared (FTIR) spectroscopy. Modification significantly reduced the glass transition temperature (Tg), indicating enhanced chain mobility due to the introduction of bulky side chains. Prepared liposomes, embedding SB and extracted smoke tree compounds, exhibited particle sizes ~2000 nm with moderate polydispersity (~0.340) and zeta potential values around –20 mV, demonstrating lower colloidal stability over 60 days, thereby justifying their encapsulation within films. Optical microscopy revealed uniform liposome dispersion in Pull-Iso film with 0.5 g of liposomes, while higher liposome loading (0.75 g of liposomes) induced aggregation and microstructural irregularities. Mechanical analysis showed a reduction in tensile strength and strain at higher liposome content. The incorporation of liposomes encapsulating STExt and SB significantly enhanced the antioxidant activity of Pull-Iso-based films in a concentration-dependent manner, as demonstrated by DPPH and ABTS radical scavenging assays. These preliminary findings suggest that pullulan esterification and controlled liposome incorporation may enable the development of flexible, bioactive-loaded films, which could represent a promising platform for advanced wound dressing applications, warranting further investigation. Full article
(This article belongs to the Special Issue Biomedical Applications of Polymeric Materials, 3rd Edition)
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20 pages, 3818 KB  
Article
Mechanistic Shifts in Organic Carbon Stabilization in a Black Soil Driven by Nitrogen Fertilization
by Yantian Cui, Qi Li, Hongyan Chang, Yanan Li, Chengyu Wang, Rong Jiang, Shuxia Liu and Wentian He
Agronomy 2026, 16(2), 268; https://doi.org/10.3390/agronomy16020268 - 22 Jan 2026
Viewed by 50
Abstract
The phaeozem in Northeast China is rich in soil organic carbon (SOC). However, the excessive and inefficient application of chemical fertilizers, particularly nitrogen fertilizers, has primarily led to a decrease in soil pH in this region. Currently, the relationship between soil pH and [...] Read more.
The phaeozem in Northeast China is rich in soil organic carbon (SOC). However, the excessive and inefficient application of chemical fertilizers, particularly nitrogen fertilizers, has primarily led to a decrease in soil pH in this region. Currently, the relationship between soil pH and the stability of soil organic carbon (SOC) remains ambiguous. This study, conducted over 13 years of field experiments, focused on soils exhibiting varying degrees of pH resulting from different nitrogen application rates. The research employed aggregate classification, 13C nuclear magnetic resonance spectroscopy, and analysis of microbial community composition to investigate the alterations in the SOC stabilization mechanisms under varying nitrogen application levels. Our results demonstrated that the decline in soil pH led to reductions in macroaggregates (>2 mm) and the soil aggregate destruction rate (PAD) by 4.8–14.6%, and in soil aggregate unstable agglomerate index (ELT) by 9.7–13.4%. The mean weight diameter (MWD) and geometric mean diameter (GMD) exhibited significant declines (p < 0.05) with decreasing pH levels. According to the 13C NMR analysis, the SOC was predominantly composed of O-alkyl carbon and aromatic carbon. At a pH of 5.32, the Alip/Arom values decreased, while the molecular structure of SOC became more complex under different levels of pH. In addition, the increase in [Fe(Al)-OC] (31.4–71.9%) complex indicates a shift in the stability of organic carbon from physical protection to organic mineral binding. Declining soil pH significantly reduced the diversity of soil microbial communities and promoted a shift toward copiotrophic microbial groups. Overall, declining soil pH resulted in a decline in soil aggregate stability and an increase in SOC aromaticity. This drove the shift in the stabilization mechanism of SOC in the black soil ecosystem of meadows in Northeast China from physical protection to chemical stability. Full article
(This article belongs to the Section Soil and Plant Nutrition)
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31 pages, 6046 KB  
Article
Geopolymerization of Untreated Dredged Sediments for Sustainable Binder Development
by Lisa Monteiro, Humberto Yáñez-Godoy, Nadia Saiyouri and Jacqueline Saliba
Materials 2026, 19(2), 433; https://doi.org/10.3390/ma19020433 - 22 Jan 2026
Viewed by 84
Abstract
The valorization of dredged sediments represents a major environmental and logistical challenge, particularly in the context of forthcoming regulations restricting their marine disposal. This study investigates the potential of untreated dredged sediments as sustainable raw materials for geopolymer binder development, with the dual [...] Read more.
The valorization of dredged sediments represents a major environmental and logistical challenge, particularly in the context of forthcoming regulations restricting their marine disposal. This study investigates the potential of untreated dredged sediments as sustainable raw materials for geopolymer binder development, with the dual objective of sustainable sediment management and reduction in cement-related environmental impact. Dredged sediments from the Grand Port Maritime de Bordeaux (GPMB) were activated with sodium hydroxide (NaOH) and sodium silicate (Na2SiO3), both alone and in combination, with supplementary aluminosilicate and calcium-rich co-products, to assess their reactivity and effect on binder performance. A multi-scale experimental approach combining mechanical testing, calorimetry, porosity analysis, Scanning Electron Microscopy and Energy-Dispersive Spectroscopy (SEM–EDS), X-ray diffraction (XRD), Thermogravimetric Analysis (TGA), and solid-state Nuclear Magnetic Resonance (NMR) was employed to challenge the commonly assumed inert behavior of sediments within geopolymer matrices, to elucidate gel formation mechanisms, and to optimize binder formulation. The results show that untreated sediments actively participate in alkali activation, reaching compressive strengths of up to 5.16 MPa at 90 days without thermal pre-treatment. Calcium-poor systems exhibited progressive long-term strength development associated with the formation of homogeneous aluminosilicate gels and refined microporosity, whereas calcium-rich systems showed higher early age strength but more limited long-term performance, linked to heterogeneous gel coexistence and increased total porosity. These findings provide direct evidence of the intrinsic reactivity of untreated dredged sediments and highlight the critical role of gel chemistry and calcium content in controlling long-term performance. The proposed approach offers a viable pathway for low-impact, on-site sediment valorization in civil engineering applications. Full article
(This article belongs to the Special Issue Advances in Natural Building and Construction Materials (2nd Edition))
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20 pages, 10017 KB  
Article
Calcium-Modified Coal-Based Humin Waste Residue: Enhanced Cadmium Remediation in Combined Soil–Plant Systems
by Fei Wang, Nan Guo, Yuxin Ma, Zhi Yuan, Xiaofang Qin, Yun Jia, Guixi Chen, Haokai Yu, Ping Wang and Zhanyong Fu
Sustainability 2026, 18(2), 1103; https://doi.org/10.3390/su18021103 - 21 Jan 2026
Viewed by 104
Abstract
Coal-based humic acid waste residue is a solid waste generated during the production of humic acid products. The extraction of coal-based humin (NHM) from such residues presents an effective approach for solid waste resource recovery. In this study, a novel calcium-based humin (Ca-NHM) [...] Read more.
Coal-based humic acid waste residue is a solid waste generated during the production of humic acid products. The extraction of coal-based humin (NHM) from such residues presents an effective approach for solid waste resource recovery. In this study, a novel calcium-based humin (Ca-NHM) was synthesized via a low-temperature-assisted method. The material was characterized and its cadmium passivation mechanism was investigated using scanning electron microscopy (SEM), zeta potential analysis (Zeta), carbon nuclear magnetic resonance (13C-CPMAS-NMR), and X-ray photoelectron spectroscopy (XPS). Soil incubation experiments were conducted to determine the actual cadmium adsorption capacity of coal-based humin in soils and to evaluate the stability of cadmium passivation. Plant cultivation experiments were carried out to verify the effects of coal-based humin on migration and transformation in soil, as well as on cadmium bioefficiency. The results showed that Ca-NHM passivated soil cadmium through multiple mechanisms such as ion exchange, electrostatic adsorption, complexation reactions, and physical adsorption. Compared with NHM, Ca-NHM exhibited a 69.71% increase in passivation efficiency, and a 2.44% reduction in cadmium leaching concentration. In Ca-NHM treatments, the above- and below-ground biomass of pakchoi increased by 18.06%, and 80.95%, respectively, relative to the control group. Furthermore, Ca-NHM enhanced the cadmium resistance of pakchoi, reduced the enrichment coefficient, activity coefficient, and activity-to-stability ratio in the above-ground portion of pakchoi, and maintained a transfer coefficient below 1, thereby alleviating cadmium toxicity. In summary, this study provides a theoretical foundation for understanding the mechanisms by which coal-based humin mitigates cadmium toxicity in pakchoi. Full article
(This article belongs to the Special Issue Sustainable Risk Assessment and Remediation of Soil Pollution)
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20 pages, 2026 KB  
Article
Temporal Urinary Metabolomic Profiling in ICU Patients with Critical COVID-19: A Pilot Study Providing Insights into Prognostic Biomarkers via 1H-NMR Spectroscopy
by Emir Matpan, Ahmet Tarik Baykal, Lütfi Telci, Türker Kundak and Mustafa Serteser
Curr. Issues Mol. Biol. 2026, 48(1), 112; https://doi.org/10.3390/cimb48010112 - 21 Jan 2026
Viewed by 123
Abstract
Although the impact of COVID-19, caused by SARS-CoV-2, may appear to have diminished in recent years, the emergence of new variants still continues to cause significant global health and economic challenges. While numerous metabolomic studies have explored serum-based alterations linked to the infection, [...] Read more.
Although the impact of COVID-19, caused by SARS-CoV-2, may appear to have diminished in recent years, the emergence of new variants still continues to cause significant global health and economic challenges. While numerous metabolomic studies have explored serum-based alterations linked to the infection, investigations utilizing urine as a biological matrix remain notably limited. This gap is especially significant given the potential advantages of urine, a non-invasive and easily obtainable biofluid, in clinical settings. In the context of patients in intensive care units (ICUs), temporal monitoring through such non-invasive samples may offer a practical and effective approach for tracking disease progression and tailoring therapeutic interventions. This study retrospectively explored the longitudinal metabolomic alterations in COVID-19 patients admitted to the ICU, stratified into three prognostic outcome groups: healthy discharged (HD), polyneuropathic syndrome (PS), and Exitus. A total of 32 urine samples, collected at four distinct time points per patient during April 2020 and preserved at −80 °C, were analyzed by proton nuclear magnetic resonance (1H-NMR) spectroscopy for comprehensive metabolic profiling. Statistical evaluation using two-way ANOVA and ANOVA–Simultaneous Component Analysis (ASCA) identified significant prognostic variations (p < 0.05) in the levels of taurine, 3-hydroxyvaleric acid and formic acid. Complementary supervised classification via random forest modeling yielded moderate predictive performance with out-of-bag error rate of 40.6% based on prognostic categories. Particularly, taurine, 3-hydroxyvaleric acid and formic acid levels were highest in the PS group. However, no significant temporal changes were observed for any metabolite in analyses. Additionally, metabolic pathway analysis conducted using the Kyoto Encyclopedia of Genes and Genomes (KEGG) database highlighted the “taurine and hypotaurine metabolism” pathway as the most significantly affected (p < 0.05) across prognostic classifications. Harnessing urinary metabolomics, as indicated in our preliminary study, could offer valuable insights into the dynamic metabolic responses of ICU patients, thereby facilitating more personalized and responsive critical care strategies in COVID-19 patients. Full article
(This article belongs to the Section Biochemistry, Molecular and Cellular Biology)
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32 pages, 2940 KB  
Article
Integrated In Vitro and In Silico Profiling of Piperazinyl Thiosemicarbazone Derivatives Against Trypanosoma cruzi: Stage-Specific Activity and Enzyme Inhibition
by Héctor A. Baldoni, María L. Sbaraglini, Darío E. Balcazar, Diego G. Arias, Sergio A. Guerrero, Catalina D. Alba Soto, Wioleta Cieslik, Marta Rogalska, Jaroslaw Polański, Ricardo D. Enriz, Josef Jampilek and Robert Musiol
Pharmaceuticals 2026, 19(1), 182; https://doi.org/10.3390/ph19010182 - 20 Jan 2026
Viewed by 279
Abstract
Background: Trypanosoma cruzi, the causative agent of Chagas disease, remains a major public health concern, and there is a continued need for new antitrypanosomal agents. Thiosemicarbazone (TSC) derivatives have emerged as a promising class of compounds with potential antiparasitic activity. Objectives: [...] Read more.
Background: Trypanosoma cruzi, the causative agent of Chagas disease, remains a major public health concern, and there is a continued need for new antitrypanosomal agents. Thiosemicarbazone (TSC) derivatives have emerged as a promising class of compounds with potential antiparasitic activity. Objectives: This study aimed to report the synthesis, characterization, and biological profiling of a novel series of thiosemicarbazone derivatives as antitrypanosomal agents against Trypanosoma cruzi. Methods: Fourteen new compounds and six previously described analogues were prepared and characterized by 1H/13C nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry (MS). As a preliminary in vitro screen, activity was assessed by direct parasite counting in epimastigote and bloodstream trypomastigote forms, as tractable models of replicative and infective stages sharing core metabolic targets with intracellular amastigotes. Epimastigote potency was quantified as half-maximal effective concentrations (EC50) derived from dose–response curves, whereas trypomastigote response was evaluated as percent viability after treatment at a fixed concentration of 20 µM. Mechanistic profiling included inhibition assays against the cysteine protease cruzipain (CZP) and selected redox defense enzymes, complemented by in silico similarity clustering and binding-pose affinity scoring. Results: A nitro-methoxy-substituted TSC showed potent CZP inhibition but limited trypomastigote efficacy, whereas brominated analogues displayed dual-stage activity independent of CZP inhibition. Tanimoto similarity analysis identified distinct structure–activity clusters, linking nitro-methoxy substitution to epimastigote selectivity and brominated scaffolds to broader antiparasitic profiles, with hydrophobicity and steric complementarity as key determinants. Enzymatic assays revealed no significant inhibition of cytosolic tryparedoxin peroxidase (cTXNPx) or glutathione peroxidase type I (TcGPx-I), suggesting redox disruption is not a primary mode of action. In vitro and in silico analyses showed low or no non-specific cytotoxicity under the tested conditions, supporting further optimization of these derivatives as antitrypanosomal preliminary hits. Key hits included derivative 3e (epimastigote EC50 = 0.36 ± 0.02 µM) and brominated analogues 2c and 2e (epimastigote EC50 = 3.92 ± 0.13 and 4.36 ± 0.10 µM, respectively), while docking supported favorable binding-pose affinity (e.g., ΔGS-pose = −20.78 ± 2.47 kcal/mol for 3e). Conclusions: These results support further optimization of the identified thiosemicarbazone derivatives as preliminary antitrypanosomal hits and provide insight into structure–activity relationships and potential mechanisms of action. Full article
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19 pages, 13234 KB  
Article
Cracking-Resistance Mechanism of Fiber-Reinforced Coal-Based Solid-Waste Grouting Materials
by Shuai Guo, Weifeng Liang, Xiangru Wu, Chenyang Li, Hongzeng Li, Yahui Liu, Shenyang Ouyang, Yachao Guo and Junmeng Li
Materials 2026, 19(2), 389; https://doi.org/10.3390/ma19020389 - 18 Jan 2026
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Abstract
Grouting technology can be employed to repair cracks in an aquifer to maintain its stability; however, existing grouting materials tend to come with problems such as low flexural strength, poor cracking resistance, and the coupled effects of fiber reinforcement and sulfoaluminate cement (SAC) [...] Read more.
Grouting technology can be employed to repair cracks in an aquifer to maintain its stability; however, existing grouting materials tend to come with problems such as low flexural strength, poor cracking resistance, and the coupled effects of fiber reinforcement and sulfoaluminate cement (SAC) addition on hydrate evolution, and pore-refinement and crack-resistance mechanisms in coal-based solid-waste cementitious grouts remain insufficiently understood. In this paper, fiber-modified coal-based solid-waste grouting (F-CWG) materials were prepared by mixing different contents of sulfoaluminate cement (SAC) and different fibers. The mechanical strength, microstructure, hydration products, and pore evolution characteristics were analyzed by means of mechanical property tests, energy-dispersive X-ray spectroscopy (SEM/EDS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and nuclear magnetic resonance (NMR). The results show that the mechanical strength decreases at first due to insufficient early-stage hydration products. Specifically, the 28 d compressive and flexural strengths decrease from 15.34 MPa and 4.55 MPa at 0% SAC to 8.18 MPa and 2.99 MPa at 40% SAC but increase again to 13.36 MPa and 3.79 MPa at 60% SAC as the formation of ettringite (AFt) and C–S–H is promoted with higher SAC content. Among the tested fibers, a dosage of 0.6% generally improves mechanical strength and refines pore structure, with PVA and steel fibers showing the most pronounced effects. Our results reveal the mechanism behind the enhancement of cracking resistance in F-CWG materials, providing a scientific basis for grouting and water-preservation mining, and are of great significance in improving the utilization rate of coal-based solid waste. Full article
(This article belongs to the Special Issue Low-Carbon Cementitious Composites)
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22 pages, 867 KB  
Article
A Major Update and Improved Validation Functionality in the mwtab Python Library and the Metabolomics Workbench File Status Website
by P. Travis Thompson and Hunter N. B. Moseley
Metabolites 2026, 16(1), 76; https://doi.org/10.3390/metabo16010076 - 15 Jan 2026
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Abstract
Background: The Metabolomics Workbench (MW) is a public scientific data repository consisting of experimental data and metadata from metabolomics studies collected with mass spectroscopy (MS) and nuclear magnetic resonance (NMR) analyses. Although not as rapidly as in the past, MW has steadily evolved, [...] Read more.
Background: The Metabolomics Workbench (MW) is a public scientific data repository consisting of experimental data and metadata from metabolomics studies collected with mass spectroscopy (MS) and nuclear magnetic resonance (NMR) analyses. Although not as rapidly as in the past, MW has steadily evolved, updating its mwTab and JSON deposition text file formats and its web-based infrastructure. However, the growth of MW has been exponential since its inception in 2013 and continues to be exponential, with the number of datasets hosted on the repository increasing by 50% since April 2024. As part of regular maintenance to keep up with changes to the mwTab file format and an earnest effort to use MW datasets in meta-analyses, the mwtab Python package has been updated. Methods: Updates include better error handling for batch processing, better parsing to read more files without error, and extensive improvements to the validation capabilities of the package. These updates also required our mwFileStatusWebsite to be updated and improved. Results: We used the enhanced validation features of the mwtab package to evaluate all available datasets in MW to facilitate improved curation, FAIRness of the repository, and reuse for meta-analyses. Conclusions: Version 2.0.0 of the mwtab Python package is now officially released and freely available on GitHub and the Python Package Index (PyPI) under a Clear Berkeley Software Distribution (BSD) license, with documentation available on GitHub. The updated mwFileStatusWebsite is also officially in its 2.0.0 version. Full article
(This article belongs to the Section Bioinformatics and Data Analysis)
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19 pages, 4774 KB  
Article
Valorization of Orange Peels for Pectin Extraction from BARI Malta-1 (Sweet Orange): A Green Approach for Sustainable Utilization of Citrus Waste
by M. A. A. Shofi Uddin Sarkar, Md Murshed Bhuyan and Sharmeen Nishat
Polysaccharides 2026, 7(1), 8; https://doi.org/10.3390/polysaccharides7010008 - 12 Jan 2026
Viewed by 206
Abstract
The agro-industrial valorization of citrus waste represents a promising avenue to employ underutilized bioresources. This research investigated the potential of the peels of BARI malta 1 (sweet orange), a widely grown variety in Bangladesh, as a viable and new source for pectin extraction. [...] Read more.
The agro-industrial valorization of citrus waste represents a promising avenue to employ underutilized bioresources. This research investigated the potential of the peels of BARI malta 1 (sweet orange), a widely grown variety in Bangladesh, as a viable and new source for pectin extraction. Pectin is a polysaccharide, having extensive applications in the pharmaceuticals, cosmetics, and food business as a thickening, texturizer, emulsifier, gelling agent, and stabilizer. This study investigated the optimum extraction conditions for maximum yield, characterization, and physicochemical properties of the obtained pectin and compared the results with the pectin obtained from other sources. Comprehensive characterization through Fourier-Transform Infrared Spectroscopy (FTIR), Nuclear Magnetic Resonance (NMR) spectroscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), Differential Scanning Calorimetry (DSC), and Field Emission Scanning Electron Microscopy (FESEM) confirmed the structural identity, crystallinity, thermal stability, and morphological features of the extracted pectin. Physicochemical properties, including moisture content, ash content, equivalent weight, methoxyl content, and degree of esterification, indicate the suitability and superiority of the extracted pectin for industrial applications. This research approach not only supports eco-friendly processing of citrus waste but also opens avenue for circular economy initiatives in Bangladesh. Full article
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