Search Results (150)

Sustainable food production systems based on the use of biofertilizers and soil improvers are proposed to mitigate agricultural-related environmental impacts and address the climate crisis. In particular, plant growth-promoting microbes (PGPM) and biochar (Char) have been reported to improve plant growth, soil quality, and crop yield; however, their effects on food quality remain debated. In this study, untargeted metabolomics based on ultra-high performance liquid chromatography–ion mobility–high-resolution mass spectrometry (UHPLC-IMS-HRMS) and proton nuclear magnetic resonance spectroscopy (¹H-NMR) are proposed to achieve a comprehensive investigation of the effects of Char, PGPM and Char+PGPM on durum wheat. A total of 88 metabolites were annotated by UHPLC-IMS-HRMS, mainly belonging to carbohydrates, flavones, flavonoids, glycerophospholipids, and glycolipids, while 30 compounds were annotated by ¹H-NMR, mostly amino acids and short-chain carboxylic acids. The two datasets were merged with the gluten protein content dataset by using low- and mid-level data fusion approaches, obtaining models that exhibit excellent classification performance. Integrated analysis highlighted that the combined Char+PGPM treatment induced metabolic changes across multiple chemical classes, including enrichment of flavonoids and lipids, and downregulation of carbohydrate metabolites, suggesting a redistribution of carbon resources and modulation of secondary metabolism with potential implications on wheat grain quality. Full article

Antimicrobial resistance (AMR) remains a major threat to modern medicine, fueled by the excessive use of antibiotics and the spread of multidrug-resistant pathogens such as methicillin-resistant Staphylococcus aureus (MRSA). In this study, we designed and synthesized a series of 2-aryl-4-aminoquinazoline derivatives bearing an aminoalkylimidazole linker, combining two pharmacophoric motifs associated with antimicrobial activity. Starting from anthranilamide, the compounds were prepared in three straightforward steps, affording good yields and high purity. Their structures were confirmed by FT-IR spectroscopy, ¹H and ¹³C nuclear magnetic resonance (NMR), and high-resolution mass spectrometry (HRMS). Biological evaluation showed that series 5 exhibited strong selectivity toward S. aureus, with compounds 5c and 5d displaying minimum inhibitory concentrations (MICs) between 2.2 and 4.4 µM. No significant activity was observed against other tested strains. Cytotoxicity assays in HepG2 cells revealed moderate to low inhibition. Molecular docking indicated preferential binding to dihydrofolate reductase (DHFR) and relevant interactions with topoisomerase IV, resembling reference inhibitors. ADME analysis predicted favourable absorption, blood–brain barrier permeability, and compliance with Lipinski’s rules. Full article

Epilepsy remains one of the most prevalent neurological disorders, characterised by complex aetiology encompassing genetic, structural, metabolic, and inflammatory factors. Despite advances in neuroimaging and neurophysiological diagnostics, there is a persistent lack of sensitive and specific biomarkers to enable early diagnosis, risk stratification, and monitoring of therapeutic efficacy. Key epilepsy biomarkers include neurotransmitters, energy–related compounds, tryptophan pathway metabolites, and choline derivatives. Their determination employs liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS), high–performance liquid chromatography (HPLC) with electrochemical or fluorescence detection, gas chromatography with tandem mass spectrometry (GC–MS/MS), high–resolution mass spectrometry (HRMS), and proton nuclear magnetic resonance (¹H–NMR) spectroscopy, revealing metabolic disturbances in neurotransmission, energy metabolism, and oxidative stress associated with epileptogenesis. Among these techniques, LC–MS/MS currently provides the highest analytical sensitivity and specificity for quantifying low–abundance epilepsy–related metabolites, while HPLC with conventional detection remains a simpler and more cost–effective alternative for routine clinical laboratories. This review presents the current state of knowledge regarding chromatographic techniques applied to the analysis of mentioned metabolites, as well as therapeutic drug monitoring of antiepileptic drugs. Key sample preparation stages are also discussed. Various biological matrices–plasma, serum, urine, cerebrospinal fluid (CSF), dried blood spots (DBSs), and brain tissue—are evaluated. Novel approaches are also presented, including hair samples, microsampling techniques, and headspace analysis of volatile metabolites. Chromatographic techniques constitute the foundation of contemporary metabolomic research in epileptology, enabling biomarker identification and supporting personalised medicine. Further standardisation and translational validation remain necessary, as current evidence is insufficient for routine clinical implementation. Full article

Background/Objectives: Imatinib, the first tyrosine kinase inhibitor, marks the beginning of a revolution in clinical oncology. Disrupting oncogenic kinase-dependent signaling pathways represents a key strategy for advancing targeted cancer therapies. Terpene analogues of imatinib were developed to probe the influence of terminal ring modifications on BCR-ABL inhibition and downstream oncogenic signaling. Methods: Nine novel imatinib analogues bearing bulky aliphatic moieties were designed, synthesised, and structurally characterized by ¹H/¹³C NMR spectroscopy and high-resolution mass spectrometry (HRMS). Molecular docking calculations were performed to assess the binding modes and intermolecular interactions. The cytotoxicity of the newly synthesized imatinib derivatives was evaluated across a panel of BCR-ABL+ leukemia cell lines. Results: Molecular docking analyses demonstrated conserved interactions within the ATP-binding site of BCR-ABL for all derivatives, with calculated docking scores ranging between 123 and 128, while modifications at the terminal ring introduced subtle changes in electrostatic and steric profiles. Biological evaluation using MTT-based cytotoxicity assays in BCR-ABL+ leukemic cell lines revealed enhanced antiproliferative activity compared with imatinib, with compounds 6a (flexible cyclohexyl) and 6d (rigid camphane-type (+)-isopinocampheyl) exhibiting the lowest micromolar activity in the AR-230 model (IC₅₀ values of 1.1 and 1.2 μM, respectively). Proteome-wide phosphokinase profiling demonstrated shared suppression of STAT5/3/6, RSK1/2, S6K1/p70, and Pyk2, confirming effective disruption of canonical BCR-ABL pathways. Critically, the terpene moiety dictated downstream pathway bias: 6a preferentially attenuated CREB activation, whereas 6d more effectively suppressed the PI3K/Akt oncogenic axis and strongly activated proapoptotic p53-mediated stress responses. Conclusions: Our findings establish terpene-engineered imatinib analogues as tunable modulators and promising candidates for targeting downstream BCR-ABL signaling pathways in leukemia treatment. Full article

Three painted valuable wood sculptures from conventual collections in Apulia (Southern Italy), made between the beginning of the 17th century and the first half of the 18th century, were studied to shed light on the pictorial materials and techniques of the Neapolitan Baroque sculpture in Southern Italy. A multi-analytical approach was implemented using integrated micro-invasive techniques, including polarized light microscopy (PLM) in ultraviolet (UV) and visible (VIS) light, scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS), Fourier-Transform Infrared (FTIR) spectroscopy, and pyrolysis–gas chromatography/high-resolution mass spectrometry (Py-GC/HRMS). The stratigraphic sequences were microscopically identified, and the pictorial layers were discriminated on the basis of optical features, elemental compositions, and mapping. Organic components were detected by FTIR as lipids and proteinaceous compounds for binders, while terpenic resins were detected as varnishes. Accordingly, PY-GC/HRMS identified siccative oils, animal glue, egg, and colophony. The results allowed the identification of the painting techniques used for the pictorial films and the ground preparation layers and supported the distinction between original and repainting layers. The results of this multi-analytical approach provide insights into Baroque wooden sculpture in Southern Italy and offers information to support restorers in conservation works. Full article

China is the world’s largest producer of acrylic fiber, and the wastewater generated from its production contains a significant amount of biologically refractory organic pollutants. However, comprehensive screening studies on organic compounds in such wastewater remain limited, which hampers effective wastewater treatment and ecological risk management to some extent. In this study, high-resolution mass spectrometry (HRMS) was combined with comprehensive two-dimensional gas chromatography (GC×GC) and ultra-performance liquid chromatography, along with multiple characterization techniques—including proton nuclear magnetic resonance spectroscopy, infrared spectroscopy, and fluorescence spectroscopy—to qualitatively analyze organic compounds present in wastewater from four stages of wet-spun acrylic fiber production: acrylonitrile mixed wastewater, polymerization wastewater, spinning wastewater, and final mixed wastewater. The results indicated that sulfonate esters, various other esters, alkanes, heterocyclic compounds, aromatic compounds, and substances containing multiple conjugated systems were commonly present across all four sample types, potentially contributing to the poor biodegradability of the wastewater. Additionally, a higher abundance of volatile organic compounds was detected in the mixed wastewater, while acrylonitrile appeared to be more concentrated in the spinning wastewater. The complementary use of spectral analysis, proton nuclear magnetic resonance, and HRMS provided a robust analytical foundation for identifying organic pollutants in acrylic fiber production wastewater. Full article

The multicomponent synthesis of a novel and highly symmetric polyheterocycle based on the pyrrolo[3,4-b]pyridin-5-one core incorporating the privileged tetrahydroisoquinoline moiety is described. The target compound was synthesized as an inseparable mixture of stereoisomers through a pseudo-repetitive Ugi–Zhu five-component reaction (PR-UZ-5CR) coupled to a double post-transformation sequence involving an intermolecular aza Diels–Alder cycloaddition, an intramolecular N-acylation, and a final tandem aromatization step. The product was prepared in 63% overall yield, and with an excellent atom economy of 85%, within a total reaction time of 85 min, and a temperature range from 25 to 65 °C. Structural elucidation and molecular mass confirmation were successfully achieved through NMR and FT-IR spectroscopy, and high-resolution mass spectrometry (HRMS), respectively. Full article

Substituted thiourea derivatives represent a structurally diverse group of compounds with high biological activity. In this paper, we present the synthesis of N-(9-ethyl-9H-carbazol-2-yl)-N′-(1-phenylethyl)thiourea by condensation reaction. The structure of the title compound was confirmed by ¹H and ¹³C nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), and high-resolution mass spectrometry (HRMS). Full article

Three new terpyridine derivatives which contain a pendant furan heterocycle have been prepared and characterized. The first two, 4′-(4,5-dimethylfuran-2-yl)-2,2′:6′,2″-terpyridine (1) and 4′-((1,3-dioxolan-2-yl)furan-2-yl)-2,2′:6′,2″-terpyridine (2), are obtained through the reaction of 2-acetylpyridine and suitable furaldehydes using the Kröhnke reaction. The last one, 4′-(5-formylfuran-2-yl)-2,2′:6′,2′’-terpyridine (3) is obtained via acidic hydrolysis of the acetal onto terpyridine (2). The structures of these new compounds are confirmed using different analytical techniques such as NMR and infrared spectroscopy (ATR-IR) as well as by High Resolution Mass Spectrometry (HRMS). Full article

Background/Objectives: The aim of this study was to reveal the influence of the natural nanoparticles (Nnps) isolated from Gegen–Qinlian Decoction (GQD), i.e., GQD-Nnps, on the intestinal absorption and pharmacokinetic properties of several representative active GQD constituents. Methods: The morphology of GQD-Nnps was examined using scanning electron microscopy (SEM). Protein and polysaccharide contents were measured using the bicinchoninic acid (BCA) assay and phenol–sulfuric acid method, respectively. Major GQD constituents were quantified by liquid chromatography–tandem mass spectrometry (LC-MS/MS). Formation mechanisms were explored using dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FTIR), and high-resolution mass spectrometry (HRMS). Pharmacokinetic studies were conducted in mice with dextran sulfate sodium (DSS)-induced UC. Results: GQD-Nnps were spherical, with a size of 110.9 ± 8.1 nm and a zeta potential of −13.7 ± 1.5 mV. GQD-Nnps were primarily composed of proteins and polysaccharides. FTIR analysis revealed significant hydrogen bonding interactions between the small molecular and macromolecular constituents of GQD. HRMS analyses indicated complex formation among small molecules, particularly berberine, baicalin, and glycyrrhizic acid. DLS demonstrated good stability of GQD-Nnps in artificial gastric and intestinal fluids. Pharmacokinetic studies showed that, except for puerarin, blood and liver exposure levels of several constituents in the GQD-Nnps group were significantly higher than those in the GQD extract group, suggesting enhanced colonic absorption and hepatic distribution. Conclusions: GQD-Nnps create an oral drug delivery system through complex interactions, significantly enhancing the colonic absorption and hepatic distribution of several active GQD constituents. Full article

The combination of multicomponent reactions with post-transformation processes is a powerful strategy for the rapid synthesis of structurally complex polyheterocycles. Herein, we describe the preparation of the novel compound 2-benzyl-6-(3-((7-chloroquinolin-4-yl)amino)propyl)-3-morpholino-7-(4-(pyridin-2-yl)phenyl)-6,7-dihydro-5H-pyrrolo[3,4-b]pyridin-5-one via a sequence that combines an Ugi-Zhu reaction with a cascade process (aza-Diels–Alder/N-acylation/aromatization) under microwave irradiation in chlorobenzene using ytterbium (III) triflate (Yb(OTf)₃) as the catalyst. The method provided the target polyheterocycle in 75% yield and 85% atom economy. Structural characterization was performed by 1D (¹H and ¹³C) and 2D (COSY, HSQC and HMBC) NMR spectroscopy, and the molecular mass was confirmed by high-resolution mass spectrometry (HRMS). These results illustrate the effectiveness of MCR as powerful synthetic tools for expanding chemical diversity. Full article

This study explores the photoprotective and antioxidant potential of cosmetic emulsions formulated with Alnus glutinosa (black alder) extracts. Extraction of bioactive compounds was performed using Soxhlet, ultrasound-assisted, and microwave-assisted techniques with ethanol and water as solvents. The phytochemical profiles of the resulting extracts were characterized via UV-Vis spectroscopy, Fourier-transform infrared spectroscopy (FTIR), and liquid chromatography–high-resolution mass spectrometry (LC-HRMS). The extracts were incorporated into oil-in-water emulsions and assessed for antioxidant activity using the DPPH radical scavenging assay, pH and viscosity stability, and color L*a*b* values. Among the extraction methods, ethanol-based Soxhlet extraction yielded the highest concentration of bioactive compounds and demonstrated superior antioxidant and photoprotective efficacy. This is the first report that evaluates the antioxidant properties of A. glutinosa-enriched emulsions, supporting their application as multifunctional, plant-derived cosmeceuticals for skin protection. Full article

This article focuses on the utilization of the supramolecular self-assembly of renewable materials derivatives to obtain functional compounds. Novel bio-based amphiphile molecules (CALAH and PALAH) were synthesized through a tailored process, involving Williamson ether synthesis and amidation reactions, employing renewable amino acid and cashew nut shell liquid (CNSL) derivatives as essential reactants. Their molecular structures were confirmed by nuclear magnetic resonance (NMR), high-resolution mass spectrometry (HRMS), and Fourier-transform infrared spectroscopy (FT-IR). Notably, these compounds self-assemble into nanofibers that organize into a fibrous network, unexpectedly exhibiting two distinct morphologies: curved and rigid nanostructures. These structures were characterized by scanning electron microscopy (SEM), and their formation mechanisms were elucidated through temperature-dependent NMR studies and density functional theory (DFT) calculations. The sodium salts of the compounds (PALA and CALA) exhibited fundamental surfactant properties, exhibiting a hydrophilic lipophilic balance (HLB) value of 13.7 and critical micelle concentration (CMC) values of 1.05 × 10⁻⁵ M and 4.10 × 10⁻⁶ M. They also demonstrated low cytotoxicity, suggesting potential suitability in consumer applications. Furthermore, the compounds exhibited multi-functional performance as effective inhibitors of Staphylococcus aureus and efficient adsorbents for gaseous pollutants. Full article

Diols represent a structurally diverse class of compounds with considerable biological and functional significance. Herein, we describe the synthesis of 1,1-bis(4-ethylphenyl)propan-1,2-diol (BEPP) via a Grignard reaction. The structure of BEPP was unambiguously elucidated by ¹H and ¹³C nuclear magnetic resonance (NMR), heteronuclear multiple-bond correlation (HMBC), high-resolution mass spectrometry (HRMS), and infrared (IR) spectroscopy. Full article