Search Results (532)

Broth cooking is a traditional pretreatment and ripening strategy for high-commercial-value dehydrated marine food, effectively enhancing its texture and rehydration properties. In this work, we characterized the structural information of Maillard reaction products (MRPs) derived from beef scrap stock and investigated their effects on the texture and rehydration performance of dehydrated abalone. The optical and structural properties of the MRPs were analyzed using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), and fluorescence spectroscopy. These MRPs showed osmosis in abalone processing including pretreatment and drying. Low-field nuclear magnetic resonance (LF-NMR) results revealed that MRP pretreatment improved the moisture migration and physicochemical properties of dehydrated abalone. These findings suggest that MRPs, owing to their high osmotic efficiency and nanoscale size, could serve as promising food additives and potential alternatives to traditional penetrating agents in the food industry, enhancing the rehydration performance of dried seafood and reducing quality deterioration. Full article

In boron neutron capture therapy (BNCT), the intracellular localization and concentration of boron-10 atoms significantly influence therapeutic efficacy. Although various boronic-acid-targeted fluorescent probes have been developed to evaluate BNCT agents, most of these probes emit at short wavelengths and are, therefore, incompatible with common nuclear-staining reagents such as Hoechst 33342 and 4′,6-diamidino-2-phenylindole (DAPI). While our previously reported probe, BS-631, emitted fluorescence above 500 nm, it exhibited limitations in terms of reaction rate and fluorescence intensity. To address these issues, we developed a boronic-acid-targeted fluorescent probe with a longer emission wavelength, rapid reactivity, and strong fluorescence intensity. Herein, we designed and synthesized BTTQ, a probe based on a 2-(2-hydroxyphenyl)benzothiazole core structure. BTTQ exhibited immediate fluorescence upon reaction with 4-borono-L-phenylalanine (BPA), with an emission wavelength of 567 nm and a sufficiently high fluorescence quantum yield for detection. BTTQ quantitatively detected BPA with high sensitivity (quantification limit of 10.27 µM), suitable for evaluating BNCT agents. In addition, BTTQ exhibited selective fluorescence for BPA over metal cations. Importantly, BTTQ enabled fluorescence microscopic imaging of intracellular BPA distribution in living cells co-stained with Hoechst 33342. These results suggest that BTTQ is a promising fluorescent probe for the evaluation of future BNCT agents. Full article

The habenula (Hb) of the epithalamus is formed of the medial (MHb) and lateral (LHb) parts. The improper functioning of the Hb may lead to depression and anxiety. The glutamate excitotoxicity is accompanied by astroglia reactivity and leads to the damage of nervous system structures. The aim of the study was to assess the influence of monosodium glutamate (MSG) administrated subcutaneously to rats in doses of 2 g/kg b.w. (I) and 4 g/kg b.w. (II), on astroglia in the MHb and LHb. Based on immunohistochemical reactions, the morphology, number of astrocytes immunoreactive for glial fibrillary acidic protein (GFAP-IR) and S100β protein (S100β-IR), and their surface area, perimeter, number and length of processes, and cytoplasmic-nuclear immunostaining intensity for the studied proteins were assessed. In the MHb of animals receiving MSG, especially at a high dose, hypertrophy and an increase in the number of GFAP-IR and S100β-IR cells were demonstrated. In the LHb, only hypertrophy of processes in S100β-positive glia was observed. The immunostaining intensity increased in GFAP-IR glia and decreased in S100β-IR cells only in animals from group I. The results revealed that astroglia respond to MSG depending on its dose and the Hb part. This different behavior of glia may indicate their different sensitivity and resistance to damaging factors. Full article

In this work, we report a novel mechanochemical synthesis method for the synthesis of quinoxaline derivatives—a spiral gas–solid two-phase flow approach, which enables the efficient preparation of quinoxaline compounds. Compared to conventional synthetic methods, this approach eliminates the need for heating or solvents while significantly reducing reaction time. The structures of the synthesized compounds were characterized using nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), ultraviolet-visible (UV–Vis) absorption spectroscopy, powder X-ray diffraction (XRD), differential scanning calorimetry (DSC), and high-performance liquid chromatography (HPLC). Using the synthesis of 2,3-diphenylquinoxaline (1) as a model reaction, the synthetic process was investigated with UV–Vis spectroscopy. The results demonstrate that when the total feed amount was 2 g with a carrier gas pressure of 0.8 MPa, the reaction completed within 2 min, achieving a yield of 93%. Furthermore, kinetic analysis of the reaction mechanism was performed by monitoring the UV–Vis spectra of the products at different time intervals. The results indicate that the synthesis of 1 follows the A4 kinetic model, which describes a two-dimensional diffusion-controlled product growth process following decelerated nucleation. Full article

The valence-shell electronic state spectroscopy of β-butyrolactone (CH₃CHCH₂CO₂) is comprehensively investigated by employing experimental and theoretical methods. We report a novel vacuum ultraviolet (VUV) absorption spectrum in the photon wavelength range from 115 to 320 nm (3.9–10.8 eV), together with ab initio quantum chemical calculations at the time-dependent density functional (TD-DFT) level of theory. The dominant electronic excitations are assigned to mixed valence-Rydberg and Rydberg transitions. The fine structure in the CH₃CHCH₂CO₂ photoabsorption spectrum has been assigned to C=O stretching, $v_7^{\prime }\left(a\right)$, CH₂ wagging, $v_{14}^{\prime }\left(a\right)$, C–O stretching, $v_{22}^{\prime }\left(a\right)$, and C=O bending, $v_{26}^{\prime }\left(a\right)$ modes. Photolysis lifetimes in the Earth’s atmosphere from 0 km up to 50 km altitude have been estimated, showing to be a non-relevant sink mechanism compared to reactions with the ^•OH radical. The nuclear dynamics along the C=O and C–C–C coordinates have been investigated at the TD-DFT level of theory, where, upon electronic excitation, the potential energy curves show important carbonyl bond breaking and ring opening, respectively. Within such an intricate molecular landscape, the higher-lying excited electronic states may keep their original Rydberg character or may undergo Rydberg-to-valence conversion, with vibronic coupling as an important mechanism contributing to the spectrum. Full article

Bis(2-ethylhexyl) phosphate (P204) is widely used in extraction processes in the nuclear and rare earth industries. However, its high solubility in water results in high levels of total organic carbon and phosphorus in aqueous environments, and may also lead to radioactive contamination when it is used to combine with radionuclides. In this paper, we characterized a coconut shell activated carbon (CSAC) and a coal-based activated carbon (CBAC) for the adsorption of P204 and then evaluated their adsorption performance through batch and column experiments. The results found that, except for the main carbon matrix, CSAC and CBAC carried rich oxygen-containing functional groups and a small amount of inorganic substances. Both adsorbents had porous structures with pore diameters less than 4 nm. CSAC and CBAC showed good removal performance for P204 under low pH conditions, with removal efficiencies significantly higher than those of commonly used adsorption resins (XAD-4 and IRA900). The adsorption kinetics of P204 conformed to the pseudo-second-order kinetic model, and the adsorption isotherms conformed to the Langmuir model, indicating a monolayer chemical reaction mechanism. Both adsorbents exhibited strong anti-interference capabilities; their adsorption performance for P204 did not change greatly with the ambient temperature or the concentrations of common interfering ions. Column experiments demonstrated that CSAC could effectively fix dissolved P204 with a removal efficiency exceeding 90%. The fixed P204 could be desorbed with acetone. The findings provide an effective method for the recovery of P204 and the regeneration of spent activated carbon, which shows promise for practical applications in the future. Full article

A series of new amide-based cyclotriphosphazene molecules consisting of different terminal groups (heptyl, decyl, and tetradecyl) at the periphery was successfully synthesized and characterized. The reaction began with the alkylation of methyl-4-hydroxybenzoate with 1-bromoheptane, 1-bromodecane, and 1-bromotetradecane, which was followed by reduction with potassium hydroxide to form a series of benzoic acid intermediates (1a–c). These intermediates underwent a reaction with thionyl chloride, followed by a reaction with 4-nitroaniline and triethylamine, to form para-substituted amides (2a–c). Further reduction of intermediates 2a–c with sodium sulfide hydrate produced the anilines 3a–c. Another reaction of hexachlorocyclotriphosphazene (HCCP) with methyl-4-hydroxybenzoate yielded intermediate 4, which was then reduced with sodium hydroxide to form intermediate 5. Finally, chlorination of intermediate 5 with thionyl chloride, followed by a reaction with the aniline derivatives (3a–c), formed the hexasubstituted cyclotriphosphazene compounds 6a–c, with two amide linkages. The structures of these compounds were confirmed using Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy and CHN elemental analysis. Full article

This study investigates the potential for the microbial transformation of camelliagenin B, a saponin derived from Camellia oleifera seed cake meal, to develop novel metabolites. We employed three microbial strains, specifically Bacillus subtilis ATCC 6633, Bacillus megaterium CGMCC 1.1741, and Streptomyces griseus ATCC 13273, to biotransform camelliagenin B into its derivatives. The compounds were purified and separated using chromatographic techniques, such as high-performance liquid chromatography (HPLC). Structural identification was carried out using spectroscopic methods, including nuclear magnetic resonance (NMR) and mass spectrometry (MS). Ten bioactive compounds were obtained (1a-1j), of which nine were novel with multiple tailoring reactions, such as allyl oxidation, C-C double-bond rearrangement, hydroxylation, dehydrogenation, and glycosylation, observed in camelliagenin B analogs. The structures of these compounds were determined by 1D/2D NMR and HR-ESI-MS analysis. Therefore, this study showcases the capacity of microbial transformation as a sustainable and environmentally friendly method for generating bioactive compounds from C. oleifera seed cake meals. The individual chemicals can potentially facilitate the design of novel medicinal agents, functional foods, and natural preservatives. Full article

Searching for new and efficient transfer hydrogenation catalysts, a series of new organometallic ruthenium(II)-arene complexes of the formulae [Ru(η⁶-p-cymene)(L)Cl][PF₆] (1–8) and [Ru(η⁶-p-cymene)(L)Cl][Ru(η⁶-p-cymene)Cl₃] (9–11) were synthesized and fully characterized. These were prepared from the reaction of pyridine–quinoline and biquinoline-based ligands (L) with [Ru(η⁶-p-cymene)(μ-Cl)Cl]₂, in 1:2 and 1:1, metal (M) to ligand (L) molar ratios. Characterization includes a combination of spectroscopic methods (FT-IR, UV-Vis, multi nuclear NMR), elemental analysis and single-crystal X-ray crystallography. The pyridine–quinoline organic entities encountered, were prepared in high yield either via the thermal decarboxylation of the carboxylic acid congeners, namely 2,2′-pyridyl-quinoline-4-carboxylic acid (pqca), 8-methyl-2,2′-pyridyl-quinoline-4-carboxylic acid (8-Mepqca), 6′-methyl-2,2′-pyridyl-quinoline-4-carboxylic acid (6′-Mepqca) and 8,6′-dimethyl-2,2′-pyridyl-quinoline-4-carboxylic acid (8,6′-Me₂pqca), affording the desired ligands pq, 8-Mepq, 6′-Mepq and 8,6′-Me₂pq, or by the classical Friedländer condensation, to yield 4,6′-dimethyl-2,2′-pyridyl-quinoline (4,6′-Me₂pq) and 4-methyl-2,2′-pyridyl-quinoline (4-Mepq), respectively. The solid-state structures of complexes 1–4, 6, 8 and 9 were determined showing a distorted octahedral coordination geometry. The unit cell of 3 contains two independent molecules (Ru-3), (Ru′-3) in a 1:1 ratio, due to a slight rotation of the arene ring. All complexes catalyze the transfer hydrogenation of acetophenone, using 2-propanol as a hydrogen donor in the presence of KOiPr. Among them, complexes 1 and 5 bearing methyl groups at the 8 and 4 position of the quinoline moiety, convert acetophenone to 1-phenylethanol quantitatively, within approximately 10 min with final TOFs of 1600 h⁻¹. The catalytic performance of complexes 1–11, towards the transfer hydrogenation of p-substituted acetophenone derivatives and benzophenone, ranges from moderate to excellent. An inner-sphere mechanism has been suggested based on the detection of ruthenium(II) hydride species. Full article

A quantitative characterization of the change in coal molecular structures with different cyclical microwave modification parameters and a better understanding of the reaction mechanism of the modification are of great significance for the commercial extraction of coal bed methane (CBM). Therefore, long-flame coal samples obtained from the Ordos Basin, China, were modified by microwave radiation with different times, and the long-flame coal molecular structure parameters were determined by solid-state ¹³C nuclear magnetic resonance (ss¹³C NMR), Fourier transform infrared (FTIR) spectrometry, and X-ray photoelectron spectrometry (XPS). Atomistic representations of the raw long-flame coal molecular model and modified long-flame coal molecular models were established. The temperature rise, pore volume increase, mineral removal, and functional group changes after the modification have a negative effect on methane adsorption. After the modification, the decrease in surface area of the micropores reduced the adsorption site of methane in coal. As a result, the methane adsorption amount decreased linearly with the decreasing surface area. The CH₄ adsorption isotherms of the long-flame models were dynamically simulated and analyzed. The results of this study can prove that after multiple cycles of microwave modifications, the functional groups in long-flame coal were fractured, and the number of micropores was reduced, which effectively decreased the methane adsorption performance in long-flame coal seams, thereby promoting methane extraction. Microwave modification is a promising method for enhancing CBM recovery. Full article

Main-chain conjugated and non-conjugated polyelectrolytes are an important class of materials that have many technological applications ranging from fire-retardant materials to carbon-nanotube composites, nonlinear optical materials, electrochromic materials for smart windows, and optical sensors for biomolecules. Here, we describe a series of poly(pyridinium salt)s-fluorene containing 9,9-bis(4-aminophenyl)fluorene moieties with various organic counterions that were synthesized using ring-transmutation polymerization and metathesis reactions, which are non-conjugated polyelectrolytes. Their chemical structures were characterized by Fourier transform infrared (FTIR), proton (¹H) and fluorine 19 (¹⁹F) nuclear magnetic resonance (NMR) spectrometers, and elemental analysis. They exhibited polyelectrolytic behavior in dimethyl sulfoxide. Their lyotropic liquid-crystalline phases were examined by polarizing optical microscopy (POM) and small angle X-ray scattering (SAXS) studies. Their emission spectra exhibited a positive solvatochromism on changing the polarity of solvents. They emitted greenish-yellow lights in polar organic solvents. They formed aggregates in polar aprotic and protic solvents with the addition of water (v/v, 0–90%), whose λ_em peaks were blue shifted. Full article

Cyclic Olefin Copolymer (COC) is an amorphous thermoplastic polymer synthesized through the catalytic copolymerization of α-olefin and cyclic olefin. When used in pre-filled syringes and pharmaceutical packaging, COCs require radiation sterilization. The radiation sterilization alters the microstructure of COC, which ultimately affects its performance and biosafety. In this study, to investigate the effects of γ-radiation on COC microstructures, ethylene-norbornene copolymers with various compositions, representative of COC, are studied by nuclear magnetic resonance (NMR) and small angle X-ray scattering (SAXS) techniques. During irradiation, the COC containing 35 mol% norbornene produced free radicals that triggered migration and reaction processes, leading to the formation of entanglements within flexible chain segments. This, in turn, affected nearby ring structures with high steric hindrance, resulting in a 9.2% decrease in internal particle size and an increase in particle spacing. Conversely, when the norbornene content in COC was increased to 57 mol%, the internal particle size increased by 17.9%, while the particle spacing decreased. Full article

Biflavonoids are a unique subclass of dietary polyphenolic compounds known for their diverse bioactivities. Despite these benefits, these biflavonoids remain largely underexplored due to their limited natural availability and harsh conditions required for their synthesis, which restricts broader research and application in functional foods and nutraceuticals. To address this gap, we synthesized a library of rare biflavonoids using a radical–nucleophile coupling reaction previously reported by our group. The food grade coupling reaction under weakly alkaline water at room temperature led to isolation of 28 heterocoupled biflavones from 11 monomers, namely 3′,4′-dihydroxyflavone, 5,3′,4′-trihydroxyflavone, 6,3′,4′-trihydroxyflavone, 7,3′,4′-trihydroxyflavone, diosmetin, chrysin, acacetin, genistein, biochanin A, and wogonin. The structures of the dimers are characterized by nuclear magnetic resonance spectroscopy (NMR) and high-resolution mass spectroscopy (HRMS). In addition, we evaluated the antioxidant potential of these biflavones using a DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging assay and the DPPH value ranges between 0.75 to 1.82 mM of Trolox/mM of sample across the 28 synthesized dimers. Additionally, a three-dimensional quantitative structure–activity relationship (3D-QSAR) analysis was conducted to identify structural features associated with enhanced antioxidant activity. The partial least squares (PLS) regression QSAR model showed acceptable r² = 0.936 and q² = 0.869. Additionally, the average local ionization energy (ALIE), electrostatic potential (ESP), Fukui index (F-), and electron density (ED) were determined to identify the key structural moiety that was capable of donating electrons to neutralize reactive oxygen species. Full article

The modified asphalt with high softening point was prepared by air oxidation polymerization with coal liquefied asphalt as raw material. The quality control model regarding the coking value and softening point of the product were established based on the DFSS (Design for Six Sigma) and RSM (response surface method). By means of elemental analysis, infrared, XPS, XRD, nuclear magnetic, MALDI-TOF and other characterization methods, the composition and structure characteristics of the modified asphalt were analyzed. Using the target product as raw material, general base asphalt carbon fiber was prepared by spinning, pre-oxidation and carbonization. The results show that the fitting effect of the quality control model about the coking value and softening point of the product is good, and the operating window range of the polymerization process parameters corresponding to the preparation of target product is wide. It can be found that the oxidation time and oxidation temperature has the most significant effect on the coking value and softening point of products, respectively, and all of them show a positive correlation. The dealkylation reaction and oxidative crosslinking reaction were carried out at the same time, and the bridging products of methylene bridging products, ether–oxygen bonds, carbonyl bonds, anhydride bonds and other oxygen-containing groups were generated. The properties of carbon fiber prepared with the target product are better: the tensile strength is 775 MPa, the elastic modulus is 68.6 GPa and the elongation at break is 1.13%. Full article

Wood adhesives play a critical role in the wood processing industry; however, traditional formaldehyde-based adhesives pose health risks and are reliant on non-renewable resources. This study aims to develop a bio-based wood adhesive with excellent water resistance, focusing on environmentally friendly solutions. The synthesis of an oxidized starch-lignin (OSTL) composite adhesive was accomplished by modifying starch via oxidation and subsequent cross-linking with lignin. Ammonium persulfate (APS) was employed for oxidation of starch, introducing aldehyde groups that upgrade its reactivity with lignin. Subsequently, the oxidized starch (OST) was cross-linked with the phenolic rings of lignin, resulting in a strong network structure. The oxidation of starch and its cross-linking mechanism with lignin were investigated using the Fourier transform infrared (FT-IR), proton nuclear magnetic resonance (1H-NMR), and X-ray photoelectron spectroscopy (XPS) techniques, proving the formation of aldehyde and carboxyl groups with subsequent reaction possibilities. The effects of oxidant dosage, oxidation time, and the ratio of starch to lignin on the adhesive properties were systematically studied. The results demonstrated that the OSTL adhesive, prepared under optimized conditions, exhibited outstanding adhesion strength (1.23 MPa in dry state) and water resistance (0.94 MPa after 24 h cold water immersion, 1.04 MPa after 3 h in hot water, and 0.69 MPa after 3 h in boiling water), significantly outperforming conventional wood adhesives in terms of cold water, hot water, and boiling water resistance. In addition, the thermal behavior of the OSTL adhesive was further validated using differential scanning calorimetry (DSC) as well as thermogravimetric analysis (TGA). This study presents new insights and technical support for the development of green, environmentally friendly, and highly water-resistant lignin-based bio-adhesives. Full article