Mechanochemical-Assisted Extraction and Biological Activity Research of Phenolic Compounds from Lotus Seedpod (Receptaculum Nelumbinis).

To explore the feasibility of the mechanochemical-assisted extraction (MCAE) of phenolic compounds from lotus seedpod (Receptaculum Nelumbinis), a single-factor experiment combined with response-surface methodology (RSM) was used to optimize the extraction process. The results showed the optimal extraction conditions as follows: Li2CO3 as a solid reagent (25%), an extraction time of 80 min, liquid/solid ratio of 42.8 mL/g, and extraction temperature of 80.7 °C; and the maximum value of total phenolic content (TPC) was 106.15 ± 1.44 gallic acid equivalents (GAE)/g dry weight (DW). Additionally, the 2,2-Diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azinobis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), and ferric reducing antioxidant power (FRAP) were 279.75 ± 18.71, 618.60 ± 2.70, and 634.14 ± 7.17 µmol TE/g, respectively. Ultra-high pressure liquid chromatography combined with triple-time-of-flight mass spectrophotometry (UPLC-Triple-TOF/MS) analysis identified eight phenolic compounds mainly consisting of polyphenols and flavonoids. Moreover, the phenolic compounds showed potent inhibitory effects on both α-amylase and α-glucosidase, with inhibition rates of over 80%. Furthermore, the results showed different degrees of inhibition activity against Bacillus subtilis, Staphylococcus aureus, and Escherichia coli, among which the inhibitory effect on the growth of B. subtilis was the best. This paper shows that the phenolic compounds have good biological activities, which provides a reference for the further exploitation of LSP.

Fabrication and Characterization of Complex Coacervation: The Integration of Sesame Protein Isolate-Polysaccharides.

The exceptional biocompatibility of emulsion systems that rely on stabilizing protein-polysaccharide particles presents extensive possibilities for the transportation of bioactive carriers, making them highly promising for various biological applications. The current work aimed to explore the phenomenon of complex coacervation between sesame protein isolate (SPI) and four distinct polysaccharides, namely, Arabic gum (GA), carrageenan (CAR), sodium carboxymethyl cellulose (CMC), and sodium alginate (SA). The study objective was achieved by fabricating emulsions through the blending of these polymers with oil at their maximum turbidity level (φ = 0.6), followed by the measurement of their rheological properties. The turbidity, ζ-potential, and particle size were among the techno-parameters analyzed to assess the emulsion stability. The microstructural characterization of the emulsions was conducted using both transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Furthermore, the functional properties were examined using Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The SPI incorporated with SA, CMC, and CAR reached the maximum turbidity (0.2% w/v) at a ratio of 4:1, corresponding to the pH values of 4.5, 3, or 3.5, respectively. The SPI-GA mixture exhibited the maximum turbidity at a ratio of 10:1 and pH 4.5. Results from the FTIR and XRD analyses provided evidence of complex formation between SPI and the four polysaccharides, with the electrostatic and hydrogen bond interactions facilitating the binding of SPI to these polysaccharides. SPI was bound to the four polysaccharides through electrostatic and hydrogen bond interactions. The SPI-CMC and SPI-SA emulsions were more stable after two weeks of storage.

Realization of High Magnetization in Artificially Designed Ni/NiO Layers through Exchange Coupling.

High-magnetization materials play crucial roles in various applications. However, the past few decades have witnessed a stagnation in the discovery of new materials with high magnetization. In this work, Ni/NiO nanocomposites are fabricated by depositing Ni and NiO thin layers alternately, followed by annealing at specific temperatures. Both the as-deposited samples and those annealed at 373 K exhibit low magnetization. However, the samples annealed at 473 K exhibit a significantly enhanced saturation magnetization exceeding 607 emu cm-3 at room temperature, surpassing that of pure Ni (480 emu cm-3 ). Material characterizations indicate that the composite comprises NiO nanoclusters of size 1-2 nm embedded in the Ni matrix. This nanoclustered NiO is primarily responsible for the high magnetization, as confirmed by density functional theory calculations. The calculations also indicate that the NiO clusters are ferromagnetically coupled with Ni, resulting in enhanced magnetization. This work demonstrates a new route toward developing artificial high-magnetization materials using the high magnetic moments of nanoclustered antiferromagnetic materials.

Determination of the Anti-Oxidative Stress Mechanism of Isodon suzhouensis Leaves by Employing Bioinformatic and Novel Research Technology.

Isodon suzhouensis from Suzhou, China, is a traditional Chinese herb with wide applications in medicine and food. The antioxidant activity against oxidative stress of the leaves of Isodon suzhouensis is a myth since long and is not explored earlier thoroughly. The present study is focused to explore the active components in Isodon suzhouensis leaf extracts responsible for antioxidant effects against oxidative stress and the potential mechanism of this activity. We obtained the chromatograms of Isodon suzhouensis leaf extracts by the high-performance liquid phase (HPLC) for possible detection of antioxidant constituents. Some compounds in Isodon suzhouensis leaf extracts were then further assessed through the luminol luminescence mechanism combined with HPLC analysis as well as with SwissTargetPrediction database that helped to screen out the other constituents. The targets for effects against oxidative stress were then further screened through the GeneCards database, and the PPI network was constructed. The targets were analyzed by GO and KEGG using the David database. The obtained results were then further studied by employing in vitro experimentation and protein expression analyses by Western blotting. It is found that Isodon suzhouensis leaf extracts contain rutin, isoquercetin, glaucocalyxin A, glaucocalyxin B, and other compounds with antioxidant activity. The activity map of the free radical scavenging signals from Isodon suzhouensis showed a strong ability to scavenge free radicals with the highest capacity of glaucocalyxin B followed by isoquercetin succeeding the glaucocalyxin A supervening the rutin. Further network pharmacological analyses and in vitro experimentation showed that Isodon suzhouensis leaf extracts interfere with TNF and the p38 MAPK signaling pathway for antioxidant effects against oxidative stress. Conclusively, it is found that Isodon suzhouensis leaf extracts possess strong antioxidant potential via targeting TNF and p38 MAPK signaling pathways against oxidative stress, providing scientific foundation for further studies on Isodon suzhouensis for the further therapeutic approach.

Identification of phytochemicals and antioxidant activity of Premna microphylla Turcz. stem through UPLC-LTQ-Orbitrap-MS.

Premna microphylla Turcz. is a commonly used traditional Chinese medicine totreatdysentery and appendicitis. Present study is focused to explore antioxidants and other compounds in the Premna microphylla Turcz. stem. Assessment of chemical composition was done with high sensitivity UPLC-LTQ-Orbitrap-MS and for Separation Thermo Hypersil Gold (100 mm × 2.1 mm, 1.9 µm) was used while electrospray ionization (ESI) was used for the mass spectrometry. 18 compounds were identified including Vitexin (1), Schaftoside (2), Vicenin-2 (3), Apigenin-6, 8-di-C-arabinoside (4), Apigenin-7-O-ß-d-glucoside (5), Carnosic acid (6), Apigenin-8-C-ß-d-xylopyranoside (7), Prostratin (8), Aurantio-obtusin-ß-d-glucoside (9), Royleanone (10), 5-hydroxy-7,3',4'-Trimethoxy flavonols (11), 6-Hydroxy-5,6-dehydrosugiol (12), 14-deoxycoleon (13), Arucadiol (14), Obtusinone-B (15), Trehalose (16), Citric acid (17) and Betaine (18). Among these, 6 compounds including (6), (8), (9), (16), (17) and (18) were identified first time within this genus and plant. Study highlights the importance of Premna microphylla Turcz. stem extract for strong therapeutic potential against oxidation-related diseases.

Green and Efficient Extraction Approach for Polyphenol Recovery from Lotus Seedpods (Receptaculum Nelumbinis): Gas-Assisted Combined with Glycerol.

In this paper, the gas-assisted combined with glycerol extraction (GAGE) for polyphenol recovery from lotus seedpods (LSPs) was modeled and optimized. Box-Behnken design was applied to optimize the total polyphenol content (TPC) of LSP along with enhancing antioxidant activities using response surface methodology based on the TPC extraction yield (%), which was affected by glycerol concentration, time, temperature, and glycerol-to-solid ratio. The optimal conditions for the LSP extract were glycerol-to-solid ratio, 42 mL/g; time, 50 min; concentration of glycerol, 45%; and temperature, 70 °C. Ultra-high-pressure liquid chromatography integrated with triple-time-of-flight mass spectrophotometry (UPLC-Triple-TOF/MS) analysis revealed nine biologically active polyphenols. Furthermore, Fourier-transform infrared spectroscopy and scanning electron microscopy results demonstrated the effect and influence during extraction. The findings suggested that GAGE is a potential, green, and high-efficiency alternative that could be used to recover polyphenols from plant source byproducts.

Green Extraction of Phenolic Compounds from Lotus Seedpod (Receptaculum Nelumbinis) Assisted by Ultrasound Coupled with Glycerol.

Lotus Receptaculum Nelumbinis has been sparking wide research interests due to its rich phenolic compounds. In the present work, ultrasonic-assisted extraction coupled with glycerol was employed to extract phenolic compounds from Receptaculum Nelumbinis and the process was optimized using a response surface methodology with Box-Behnken design (BBD). The optimal conditions for the total phenolic content (TPC) extract were obtained: glycerol concentration of 40%, an extraction temperature of 66 °C, ultrasonic time of 44 min, and the solvent-to-solid ratio of 55 mL/g. Under these optimum extraction conditions, the extraction yield of TPC was 92.84 ± 2.13 mg gallic acid equivalents (GAE) /g. Besides, the antioxidant activities demonstrated the ability of free radical scavenging by four different methods that included 2,2-Diphenyl-1-picrylhydrazyl (DPPH), ferric reducing antioxidant power (FRAP), 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), and reducing activity (RA) were 459.73 ± 7.07, 529.97 ± 7.30, 907.61 ± 20.28, and 983.66 ± 11.80 µmol TE/g, respectively. Six phenolic compounds were identified by ultra-high pressure liquid chromatography combined with triple-time-of-flight mass spectrophotometry (UPLC-Triple-TOF/MS) from the extracts. Meanwhile, Fourier transform infrared (FTIR) was conducted to identify the characteristic functional groups of the extracts and thus reflected the presence of polyphenols and flavonoids. Scanning electron microscopy (SEM) illustrated the microstructure difference of four treatments, which might explain the relationships between antioxidant activities and the structures of phenolic compounds.

Colossal Magnetization and Giant Coercivity in Ion-Implanted (Nb and Co) MoS2 Crystals.

Colossal saturation magnetization and giant coercivity are realized in MoS2 single crystals doped with Nb and/or Co using an ion implantation method. Magnetic measurements have demonstrated that codoping with 2 at % Nb and 4 at % Co invoked a "giant" coercivity, as high as 9 kOe at 100 K. Doping solely with 5 at % Nb induces a "colossal" magnetization of 1800 emu/cm3 at 5 K, which is higher than that of metallic Co. The high magnetization is due to the formation of Nb-rich defect complexes, as confirmed by first-principles calculations. It is proposed that the high coercivity is due to the combined effects of strong directional exchange coupling induced by the Nb and Co doping and pinning effects from defects within the layered structure. This high magnetization mechanism is also applicable to 2D materials with bilayers or few layers of thickness, as indicated by first-principles calculations. Hence, this work opens a potential pathway for the development of 2D high-performance magnetic materials.

Critical Control of Highly Stable Nonstoichiometric Mn-Zn Ferrites with Outstanding Magnetic and Electromagnetic Performance for Gigahertz High-Frequency Applications.

Pristine nonstoichiometric Mn-Zn ferrites were synthesized using a facile "heating-up" method. A route for achieving very stable single-crystal spinel Mn-Zn ferrites with enhanced magnetic performance and Curie temperature was explored using annealing procedures, where the protective gas flow velocities, heating rates, and annealing temperatures were critical in determining the phase structures and performance. The annealed Mn-Zn ferrites showed ultrahigh saturation magnetizations of ∼120 emu/g and an ultrahigh Curie temperature of ∼750 K. Mössbauer spectra indicated that the valence state of Mn was maintained at Mn2+, and both Mn and Zn were located at A sites in the inverse spinel structure for the highly stable Mn-Zn ferrites. An excellent microwave-absorbing capability in a broad frequency range of 0.1-18 GHz was realized owing to the large magnetic and dielectric losses. The optimal match thickness of Mn-Zn ferrites was found to be 1.5 mm, corresponding to a maximum reflection loss of 22 dB at 16 GHz. These results indicate that the synthesized Mn-Zn ferrites exhibit significant advantages in microwave absorption in the high-frequency range. The demonstrated multicomponent ferrites with high magnetic performance and Curie temperature may find broad applications in various complicated environments, such as those having elevated temperatures.

High Coercivity and Magnetization in WSe2 by Codoping Co and Nb.

Introducing ferromagnetism in transition metal dichalcogenides has attracted lots of attention due to the possible applications in spintronics devices. Generally, single magnetic element doping is used to introduce magnetism. However, mostly, weak ferromagnetism is observed. In this work, codoping of two kinds of transition metals (Nb and Co) into WSe2 is used to study its magnetic properties. In detail, single crystal WSe2 is codoped with 4 at% Co and various concentrations of Nb by employing the physical ion implantation method. Raman, X-ray diffraction and X-ray photoelectron spectroscopy results reveal the effective substitutional doping of implanted elements (Co and Nb). Magnetic measurements illustrate that both un-doped and 4 at% Co doped WSe2 show weak ferromagnetism whereas magnetization is strongly enhanced when Co and Nb are codoped into WSe2 . The magnetization is comparable with a ferromagnet, which may be attributed to Co, Nb doping and defects. In addition, a large coercivity of ≈1.2 kOe is observed in the 1 at% Nb-4 at% Co codoped WSe2 sample, which may be ascribed to the combined effect of doping-induced stress, defect-dictated pinning and anisotropy of NbSe bond owing to the charge transfer between Nb and Se ions.

Confinement-Induced Giant Spin-Orbit-Coupled Magnetic Moment of Co Nanoclusters in TiO2 Films.

High magnetization materials are in great demand for the fabrication of advanced multifunctional magnetic devices. Notwithstanding this demand, the development of new materials with these attributes has been relatively slow. In this work, we propose a new strategy to achieve high magnetic moments above room temperature. Our material engineering approach invoked the embedding of magnetic nanoclusters in an oxide matrix. By precisely controlling pulsed laser deposition parameters, Co nanoclusters are formed in a 5 at % Co-TiO2 film. The presence of these nanoclusters was confirmed using transmission electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray absorption fine structure. The film exhibits a very high saturation magnetization of 99 emu/cm3. Detailed studies using X-ray magnetic circular dichroism confirm that Co has an enhanced magnetic moment of 3.5 µB/atom, while the Ti and O also contribute to the magnetic moments. First-principles calculations supported our hypothesis that the metallic Co nanoclusters surrounded by a TiO2 matrix can exhibit both large spin and orbital moments. Moreover, a quantum confinement effect results in a high Curie temperature for the embedded Co nanoclusters. These findings reveal that 1-2 nm nanoclusters that are quantum confined can exhibit very large magnetic moments above room temperature, representing a promising advance for the design of new high magnetization materials.

Intrinsic or Interface Clustering-Induced Ferromagnetism in Fe-Doped In2O3-Diluted Magnetic Semiconductors.

Five percent Fe-doped In2O3 films were deposited using a pulsed laser deposition system. X-ray diffraction and transmission electron microscopy analysis show that the films deposited under oxygen partial pressures of 10-3 and 10-5 Torr are uniform without clusters or secondary phases. However, the film deposited under 10-7 Torr has a Fe-rich phase at the interface. Magnetic measurements demonstrate that the magnetization of the films increases with decreasing oxygen partial pressure. Muon spin relaxation (µSR) analysis indicates that the volume fractions of the ferromagnetic phases in PO2 = 10-3, 10-5, and 10-7 Torr-deposited samples are 23, 49, and 68%, respectively, suggesting that clusters or secondary phases may not be the origin of the ferromagnetism and that the ferromagnetism is not carrier-mediated. We propose that the formation of magnetic bound polarons is the origin of the ferromagnetism. In addition, both µSR and polarized neutron scattering demonstrate that the Fe-rich phase at the interface has a lower magnetization compared to the uniformly distributed phases.

Ferromagnetic ordering in Mn-doped ZnO nanoparticles.

Zn1 - x Mn x O nanoparticles have been synthesized by hydrothermal technique. The doping concentration of Mn can reach up to 9 at% without precipitation or secondary phase, confirmed by electron spin resonance (ESR) and synchrotron X-ray diffraction (XRD). Room-temperature ferromagnetism is observed in the as-prepared nanoparticles. However, the room-temperature ferromagnetism disappears after post-annealing in either argon or air atmosphere, indicating the importance of post-treatment for nanostructured magnetic semiconductors.

Nanomagnetism study of highly-ordered iron oxide nanocrystal assemblies fabricated by the Langmuir-Blodgett technique.

Iron oxide nanocrystals are ideal building blocks for the construction of flexible nanodevices whose performance can be modulated by controlling the morphology of isolated particles and their organizational form. This work demonstrates the fabrication of high quality Langmuir-Blodgett (LB) nanocrystal assemblies with limited overlapping and higher coverage by systemically and combinatorially optimizing the parameters of compression pressure and quantity of spread nanocrystals. Monodispersed iron oxide nanocrystals with a diameter of 11.8 nm were synthesized by thermal decomposition of Fe(CO)5 in trioctylamine with the presence of oleic acid. Multilayer nanocrystal assemblies were obtained through a layer-by-layer (LBL) process by repeating the transfer procedure after their hydrophilicity had been improved via treatment in a UV-ozone oven. The quality of nanocrystal assemblies was investigated by UV-vis spectrometry and scanning electron microscopy. The nanomagnetism for the nanostructures of different combination manners was studied systemically by a superconducting quantum interference device (SQUID). A lower superparamagnetic blocking temperature was found in the monolayer Fe3O4 nanocrystal assembly. The superparamagnetic blocking temperature in magnetic nanocrystal assemblies could be tuned through modifying the interparticle interactions among the interlayer and intralayers by controlling the layer number of the assemblies.

Pushing extended p-quinodimethanes to the limit: stable tetracyano-oligo(N-annulated perylene)quinodimethanes with tunable ground states.

p-Quinodimethane (p-QDM) is a fundamental building block for the design of π-conjugated systems with low band gap and open-shell biradical character. However, synthesis of extended p-QDMs has usually suffered from their intrinsic high reactivity and poor solubility. In this work, benzannulation together with terminal cyano-substitution was demonstrated to be an efficient approach for the synthesis of a series of soluble and stable tetracyano-oligo(N-annulated perylene)quinodimethanes nPer-CN (n = 1-6), with the longest molecule having 12 para-linked benzenoid rings! The geometry and electronic structures of these oligomers were investigated by steady-state and transient absorption spectroscopy, nuclear magnetic resonance, electron spin resonance, superconducting quantum interference device, and FT Raman spectroscopy assisted by density functional theory calculations. They showed tunable ground states, varying from a closed-shell quinoidal structure for monomer, to a singlet biradical for dimer, trimer, and tetramer, and to a triplet biradical for pentamer and hexamer. Large two-photon absorption cross-section values were observed in the near-infrared range, which also exhibited a clear chain-length dependence.

Stable tetrabenzo-Chichibabin's hydrocarbons: tunable ground state and unusual transition between their closed-shell and open-shell resonance forms.

Stable open-shell polycyclic aromatic hydrocarbons (PAHs) are of fundamental interest due to their unique electronic, optical, and magnetic properties and promising applications in materials sciences. Chichibabin's hydrocarbon as a classical open-shell PAH has been investigated for a long time. However, most of the studies are complicated by their inherent high reactivity. In this work, two new stable benzannulated Chichibabin's hydrocarbons 1-CS and 2-OS were prepared, and their electronic structure and geometry in the ground state were studied by various experiments (steady-state and transient absorption spectra, NMR, electron spin resonance (ESR), superconducting quantum interference device (SQUID), FT Raman, X-ray crystallographic etc.) and density function theory (DFT) calculations. 1-CS and 2-OS exhibited tunable ground states, with a closed-shell quinoidal structure for 1-CS and an open-shell biradical form for 2-OS. Their corresponding excited-state forms 1-OS and 2-CS were also chemically approached and showed different decay processes. The biradical 1-OS displayed an unusually slow decay to the ground state (1-CS) due to a large energy barrier (95 ± 2.5 kJ/mol) arising from severe steric hindrance during the transition from an orthogonal biradical form to a butterfly-like quinoidal form. The quick transition from the quinoidal 2-CS (excited state) to the orthogonal biradicaloid 2-OS (ground state) happened during the attempted synthesis of 2-CS. Compounds 1-CS and 2-OS can be oxidized into stable dications by FeCl(3) and/or concentrated H(2)SO(4). The open-shell 2-OS also exhibited a large two-photon absorption (TPA) cross section (760 GM at 1200 nm).

Kinetically blocked stable heptazethrene and octazethrene: closed-shell or open-shell in the ground state?

Polycyclic aromatic hydrocarbons with an open-shell singlet biradical ground state are of fundamental interest and have potential applications in materials science. However, the inherent high reactivity makes their synthesis and characterization very challenging. In this work, a convenient synthetic route was developed to synthesize two kinetically blocked heptazethrene (HZ-TIPS) and octazethrene (OZ-TIPS) compounds with good stability. Their ground-state electronic structures were systematically investigated by a combination of different experimental methods, including steady-state and transient absorption spectroscopy, variable temperature NMR, electron spin resonance (ESR), superconducting quantum interfering device (SQUID), FT Raman, and X-ray crystallographic analysis, assisted by unrestricted symmetry-broken density functional theory (DFT) calculations. All these demonstrated that the heptazethrene derivative HZ-TIPS has a closed-shell ground state while its octazethrene analogue OZ-TIPS with a smaller energy gap exists as an open-shell singlet biradical with a large measured biradical character (y = 0.56). Large two-photon absorption (TPA) cross sections (σ((2))) were determined for HZ-TIPS (σ((2))(max) = 920 GM at 1250 nm) and OZ-TIPS (σ((2))(max) = 1200 GM at 1250 nm). In addition, HZ-TIPS and OZ-TIPS show a closely stacked 1D polymer chain in single crystals.