Olive pomace contains abundant maslinic acid and oleanolic acid, which are pentacyclic triterpenoid compounds with excellent biological activity. In this study, a method combining high-speed shear extraction and HPLC analysis was developed to determine the contents of maslinic acid and oleanolic acid in olive pomace. Single-factor experiments were conducted to optimize the high-speed shear extraction conditions, including rotation speed, liquid-to-material ratio, processing time, and extraction solvent type. The optimized extraction conditions were as follows: methanol as the extraction solvent, a rotation speed in the range of 8000-12 000 rpm, a processing time of 2 minutes, and a liquid-to-material ratio of 0.5 (mL/50 mg). The recovery rates of the HPLC method ranged from 98.34% to 109.25%, with a relative standard deviation (RSD) of less than 3.01%; LOD were 0.0035 µg mL-1 and 0.0038 µg mL-1, the LOQ were 0.012 µg mL-1 and 0.014 µg mL-1; and the intra-day and inter-day precisions were 2.07% and 2.95% and 2.9% and 2.85% for maslinic acid and oleanolic acid, respectively. This method is simple to operate and enables rapid and efficient extraction of the target components from olive pomace at room temperature, making it suitable for the quantitative determination of trace components in olive pomace.
This study developed an antimicrobial composite film with dual functions of antibacterial activity and freshness preservation. Carvacrol-loaded microcapsules were embedded into a linear low-density polyethylene (LLDPE) matrix using the melt extrusion process. Compared to the pure LLDPE film, the composite films containing 0.5
Smart nanopesticides demonstrate excellent potential in the prevention of tomato gray mold. Herein, temperature, pH and GSH triple responsive of pyraclostrobin nanopesticide (CDC-F127-P) is fabricated base on Pluronic F127 and cinnamaldehyde-derived liposome. The maximum fungicide loading of Pyr reaches 52.9%. The particle size and zeta potential are 143 nm and + 29 mV. The release of Pyr increases from 38% to 61% after 48 h as the temperature rises from 5 °C to 35 °C. The value increases from 62% to 87% when the concentration of oxalic acid rises from 0 to 20 mM, which increases from 10% to 37% as the concentration of GSH rises from 0 to 20 mM. The EC₅₀ of CDC-F127-P is 1.96 μg/mL. The inhibition rates of CDC-F127-P for mycelial growth and spore germination are 69.3% and 73.0% at 10 μg/mL. The nucleic acid and protein leakage reaches 124.8 μg/mL and 113.5 μg/mL. A spore mortality rate of 66.4% is arrived. Mitochondrial membrane potential reduces by 96% after treatment with 2 μg/mL. The CDC-F127-P shows a hemolysis rate of 1.8% and a tomato seed germination rate of 60% at 10 μg/mL. The contact angle on the tomato leaf is 74.0o. The liquid holding capacity is 27.5 mg/cm2 and the retention rats is 39.6% after simulated rainfall. The disease inhibition rates reach 64.9% and 71.0% in detached-leaf and potted-plant assays after treatment with 10 μg/mL CDC-F127-P. The triple-responsive CDC-F127-P nanopesticide offers a highly efficient and safe strategy for gray mold control and presents a novel approach for developing green nano-pesticides.
Homocysteine (Hcy), a critical biomarker implicated in over 100 clinical diseases, necessitates precise detection to enable early diagnosis and therapeutic intervention. MXene, known for its excellent electrochemical properties, is a promising material for constructing Hcy sensing platforms. However, its susceptibility to surface oxidation and tendency to restack significantly hinder its practical application in sensors. To address these limitations, we utilized a straightforward method for converting 2D MXene nanosheets directly into 3D carbon-coated MXene (MXene@C). The 3D architecture of MXene@C effectively prevents layer restacking, while the carbon coating enhances its oxidation resistance under ambient conditions. A novel electrochemical sensor for Hcy was fabricated using a composite material (Hemin/MXene@C), which synergistically combines the 3D conductive framework of MXene@C with the high catalytic activity of Hemin. The sensor demonstrated outstanding analytical performance for Hcy detection, with a broad linear range from 3.98 nM to 85.4 mu M and an ultralow detection limit of 1.33 nM. Notably, it exhibited excellent long-term stability, maintaining reliable performance for up to 15 days, attributable to the robust structural integrity of MXene@C. Furthermore, the sensor was successfully applied to detect Hcy in human serum samples with satisfactory results. The sensor demonstrates the potential of MXene@C for sensing applications and paves the way for innovative strategies in the early screening and clinical management of related disorders.
Homocysteine (Hcy) is a key biomarker for various diseases, and its precise detection is essential for early clinical diagnosis. Herein, an innovative ratiometric electrochemical aptasensor was constructed to overcome the limitations in sensitivity, selectivity, and stability in conventional Hcy detection methods. Firstly, we synthesized a novel 3D MXene/rGO aerogel loaded AuNPs composite (Au/MGA-40) with outstanding specific surface area and remarkable electrical conductivity. Next, the Hcy aptamer was self-assembled to the Au/MGA-40/MB modified electrode surface by gold sulfur bonds (Au-S). Finally, a ratiometric detection mode was established based on the linear relationship between the oxidation peak current ratios (IHcy/IMB) and the Hcy concentrations. The aptasensor exhibited excellent analytical behavior for Hcy, with a ultrawide detection range from 2.14 nM to 200 mu M and a detection limit as low as 0.835 nM. It also displayed remarkable selectivity due to the specific recognition between Hcy and the aptamer, enabling discrimination of Hcy from structurally similar molecules such as cysteine (Cys), glutathione (GSH) and methionine (Met). The ratio signal mode demonstrated superior long-term stability performance compared to conventional single signal sensors. As evidenced by the successful detection of Hcy in human serum, which underscores its potential for early screening of Hcy-related diseases.
Herein, trimethoprim-montmorillonite-polylactic acid microspheres are prepared by an intercalation-encapsulation method. The protection of montmorillonite prevents the degradation of trimethoprim (TMP) by gastric juice and improves the bioavailability of TMP. The TMP content in the microspheres is about 6
In this work, a heterostructure-based strategy is proposed to construct highly efficient electrocatalysts for the oxygen evolution reaction (OER) by coupling spinel NiCo2O4 with nitrogen-doped carbon fiber (NCF) substrates and further introducing partial sulfidation. Benefiting from the formation of a crystalline/amorphous NiCo2O4/ NiCo2S4 heterointerface and sulfur-induced electronic modulation, as well as the dandelion-like microspheres structure, the resulting NiCo2O4/NiCo2S4/NCF catalyst exhibited markedly enhanced OER activity and stability. Structural and spectroscopic analyses reveal that the synergistic interaction between the dual-phase heterostructure and the conductive NCF substrate effectively increases active site exposure, optimizes the adsorption behavior of OER intermediates, and accelerates charge-transfer kinetics, the superhydrophilicity and superaerophobicity greatly enhance electrolyte wetting of the catalyst and facilitate bubble detachment. These features collectively contribute to the superior catalytic performance. This work provides valuable insights into the rational design of advanced electrocatalysts for overall water splitting.
A salamo-based bicompartmental ligand H4L was successfully prepared, which self-assembled with copper(II) and nickel(II) salts in stoichiometric ratios of 1:2 to construct polynuclear copper(II) and nickel(II) complexes: [Cu2(HL)(NO3)(H2O)] (1) and [Ni4(mu-HL)2(mu-OAc)2]& sdot;2CH3COCH3 (2). Complex 1 contains one partially deprotonated (HL)3- part, two copper(II) atoms, one coordinated monodentate nitrate ion and one coordinated water molecule. Each copper(II) center is located in the geometric structure of square pyramidal. While complex 2 is composed of four nickel(II) atoms, two ligand (HL)3- parts, and two bridging mu-OAc- anions. The differently structural complexes acquired may be attributed to the different solvents and anions used in the synthesis process. Whether or not 3-hydroxyl group of salicylaldehyde unit in H4L is involved in the coordination further influences the diversification of the structures of the complexes. The reaction sites and intermolecular interactions were further evaluated by MEPs, IRI, Hirshfeld surface and finally the fluorescence properties were explored.
Developing intelligent and responsive antimicrobial materials is critically important for the sustainable advancement of livestock production. This study prepares a glutathione-responsive mPEG-SS-florfenicol conjugate using disulfide bonds as a linker. A non-responsive conjugate is also synthesized using an alkyl carbon chain as a linker. The structures of both conjugates are characterized through various analytical techniques, including MALDI-TOF MS. The self-assembled microstructures of the responsive and non-responsive conjugates are spherical and lamellar, respectively. At a DTT concentration of 10 mM, 90 % of florfenicol is released from the responsive conjugate within 10 h. The antibacterial activity of the responsive conjugate is 1.6 times greater than that of pure florfenicol at a concentration of 64 mu g/mL. At the same concentration, the uptake of the responsive conjugate by E. coli is ten times higher than that of the non-responsive conjugate. Compared with the non-responsive conjugate, the responsive conjugate induces more pronounced damage to the bacterial cell membrane. Molecular dynamics simulations confirm that the responsive conjugate binds to bacterial membranes more rapidly and with lower binding energy. The elimination half-life, maximum concentration (Cmax), and area under the curve of the responsive conjugate are 1.3, 1.7, and 2.4 times higher than those of commercial trimethoprim tablets, respectively.
A novel yet facile dual-channel salamo-type fluorescent probe NJS was synthesized successfully in this study. The probe NJS can efficiently detect B4O72− ions through colorimetric and fluorescent dual channels. Under sunlight, when B4O72− ionic solution was added to NJS solution, the mixed solution became a distinct yellow color, in sharp contrast to other anions. The fluorescence detection results showed that fluorescence strength of probe NJS is increased in a short time with the increasement of B4O72− ion content. In addition, the detection limit LOD of probe NJS for B4O72− ions was 2.81 × 10−8 M and the binding constant Ka was 2.20 × 104 M−1 by fluorescence titration. According to nuclear magnetic titration and relevant DFT calculations, it was speculated that after adding B4O72− ions into the probe solution, the probe NJS is deprotonated, triggering ICT and FRET effect, resulting in an increase of fluorescence intensity accompanied by redshift, and achieving the specific recognition of B4O72− ions by probe NJS. Finally, the practical application of probe NJS was studied. It was found that the probe can be used for qualitative and quantitative analysis of B4O72− ions through swab, paper test and actual water sample experiments.
Trichothecium roseum is an important postharvest pathogen that causes core rot in apples and contaminates apple juice with spores. Contact glow discharge electrolysis (CGDE) is an innovative non-thermal technique for microbial control in fresh produce, but its efficiency against T. roseum spores in apple juice and the underlying mechanism remain unclear. This study evaluated the inactivation efficiency of T. roseum spores in apple juice under different CGDE treatments and investigated the underlying mechanisms. The results showed that spore inactivation efficiency increased with the prolongation of the treatment time, reaching a reduction of 3.97 log units after 30 min. Spore inactivation followed a log-linear model. Mechanistic analysis revealed that CGDE treatment reduced the activity of antioxidant enzymes, including superoxide dismutase (SOD), catalase (CAT), peroxidase (POD) and ascorbate peroxidase (APX), leading to the accumulation of reactive oxygen species (ROS). This oxidative stress caused lipid peroxidation, reducing the unsaturated fatty acid and ergosterol content of cell membranes and producing malondialdehyde. Damage to spore cell membranes resulted in leakage of cellular contents, structural changes and damage to surface morphology. In conclusion, CGDE effectively inactivated T. roseum spores in apple juice by disrupting cell membrane integrity through ROS generation, highlighting its potential as a non-thermal microbial control method for postharvest applications.
The development of stimulus-responsive nanopesticide carriers has practical significance for improving drug utilization efficiency and reducing side effects. Herein, pH and glutathione-responsive cinnamaldehyde dimer liposome (CDC-d) is facilely fabricated via a one-step process. Carvacrol (CAR) or tebuconazole (TEB) is embedded into the liposome to obtain drug-loading nanoparticle using a simple antisolvent precipitation method. The morphology, antifungal properties, and biosafety of drug-loading nanoparticles are investigated in detail. CDC-d, CDC-d/TEB, and CDC-d/CAR present spherical particles with sizes ranging from 100 to 300 nm. The loading contents of CAR and TEB are 30.2 and 25.6%, respectively. The cumulative release rates of TEB and CAR reaches 100% and 85% after 30 min in a solution with pH of 5. The values are 40% and 60% in a 20 mM GSH solution after 30 min. The drug-loaded nanoparticles exhibit an effective antifungal activity against Fusarium oxysporum. They also show excellent wettability, adhesion, and rain erosion resistance on wheat leaves. Furthermore, this system has good biological safety for nontarget organisms. The cinnamaldehyde liposomes are expected to be outstanding pesticide delivery vesicles to use for the prevention and control of various crop diseases and pests.
Multi-component active ingredient delivery systems based on co-assembly have the merits of reducing drug dosage, attenuating pest resistance, enhancing ingredient utilization, broadening the control range, etc. and present excellent application prospects. Herein, a carrier-free co-assembled nanopesticide based on two first-line pesticides, abamectin B1a and imidacloprid, is successfully fabricated by a straightforward nanoprecipitation technique alone. NMR, UV-vis titration and molecular dynamics simulations reveal that intermolecular hydrogen bonding and van der Waals forces are the key driving forces for their binding. Less frequently encountered pi-alkyl forces also prevail in the co-assembled systems. The co-assembled nanopesticide presents a structured spherical shape with a size of similar to 200 nm. Soil permeability and UV degradation resistance are significantly higher than those of the two pure components. The surface of Ditylenchus destructor Thorne (D. destructor) treated with the nanoparticles becomes smooth, and the roughness is significantly lower than that of the control group. The activity of acetylcholinesterase (AchE) in vivo is significantly lower than that in the treatment group alone. AVM@IMI is also shown to have a better biosafety profile than commercial preparations. This strategy is expected to achieve efficient control of D. destructor and allow the green and sustainable development of agricultural controls.
The infection caused by Fusarium oxysporum severely threatens cotton production. Herein, carvacrol-chitosan nanoparticles (CS@CAR) are facilely fabricated using tripolyphosphate as a crosslinker. When the initial mass ratio of chitosan to carvacrol is 1:0.4, the nanoparticles show the best stability and drug loading. Morphological analysis reveals that the CS@CAR nanoparticles possesses a uniform spherical structure with an average diameter of approximately 150 nm. About 51.23 % of total CAR is released within the 48 h in the simulated fungal infection environment. The contact angle of drug-loaded particles decreases by 12.2 and 6.6 degrees compares with that of pure water and unloaded particles. The fluorescence intensity of leaves before and after rain erosion is 1.3 times and 1.2 times that of the pure water control group by fluorescence imaging analysis. The bacteriostatic activity of drug-loaded nanoparticles is 6-7 times that of non-drug-loaded nanoparticles. The contents of nucleic acid, protein, and malondialdehyde leaked by spores after treatment with drug-loaded particles are 1.4, 1.5 and 2.3 times those in the non-drug-loaded particle treatment group, respectively. The CS@CAR entirely prevents Fusarium oxysporum from infecting cotton leaves in spore inoculation experiments. The CS@CAR nanoparticles are expected to be used to prevent and control the infection of Fusarium oxysporum on cotton.
In this work, a double-armed salamo-based ligand H2L1 modified by pyridine ring was synthesized. It was found that the cyclic salamo-based compound H2L2 and binuclear Zn(II) complex [Zn-2(L-3)(H2O)(2)](NO3)(2)are formed on the basis of X-ray single crystal diffraction. They are obtained separately by the reactions of H(2)L(1 )with Sr(OAc)(2) and Zn(NO3)(2)& sdot;6H(2)O in different organic solutions. Interestingly, the compound H2L2 is formed by the cleavage and recombination of the ligand H2L1 catalyzed by Sr(OAc)(2), and is the first cyclic salamo-based compound. It was worth noting, in the process of forming Zn(II) complex, the ligand H2L1 is hydrolyzed to H2L3, the formation of H2L3 is due to the hydrolysis and fracture of C=N double bonds, which reduces the original formyl groups and forms a new ligand H(2)L3 containing two exposed formyl groups. The specific coordination mode of the Zn(II) complex is that Zn-1 atom is located in O4 cavity, Zn-2 atom is located in N2O2 cavity of the ligand (L-3)(2- )unit, and two oxygen atoms on formyl groups reduced by the fracture of connecting arm also participate in coordination, and two phenoxy groups on the (L-3)(2)- unit are bridged with Zn(1 )and Zn-2 atoms at the same time. In addition, two water molecules on Zn1 and Zn-2 participate in the coordination, and the Zn(II) atoms form hexacoordinated octahedral configurations. Nitrate ions do not participate in coordination, and their main function are to maintain the charge balance of the complex. UV-Vis titration experiment showed that the binding ratio between the ligand and Zn(II) atoms is 1:2, which is in accordance with the result of X-ray single crystal structure. This shows that the coordination ratio in solution state and solid state is the same. The cyclic-salamo compound H2L2 and Zn(II) complex were analyzed by DFT and Hirshfeld surface analysis. Through the analysis of fluorescence titration spectra, it was found that compared with the ligand H2L1, the fluorescence intensity increases obviously after adding Sr2+ and Zn2+ ions respectively, and gradually increases with the increasement of ion concentration.
Assessment of antibacterial efficacy and pharmacokinetics of a poly(mPEG- b -PCEA)–trimethoprim conjugate.