Search Results (334)

The development of effective and trackable drug delivery systems remains a major challenge in anticancer therapy. In this study, we designed novel polysaccharide-based theranostic carriers using a yeast-shell (YC) framework, providing a biocompatible platform for intracellular drug delivery. For the first time, a chitosan–genipin bioconjugate was synthesized via a solvent-free, green mechanochemical method and applied as an outer coating to microcarriers encapsulating the anticancer drug 5-fluorouracil (5-FU) and the fluorescent dye phenosafranin. The resulting system enabled simultaneous fluorescence tracking and the controlled release of the chemotherapeutic agent. In vitro evaluation using the MDA-MB-231 triple-negative breast cancer cell line demonstrated that 5-FU retained its antiproliferative activity, while the carriers facilitate sustained intracellular delivery. These findings highlight the potential of YC-based polysaccharide carriers, surface- modified with chitosan–genipin to enhance hydrophilicity, as a versatile platform for anticancer therapy, combining biocompatibility, traceability, and controlled drug release. Full article

A comparative study on the effects of mechanical treatment by high-energy ball milling on talc (2:1 layered silicate) and kaolinite (1:1 layer silicate) was performed. Industrial samples of talc and kaolin were characterized by XRF, thermal analysis (DTA and TG), and XRD methods. The XRD analysis evidenced the destruction of the crystalline structures of both talc and kaolinite and accessory minerals in the samples, showing an increase in the amorphous phases and a progressive change to a more disordered structure. It was found that high-energy ball milling resulted in a reduction of 48% of talc at 4 h of grinding, and the reduction increased up to ~80% at 32 h. The mechanical treatment produced a decrease in initial kaolinite content by 25% after 4 h of grinding and a reduction of ~70% after 32 h. It was deduced by this analysis that the structure of kaolinite is more difficult to destroy by high-energy ball milling than the structure of talc under the same experimental milling conditions. The structural alterations in talc and kaolinite were anisotropic, with crystal degradation along [00l], and there was a progressive loss of long-range order; moreover, the crystal dimensions following the c-axis direction became too small to produce coherent diffraction. A decrease in crystal size (coherent diffraction microdomain) was observed by the mechanical treatment, with an increase in microstrains produced by high-energy ball milling. Thus, the crystal size decreased from 280 to 200 Å in talc (direction perpendicular to 002) and from 250 to 210 Å in kaolinite (direction perpendicular to 001) after 16 h of grinding, with an important reduction in crystal size up to a value of 138 Å but only in the case of kaolinite at 80 h of grinding, with talc completely amorphous to X-rays at the same grinding time. Microstrains followed an inverse evolution compared to the crystal size, with an increase in the values obtained by progressive grinding in both talc and kaolinite. The values of microstrains were found to be of the same order for talc and kaolinite, although they were relatively higher for talc since it is associated with a greater degree of structural alteration than kaolinite. The XRD results showed an inverse correlation between both parameters, with their relative values being higher for talc compared with kaolinite. The present study is of basic interest for further investigations into the effects of high-energy ball milling using talc and kaolin as raw materials with reduced particle size, for instance, in the ceramic and paper industries. Full article

In this Short Note type article, we report the synthesis of a new hybrid molecule, N-(3,4-dimethoxyphenethyl)-2-propylpentanamide, using a solvent-minimized mechanochemical method that provides a simple and efficient synthetic approach. The process achieved high yield. The compound was confirmed by melting-point analysis, ¹H and ¹³C NMR, IR spectroscopy, and mass spectrometry. Full article

Metal–organic frameworks (MOFs), a class of porous crystalline materials, consists of metal ions or clusters coordinated to organic linkers. The unique features of MOFs such as exceptionally high surface area, chemical versatility, and tunable porosity make them highly suitable for several applications, including gas storage, drug delivery, catalysis, and sensing. Various synthesis techniques, including solvothermal, hydrothermal, microwave-assisted, mechanochemical, electrochemical, and sonochemical methods, have been used for the fabrication of MOFs. The selection and optimization of synthesis technique significantly influence the fundamental framework structure, the existence of defects, the available active sites, and the effectiveness of MOFs in special applications. This study focuses on advances in MOF fabrication techniques and examines their role in tuning the key properties of MOFs for targeted applications. The insights of this work may guide researchers in selecting or designing appropriate fabrication strategies for application-specific development of MOFs. Full article

Background/Objectives: Cocrystallisation is a well-established path for altering the physicochemical properties and bioavailability of active pharmaceutical ingredients (APIs). A common side effect of anti-tubercular medicines is the depletion of group B vitamin reserves in TB patients. Co-administration of supplements such as pyridoxine (vitamin B₆) during TB therapy may be used to ameliorate the harmful side effects of vitamin B₆ deficiency. Methods: Mechanochemical grinding and solvent evaporation experiments using pyridoxine (PN) with 4-aminosalicylic acid (PAS) and separately with pyrazinecarboxylic acid (PCBA) were conducted. The bulk powder and crystal analysis was performed using FTIR, PXRD, DSC, TGA and SCXRD. Results: The isolation and characterization of two multicomponent salts containing pyridoxine, i.e., PN-PAS·H₂O and PN-PCBA, were completed. Mechanochemistry is an efficient method for the preparation of cocrystals. Conclusions: The drug–vitamin combinations may be useful for the development of new treatment regimens with potentially improved therapeutic outcomes and reduced adverse effects. Full article

In this research, Fe-P scaffolds were successfully fabricated by the powder metallurgy method for the first time, using NaCl as the space holder for bone tissue engineering applications, with apparent porosities of approximately 70%. The Fe₃P powder was successfully synthesized by the mechanochemical method under an argon atmosphere using an initial mixture of Fe and P powders. The XRD patterns show that Fe₃P was obtained after sintering the milled powders at 1000 °C. Fe, Fe₃P, and Fe-50 wt% Fe₃P composite scaffolds and bulk pellets were prepared by sintering the milled powder at 1000 °C. Furthermore, the mechanical properties (compression strength) and bioactivity of the Fe-P scaffolds were determined. According to the compression test results, the composite scaffold showed higher compressive strength, lower fracture strain, and higher elastic modulus than the Fe and Fe₃P scaffolds, indicating that adding Fe₃P to Fe improves the mechanical properties. Moreover, among the scaffolds prepared by sintering at 1000 °C, the Fe scaffold exhibited the highest corrosion rate compared to the Fe₃P and composite samples, while the corrosion resistance of the composite sample was 3 times higher than that of the Fe sample. The ICP analysis showed that the amount of Fe released from the bulk pellets during soaking in PBS solution after four weeks was 3220 μg/dL, 4003 μg/dL, and 4774 μg/dL for the composite, Fe₃P, and Fe samples, respectively. The composite sample showed the highest cell viability, while the Fe sample had the lowest. The compressive strength (12.62 MPa) and fracture strain (5.98%) of the porous sintered composite scaffold at 1000 °C were within the range of trabecular bone, while the compressive strength of the composite sample was 17 times higher than that of the Fe sample. Furthermore, the MTS test showed that all the samples had good viability, while the composite sample had the best cell viability. The scaffolds were not cytotoxic. It can be concluded that the mechanical and biological properties of the composite sample were superior to those of the Fe and Fe₃P samples and that it may be a promising candidate for bone tissue engineering applications, especially for trabecular bone replacement. Full article

Photocatalysis is a process in which a material utilizes light energy to degrade contaminants through oxidation reactions that decompose impurities upon contact with its surface. Titanium dioxide is one of the most widely used semiconductor materials due to its abundance, chemical stability, and non-toxicity. However, its relatively wide bandgap restricts its photocatalytic activity to the ultraviolet region of the solar spectrum, limiting its overall efficiency under natural sunlight. The incorporation of copper nanoparticles into the TiO₂ matrix enhances light absorption by extending its activity into the visible range, thereby improving its energy conversion efficiency. In this study, undoped and Cu-doped TiO₂ powders were synthesized using the mechanochemical method. The characteristics of the prepared photocatalyst material were determined by XRD, SEM, absorbance, and chemical analysis. XRD analysis showed the formation of TiO₂ in its anatase and rutile phases. Sphere-like shapes with a size of 100 nm were inferred from SEM images. The photocatalytic tests revealed that the Cu-doped TiO₂ nanoparticles exhibited high photocatalytic activity in degrading contaminated water. This enhancement can be attributed to the formation of oxygen vacancies, which promote the photodegradation of organic compounds. Full article

Owing to the substantial polarity difference and weak interfacial interaction, the large-scale application of fly ash (FA) in rubber materials still faces substantial challenges. To solve this issue, this study prepared a modified hybrid SSBR@FA filler through a solution mechanochemical reaction between solution-polymerized styrene-butadiene rubber (SSBR) and FA in a lab planetary ball mill. Fourier transform infrared spectroscopy (FTIR) and energy-dispersive spectroscopy (EDS) analyses demonstrated the in situ grafting-neutralization between the carboxyl in the SSBR chains and metal oxides in FA. Transmission electron microscopy (TEM) showed that surface-grafted SSBR formed a rubber-constrained layer on FA particle surfaces, which can reduce their surface energy and improve the wettability between FA and SBR matrix. Compared with the SBR vulcanizate, the mechanical properties, thermal conductivity, and flame-retardant properties of the SBR/SSBR@FA vulcanizates were obviously improved. This was because of the uniform distribution of FA and the improved interfacial interaction between FA and the rubber matrix. For example, the tensile strength, tear strength, and elongation at break increased by 66.3%, 52.9%, and 17.7%, respectively. This easy, efficient, and environmentally modified method for FA was expected offer a practical and creative solution for its application in rubber manufacturing. Full article

Background: gemcitabine is a cytidine analog and major anticancer drug functioning as an antimetabolite. However, its administration by systemic route is accompanied by “burst” and side effects. To limit this, drugs are encapsulated in matrices; metal–organic frameworks (MOFs) are coordination polymers with strong potential for drug encapsulation and delayed release. Methods: mechano-chemical synthesis of solid-state binary complex lag(CYCU-3)(Gem) is described from aluminum MOF (Al-MOF) CYCU-3 and gemcitabine free base (Gem). Synthesis is conducted by liquid-assisted grinding (LAG) with dimethyl sulfoxide (DMSO) followed by its outgassing. The alternative “dry” synthesis results in dry(CYCU-3)(Gem). Materials were characterized by FTIR spectroscopy and XRD, and delayed Gem release was tested to phosphate buffered saline (PBS) at 37 °C. The in vitro toxicity to pancreatic cancer PANC−1 and healthy cells hTERT−HPNE E6/E7/K−RasG12D was assessed by fluorometric assay. Results: in lag(CYCU-3)(Gem) interactions MOF-drug are via non-covalent bonds at O-H and COO⁻ groups of CYCU-3 as found by FTIR marker peak shifts and crystal structure is retained, while dry(CYCU-3)(Gem) shows significant amorphization and loss of functional groups. The lag(CYCU-3)(Gem) but not dry(CYCU-3)(Gem) shows delayed Gem release for 6000 min. The suppression of PANC−1 cells by lag(CYCU-3)(Gem) is time-dependent and it correlates with delayed Gem release. For the first time, a concept of ternary stoichiometric complex lag(CYCU-3)₁(Gem)₁(CIT)₂ is tested that also contains natural organic compound citronellol (CIT), and its structure, bonding and release of Gem are compared to those of binary complex. Bonding is at the O-H groups of CYCU-3 and this complex shows delayed Gem release. Conclusions: binary and ternary complexes of Gem with CYCU-3 yield delayed release and cytotoxicity. LAG is promising for synthesis of solid-state complexes of gemcitabine for delayed release and time-dependent suppression of cancer cells. Full article

A method for the mechanochemical CuAAC click reaction (Cu⁺-promoted azido–alkyne cycloaddition) in the presence of bronze powder/copper beads without the use of a pre-introduced catalyst and ligands with greener prospect is presented. A new type of tri-, tetra-, and penta-ethylene glycols (PEGs) α,ω-disubstituted with 4-(PAH)-1H-1,2,3-triazole moieties has been synthesized by means of solvent-free click reaction in the planetary ball-milling in absence of a pre-introduced Cu(I) catalyst. The reaction afforded the above-mentioned compounds at room temperature in as short as 3 h in up to 96% yields and with E-factor values as low as 0.38. For the comparison, some of the key compounds were obtained by the conventional click synthesis in DMF solution. The compounds obtained were synthesized for the first time and can be considered as representative examples of bola-type chemosensors for the detection of electron-deficient species. This work presents a method for catalyzing a click reaction using bronze microparticles that are formed in situ during powder milling. This heterophase catalyst has been shown to be efficient and inexpensive and is suitable for green chemistry methods under solvent-free ball-milling conditions. Full article

ZnO semiconductor-based photocatalysts are mainly studied for the elimination of toxic textile dyes. Metal-doped ZnO displays better performance for this purpose. Herein, Al-doped ZnO (Al–ZnO) was prepared using the mechanochemical calcination method with varying aluminum concentrations for the degradation of the persistent methylene blue (MB) dye. Various characterization techniques, including XRD, FTIR, FESEM, TEM, UV-DRS, and XPS, revealed the improved properties of 3% Al–ZnO in degrading the MB dye. It exhibits 96.56% degradation of 25 mg/L MB dye under 60 min of natural sunlight irradiation with a catalyst dose of 0.5 g/L at a natural pH of 6.4. A smaller particle size, a lower band gap energy of 3.264 eV, and the presence of oxygen vacancies and defect states all facilitate photocatalytic degradation. Radical scavenger experiments using ascorbic acid (for •O₂⁻), 2-propanol (for •OH), and diammonium oxalate (for h⁺) confirmed the crucial role of superoxide (•O₂⁻) and hydroxyl (•OH) radicals in the degradation mechanism. The achievement of 82.80% MB degradation efficiency at the 4th cycle validates the notable stability and excellent reusability of Al–ZnO. Full article

Magnesium aluminate spinel nanoparticles (MgAl₂O₄-S-NPs) represent a promising class of nanoceramics with potential biomedical applications due to their physicochemical stability and antimicrobial properties. This study aimed to determine the structural characteristics, composition, and biological performance of MgAl₂O₄ spinel nanoparticles that were synthesized via a mechanochemical method. Structural and compositional characterization was performed using X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HR-TEM). Antibacterial activity was evaluated against Helicobacter pylori and Enterococcus faecalis using bacterial viability assays. Structural and morphological analyses confirmed the successful formation of single-phase cubic MgAl₂O₄ with a polyhedral morphology and nanoscale size distribution. Bacterial viability was quantified through optical density measurements following exposure to MgAl₂O₄-S-NPs at different concentrations. The nanoparticles exhibited both bacteriostatic and bactericidal effects, with activity being demonstrated against the tested bacterial strains. Mechanochemically synthesized MgAl₂O₄-S-NPs are promising candidates for biomedical applications, including dental materials, antimicrobial coatings, and infection-control strategies. Overall, the findings highlight the potential of MgAl₂O₄-S-NPs as effective antimicrobial agents that can be produced through an environmentally friendly synthesis route. Full article

Cu₂ZnSnSe₄ is a promising light-absorbing material for cost-effective and eco-friendly thin-film solar cells; however, its synthesis often leads to secondary phases that limit device efficiency. To overcome these challenges, we devised a straightforward and efficient method to obtain single-phase Cu₂ZnSnSe₄ nanocrystalline powders directly from the elements Cu, Zn, Sn, and Se via mechanochemical synthesis followed by vacuum annealing at 450 °C. Phase evolution monitored by X-ray diffraction (XRD) and Raman spectroscopy at two-hour milling intervals confirmed the formation of phase-pure kesterite Cu₂ZnSnSe₄ and enabled tracking of transient secondary phases. Raman spectra revealed the characteristic A₁ vibrational modes of the kesterite structure, while XRD peaks and Rietveld refinement (χ² ~ 1) validated single-phase formation with crystallite sizes of 10–15 nm and dislocation densities of 3.00–3.20 10¹⁵ lines/m². Optical analysis showed a direct bandgap of ~1.1 eV, and estimated linear and nonlinear optical constants validate its potential for photovoltaic applications. Scanning electron microscopy (SEM) analysis showed uniformly distributed particles 50–60 nm, and energy dispersive X-ray (EDS) analysis confirmed a near-stoichiometric Cu:Zn:Sn:Se ratio of 2:1:1:4. X-ray photoelectron spectroscopy (XPS) identified the expected oxidation states (Cu⁺, Zn²⁺, Sn⁴⁺, and Se²⁻). Electrical characterization revealed p-type conductivity with a mobility (μ) of 2.09 cm²/Vs, sheet resistance (ρ) of 4.87 Ω cm, and carrier concentrations of 1.23 × 10¹⁹ cm⁻³. Galvanostatic charge–discharge testing (GCD) demonstrated an energy density of 2.872 Wh/kg⁻¹ and a power density of 1083 W kg⁻¹, highlighting the material’s additional potential for energy storage applications. Full article

With the rapid increase in plastic consumption, waste polypropylene (WPP) has become one of the major components of municipal solid waste, posing significant environmental and resource challenges. According to statistics, polypropylene accounts for approximately 19.1% of the total global plastic waste, posing significant environmental challenges. In recent years, the recycling and reuse of WPP in asphalt pavement materials have received increasing attention due to its excellent mechanical properties, thermal stability, and low cost. This review systematically summarizes the physicochemical properties and recycling technologies of WPP, including mechanical, chemical, and energy recovery routes. Furthermore, the modification mechanisms, preparation methods, and performance characteristics of WPP-modified asphalt binders and mixtures are comprehensively discussed, focusing on their high-temperature stability, compatibility, low-temperature cracking resistance, and anti-moisture damage. Research indicates that WPP modification significantly enhances high-temperature rutting resistance, and thermo-chemical modifiers have successfully enabled the application of WPP in warm-mix asphalt. This review uniquely integrates recent advances in thermo-mechanochemical upcycling with mixture-level performance, bridging molecular design and field application. However, critical challenges, including poor compatibility, insufficient storage stability, and the lack of a unified assessment for the high variability of WPP raw materials, still need to be addressed. Finally, this review primarily focuses on the recycling technologies of WPP, its modification mechanisms in asphalt binders, and the resulting impact on the pavement performance of WPP-modified mixtures. Full article

This study evaluates the feasibility of achieving chemoselective aldol reactions over competing Henry reactions and employs competition experiments to establish proof of concept. A typical reaction involved using in-water reaction conditions where a concentrated organic layer containing an aldol nucleophile (1.5 equiv), a Henry nucleophile (1.5 equiv), an aldehyde electrophile (1.0 equiv), and a proline-based amino acid catalyst (2.5 mol%) constituted one phase, while the second phase was water (15 equiv). Highly enantioenriched aldol products were formed in practical yields, and a variety of Henry nucleophiles (nitroalkanes, allylic nitro compounds, and ethyl nitroacetate) were tolerated. This systematic examination of nitro compounds (pK_a 5.5–10.0) established a pK_a of ≈7.0 as the critical threshold at which nitronate formation results in Henry product formation under catalysis with 1. Reactions alternatively performed in MeOH/H₂O (3:2 equiv) solvent combinations, at times, provided improved chemoselectivity or product dr over the use of water (15 equiv) alone but required longer reaction times to produce similar yields. Reactions constrained by solubility were investigated using mechanochemical methods, but these conditions failed to deliver practical yields of either competition product. In summary, defining this category of aldol chemoselectivity may provide new tactical opportunities for the synthesis of complex molecular targets. Full article