Theranostics Using MCM-41-Based Mesoporous Silica Nanoparticles: Integrating Magnetic Resonance Imaging and Novel Chemotherapy for Breast Cancer Treatment.

Advanced breast cancer remains a significant oncological challenge, requiring new approaches to improve clinical outcomes. This study investigated an innovative theranostic agent using the MCM-41-NH2-DTPA-Gd3⁺-MIH nanomaterial, which combined MRI imaging for detection and a novel chemotherapy agent (MIH 2.4Bl) for treatment. The nanomaterial was based on the mesoporous silica type, MCM-41, and was optimized for drug delivery via functionalization with amine groups and conjugation with DTPA and complexation with Gd3+. MRI sensitivity was enhanced by using gadolinium-based contrast agents, which are crucial in identifying early neoplastic lesions. MIH 2.4Bl, with its unique mesoionic structure, allows effective interactions with biomolecules that facilitate its intracellular antitumoral activity. Physicochemical characterization confirmed the nanomaterial synthesis and effective drug incorporation, with 15% of MIH 2.4Bl being adsorbed. Drug release assays indicated that approximately 50% was released within 8 h. MRI phantom studies demonstrated the superior imaging capability of the nanomaterial, with a relaxivity significantly higher than that of the commercial agent Magnevist. In vitro cellular cytotoxicity assays, the effectiveness of the nanomaterial in killing MDA-MB-231 breast cancer cells was demonstrated at an EC50 concentration of 12.6 mg/mL compared to an EC50 concentration of 68.9 mg/mL in normal human mammary epithelial cells (HMECs). In vivo, MRI evaluation in a 4T1 syngeneic mouse model confirmed its efficacy as a contrast agent. This study highlighted the theranostic capabilities of MCM-41-NH2-DTPA-Gd3⁺-MIH and its potential to enhance breast cancer management.

Optimized Electrophoretic Deposition of Chitosan/Mesoporous Glass Nanoparticles with Gentamicin on Titanium Implants: Enhancing Hemocompatibility and Antibacterial Activity.

Titanium-based implants have long been studied and used for applications in bone tissue engineering, thanks to their outstanding mechanical properties and appropriate biocompatibility. However, many implants struggle with osseointegration and attachment and can be vulnerable to the development of infections. In this work, we have developed a composite coating via electrophoretic deposition, which is both bioactive and antibacterial. Mesoporous bioactive glass particles with gentamicin were electrophoretically deposited onto a titanium substrate. In order to validate the hypothesis that the quantity of particles in the coatings is sufficiently high and uniform in each deposition process, an easy-to-use image processing algorithm was designed to minimize human dependence and ensure reproducible results. The addition of loaded mesoporous particles did not affect the good adhesion of the coating to the substrate although roughness was clearly enhanced. After 7 days of immersion, the composite coatings were almost dissolved and released, but phosphate-related compounds started to nucleate at the surface. With a simple and low-cost technique like electrophoretic deposition, and optimized stir and suspension times, we were able to synthesize a hemocompatible coating that significantly improves the antibacterial activity when compared to the bare substrate for both Gram-positive and Gram-negative bacteria.

Tuning Textural Properties by Changing the Morphology of SBA-15 Mesoporous Materials.

Changing the morphology is an excellent option for altering the textural parameters of SBA-15 materials. This study provides a guide on how the properties of mesoporous structures behave according to their morphology and their contribution to thermal stability. The objective of this work was to synthesize different morphologies (spherical, hexagonal prisms, rice-like grains, rods, and fibers) of SBA-15 materials and evaluate the existing textural changes. The materials were synthesized by varying the temperature of the synthesis gel from 25 °C to 55 °C, with stirring at 300 or 500 rpm. The results of X-ray diffraction, Fourier transform infrared spectroscopy, N2 adsorption and desorption, and scanning electron microscopy were evaluated. Thermal stability tests were also conducted in an inert atmosphere. The materials were successfully synthesized, and it was observed that they all exhibited different characteristics, such as their ordering, interplanar distance, mesoporous parameter, specific surface area, micropore and mesopore volumes, external mesoporous area, and wall thickness. They also presented different thermal stabilities. The rice grain morphology had the highest specific surface area (908.8 cm2/g) and the best thermal stability, while the rod morphology had the best pore diameter (7.7 nm) and microporous volume (0.078 cm3/g).

Chlorin e6-Conjugated Mesoporous Titania Nanorods as Potential Nanoplatform for Photo-Chemotherapy.

Photodynamic therapy (PDT) has developed as an efficient strategy for cancer treatment. PDT involves the production of reactive oxygen species (ROS) by light irradiation after activating a photosensitizer (PS) in the presence of O2. PS-coupled nanomaterials offer additional advantages, as they can merge the effects of PDT with conventional enabling-combined photo-chemotherapeutics effects. In this work, mesoporous titania nanorods were surface-immobilized with Chlorin e6 (Ce6) conjugated through 3-(aminopropyl)-trimethoxysilane as a coupling agent. The mesoporous nanorods act as nano vehicles for doxorubicin delivery, and the Ce6 provides a visible light-responsive production of ROS to induce PDT. The nanomaterials were characterized by XRD, DRS, FTIR, TGA, N2 adsorption-desorption isotherms at 77 K, and TEM. The obtained materials were tested for their singlet oxygen and hydroxyl radical generation capacity using fluorescence assays. In vitro cell viability experiments with HeLa cells showed that the prepared materials are not cytotoxic in the dark, and that they exhibit photodynamic activity when irradiated with LED light (150 W m-2). Drug-loading experiments with doxorubicin (DOX) as a model chemotherapeutic drug showed that the nanostructures efficiently encapsulated DOX. The DOX-nanomaterial formulations show chemo-cytotoxic effects on Hela cells. Combined photo-chemotoxicity experiments show enhanced effects on HeLa cell viability, indicating that the conjugated nanorods are promising for use in combined therapy driven by LED light irradiation.

Application of Stemphylium lycopersici Extracts Immobilized on MCM-48type Mesoporous Materials as Biocatalysts for Monoacylglycerol Production.

Monoacylglycerols are eco-friendly and inexpensive emulsifiers with a range of applications. The traditional synthetic route is not eco-friendly, while enzymatic catalysis offers milder reaction conditions and higher selectivity. However, its application still is limited due to the costs. In this context, endophytic fungi can be source to new biocatalysts with enhanced catalytic activity. Based on this perspective, the aim of this study was perform the synthesis of MAG's through transesterification reactions of solketal and different vinyl esters, using crude and immobilized lipolytic extracts from the endophytic fungi Stemphylium lycopersici, isolated from Humiria balsamifera. The reactions were conducted using 100 mg of biocatalyst, 1 mmol of substrates, 9 : 1 n-heptane/acetone, at 40 °C, 200 rpm for 96 h. In the reactions using the ILE and stearate, laureate and decanoate vinyl esters it was possible to obtain the correspondent products with conversion rates of 52-75 %. Also, according to the structure drivers used in MCM-48 synthesis, different morphologies and conversions rates were observed. Employing [C16MI] Cl, [C14MI] Cl and [C4MI] Cl, the 1-lauroyl- glycerol conversion was 36 %, 79 % and 44 %, respectively. This is the first work involving the immobilization of an endophytic fungi and its utilization as a biocatalyst in the production of MAG's.

Effect of Amine, Carboxyl, or Thiol Functionalization of Mesoporous Silica Particles on Their Efficiency as a Quercetin Delivery System in Simulated Gastrointestinal Conditions.

Quercetin (Q) dietary supplements exhibit poor oral bioavailability because of degradation throughout gastrointestinal digestion (GD), which may be overcome using mesoporous silica particles (MSPs) as an oral delivery system (ODS). This study aimed to elucidate the effect of the functionalization of MSPs with amine-(A-MSP), carboxyl-(C-MSP), or thiol-(T-MSP) groups on their efficiency as a quercetin ODS (QODS). The type and degree of functionalization (DF) were used as factors in an experimental design. The Q-loaded F-MSP (F-MSP/Q) was characterized by gas physisorption analysis, loading capacity (LC), and dynamic light scattering and kinetics of Q release at gastric and intestinal pHs. Antioxidant capacity and Q concentration of media containing F-MSP/Q were evaluated after simulated GD. A-MSP showed the highest LC (19.79 ± 2.42%). C-MSP showed the lowest particle size at pH 1.5 or 7.4 (≈200 nm). T-MSP exhibited the maximum Q release at pH 7.4 (11.43%). High DF of A-MSP increased Q retention, regardless of pH. A-MSP preserved antioxidant capacity of Q-released gastric media (58.95 ± 3.34%). Nonetheless, MSP and F-MSP did not protect antioxidant properties of Q released in intestinal conditions. C-MSP and T-MSP showed essential features for cellular uptake and Q release within cells that need to be assessed.

Mesoporous Nitrogen-Doped Holey Reduced Graphene Oxide: Preparation, Purification, and Application for Metal-Free Electrochemical Sensing of Dopamine.

Holey graphenic nanomaterials with porosity within the basal plane attract significant interest. It is observed that the perforation of graphene can enhance the specific surface area of the nanosheet, ensuring effective wetting and penetration of electrolytes to the electrode surface, facilitating rapid charge transfer, and boosting the electrocatalytic efficacy of the transducers. This study reports the first example of nitrogen-doped holey reduced graphene oxide with a mesoporous morphology of the graphene basal plane (N-MHG). It is shown that N-MHG can be synthesized through a one-step hydrothermal treatment of GO using NH3 and H2O2. A straightforward procedure for the purification of N-MHG has also been developed. AFM, TEM, and Raman analyses have revealed that N-MHG possesses a highly mesoporous network structure with a pore size ranging from 10 to 50 nm. X-ray photoelectron spectroscopy data have indicated a partial reduction of the graphene oxide sheets during the etching process but also show a 3-5 times higher content of C═O and O-C═O fragments compared to rGO. This could account for the remarkable stability of the N-MHG aqueous suspension. An electrochemical sensor for dopamine analysis is assembled on a glassy carbon electrode with N-MHG/Nafion membrane and characterized by cyclic voltammetry and electrochemical impedance spectroscopy.

CO2 capture using silica-immobilized dicationic ionic liquids with magnetic and non-magnetic properties.

The need to find alternative materials to replace aqueous amine solutions for the capture of CO2 in post-combustion technologies is pressing. This study assesses the CO2 sorption capacity and CO2/N2 selectivity of three dicationic ionic liquids with distinct anions immobilized in commercial mesoporous silica support (SBA- 15). The samples were characterized by UART-FTIR, NMR, Raman, FESEM, TEM, TGA, Magnetometry (VSM), BET and BJH. The highest CO2 sorption capacity and CO2/N2 selectivity were obtained for sample SBA@DIL_2FeCl4 [at 1 bar and 25 °C; 57.31 (±0.02) mg CO2/g; 12.27 (±0.72) mg CO2/g]. The results were compared to pristine SBA-15 and revealed a similar sorption capacity, indicating that the IL has no impact on the CO2 sorption capacity of silica. On the other hand, selectivity was improved by approximately 3.8 times, demonstrating the affinity of the ionic liquid for the CO2 molecule. The material underwent multiple sorption/desorption cycles and proved to be stable and a promising option for use in industrial CO2 capture processes.

Morin loaded mesoporous molecular sieves as novel devices to the potential treatment of tumor pathologies.

Morin is an antioxidant and anticancer flavonoid, extracted from natural sources, that may exert beneficial effects for several pathologies. Despite this, the administration of morin represents a challenge due to its low aqueous solubility. Mesoporous silica materials have emerged as biocompatible tools for drug delivery, as their pore size can be modulated for maximum surface area to volume ratio. In this contribution, we evaluate the ability of iron-modified mesoporous materials, for morin loading and controlled delivery. The SBA-15 and MCM-41 sieves were synthesized and modified with iron (metal content 4.02 and 6.27 % wt, respectivily). Characterization by transmission electron microscopy, XRD and UV-Vis revealed adequate pore size and agglomerates of very small metallic nanospecies (nanoclusters), without larger iron oxide nanoparticles. FT-IR spectra confirmed the presence of silanol groups in the solid hosts, which can interact with different groups present in morin molecules. SBA-15 materials were more efficient in terms of morin loading capacity (LC) due to their larger pore diameter. LC was more than 35% for SBA-15 materials when adsorptions studies were carried out with 9 mg of drug. Antioxidant activity were assayed by using DPPH test. Free iron materials presented a significate improvement as antioxidants after morin incorporation, reaching a scavenging activity of almost a 90%. On the other hand, in iron modified mesoporous materials, the presence of morin did not affect the scavenging activity. The results could be related with the formation of a complex between the flavonoid and the iron. Finally, biosafety studies using normal epithelial cells revealed that neither the loaded nor the unloaded materials exerted toxicity, even at doses of 1 mg/ml. These findings expand knowledge about mesoporous materials as suitable carriers of flavonoids with the aim of improving therapies for a wide range of pathologies.

Advances in Nanomaterials and Composites Based on Mesoporous Materials as Antimicrobial Agents: Relevant Applications in Human Health.

Nanotechnology has emerged as a cornerstone in contemporary research, marked by the advent of advanced technologies aimed at nanoengineering materials with diverse applications, particularly to address challenges in human health. Among these challenges, antimicrobial resistance (AMR) has risen as a significant and pressing threat to public health, creating obstacles in preventing and treating persistent diseases. Despite efforts in recent decades to combat AMR, global trends indicate an ongoing and concerning increase in AMR. The primary contributors to the escalation of AMR are the misuse and overuse of various antimicrobial agents in healthcare settings. This has led to severe consequences not only in terms of compromised treatment outcomes but also in terms of substantial financial burdens. The economic impact of AMR is reflected in skyrocketing healthcare costs attributed to heightened hospital admissions and increased drug usage. To address this critical issue, it is imperative to implement effective strategies for antimicrobial therapies. This comprehensive review will explore the latest scientific breakthroughs within the metal-organic frameworks and the use of mesoporous metallic oxide derivates as antimicrobial agents. We will explore their biomedical applications in human health, shedding light on promising avenues for combating AMR. Finally, we will conclude the current state of research and offer perspectives on the future development of these nanomaterials in the ongoing battle against AMR.

Enhancing Osteoblastic Cell Cultures with Gelatin Methacryloyl, Bovine Lactoferrin, and Bioactive Mesoporous Glass Scaffolds Loaded with Distinct Parsley Extracts.

The increasing interest in innovative solutions for addressing bone defects has driven research into the use of Bioactive Mesoporous Glasses (MBGs). These materials, distinguished by their well-ordered mesoporous structure, possess the capability to accommodate plant extracts with well-established osteogenic properties, including bovine lactoferrin (bLF), as part of their 3D scaffold composition. This harmonizes seamlessly with the ongoing advancements in the field of biomedicine. In this study, we fabricated 3D scaffolds utilizing MBGs loaded with extracts from parsley leaves (PL) and embryogenic cultures (EC), rich in bioactive compounds such as apigenin and kaempferol, which hold potential benefits for bone metabolism. Gelatin Methacryloyl (GelMa) served as the polymer, and bLF was included in the formulation. Cytocompatibility, Runx2 gene expression, ALP enzyme activity, and biomineralization were assessed in preosteoblastic MC3T3-E1 cell cultures. MBGs effectively integrated PL and EC extracts with loadings between 22.6 ± 0.1 and 43.6 ± 0.3 µM for PL and 26.3 ± 0.3 and 46.8 ± 0.4 µM for EC, ensuring cell viability through a release percentage between 28.3% and 59.9%. The incorporation of bLF in the 3D scaffold formulation showed significant differences compared to the control in all assays, even at concentrations below 0.2 µM. Combinations, especially PL + bLF at 0.19 µM, demonstrated additive potential, with superior biomineralization compared to EC. In summary, this study highlights the effectiveness of MBGs in incorporating PL and EC extracts, along with bLF, into 3D scaffolds. The results underscore cytocompatibility, osteogenic activity, and biomineralization, offering exciting potential for future in vivo applications.

The role of water in reactions catalysed by hydrolases under conditions of molecular crowding.

Under macromolecular crowding (MC) conditions such as cellular, extracellular, food and other environments of biotechnological interest, the thermodynamic activity of the different macromolecules present in the system is several orders of magnitude higher than in dilute solutions. In this state, the diffusion rates are affected by the volume exclusion induced by the crowders. Immiscible liquid phases, which may arise in MC by liquid-liquid phase separation, may induce a dynamic confinement of reactants, products and/or enzymes, tuning reaction rates. In cellular environments and other crowding conditions, membranes and macromolecules provide, on the whole, large surfaces that can perturb the solvent, causing its immobilisation by adsorption in the short range and also affecting the solvent viscosity in the long range. The latter phenomenon can affect the conformation of a protein and/or the degree of association of its protomers and, consequently, its activity. Changes in the water structure can also alter the enzyme-substrate interaction, and, in the case of hydrolytic enzymes, where water is one of the substrates, it also affects the reaction mechanism. Here, we review the evidence for how macromolecular crowding affects the catalysis induced by hydrolytic enzymes, focusing on the structure and dynamics of water.

Effective intracellular release of ibuprofen triggered by thermosensitive magnetic nanocarriers.

Stimuli-responsive nanocarriers are being widely applied in the development of new strategies for the diagnosis and treatment of diseases. An inherent difficulty in general drug therapy is the lack of precision with respect to a specific pathological site, which can lead to toxicity, excessive drug consumption, or premature degradation. In this work, the controlled drug delivery is achieved by using magnetite nanoparticles coated with mesoporous silica with core-shell structure (MMS) and grafted with the thermoresponsive polymer poly [N-isopropylacrylamide-co-3-(trimethoxysilyl)propyl methacrylate] (MMS-P). The efficiency of MMS-P as a temperature-controlled drug delivery system was evaluated by in vitro release experiments using ibuprofen (IBU) in various mammalian cell models. Further, the effects of IBU as a photoprotectant in cells exposed to photodynamic therapy (PDT) in a carbaryl-induced neurodegenerative model were evaluated. The results showed that MMS-P nanocarriers do not exhibit cytotoxicity in HepG2 cells at high doses such as 7600 µg mL-1. Pre-incubation of MMS-P charged with IBU showed no effect on the PDT in N2A cells; however, it produced a further decrease in the viability of HepG2 cells, leading to a reduction to PDT resistance. On the other hand, a cytoprotective effect against carbaryl toxicity in N2A cells was observed in IBU administrated by MMS-P, which confirms the effective intracellular IBU uptake by means of MMS-P. These results encourage the potential application of MMS-P as a drug delivery system and confirm the effect of IBU as a cytoprotective agent in a neurodegenerative model.

Kinetics and Mechanism of Camptothecin Release from Transferrin-Gated Mesoporous Silica Nanoparticles through a pH-Responsive Surface Linker.

Stimuli-responsive nanomaterials have emerged as a promising strategy for inclusion in anticancer therapy. In particular, pH-responsive silica nanocarriers have been studied to provide controlled drug delivery in acidic tumor microenvironments. However, the intracellular microenvironment that the nanosystem must face has an impact on the anticancer effect; therefore, the design of the nanocarrier and the mechanisms that govern drug release play a crucial role in optimizing efficacy. Here, we synthesized and characterized mesoporous silica nanoparticles with transferrin conjugated on their surface via a pH-sensitive imine bond (MSN-Tf) to assess camptothecin (CPT) loading and release. The results showed that CPT-loaded MSN-Tf (MSN-Tf@CPT) had a size of ca. 90 nm, a zeta potential of -18.9 mV, and a loaded content of 13.4%. The release kinetic data best fit a first-order model, and the predominant mechanism was Fickian diffusion. Additionally, a three-parameter model demonstrated the drug-matrix interaction and impact of transferrin in controlling the release of CPT from the nanocarrier. Taken together, these results provide new insights into the behavior of a hydrophobic drug released from a pH-sensitive nanosystem.

Gold Nanorods with Mesoporous Silica Shell: A Promising Platform for Cisplatin Delivery.

The versatile combination of metal nanoparticles with chemotherapy agents makes designing multifunctional drug delivery systems attractive. In this work, we reported cisplatin's encapsulation and release profile using a mesoporous silica-coated gold nanorods system. Gold nanorods were synthesized by an acidic seed-mediated method in the presence of cetyltrimethylammonium bromide surfactant, and the silica-coated state was obtained by modified Stöber method. The silica shell was modified first with 3-aminopropyltriethoxysilane and then with succinic anhydride to obtain carboxylates groups to improve cisplatin encapsulation. Gold nanorods with an aspect ratio of 3.2 and silica shell thickness of 14.74 nm were obtained, and infrared spectroscopy and ζ potential studies corroborated surface modification with carboxylates groups. On the other hand, cisplatin was encapsulated under optimal conditions with an efficiency of ~58%, and it was released in a controlled manner over 96 h. Furthermore, acidic pH promoted a faster release of 72% cisplatin encapsulated compared to 51% in neutral pH.

Immobilized mesoporous materials for carvacrol delivery to the germination and early growth of tomato plants (Solanum Lycopersicum).

The immobilization of TiO2-SiO2 (TSO) materials on seed mats stands as a practical way to help the germination and early growth of tomato plants (Solanum Lycopersicum). Mesoporous materials are functionalized with triethanolamine (TEA) and loaded with the biocide molecule of carvacrol (CAR). The effect of CAR on the parameters of germination percentage, germination time, root, shoot length, and chlorophyll content of seeds and/or tomato seedlings are investigated. The germination experiments were carried out using seed mats coated with the TSO materials, also TSO powdered materials were put directly on the tomato seeds to study their effect on germination. Direct deposition of TSO composites achieved the complete germination and longer shoots due to the cooperative interactions among nanomaterials, carvacrol, and the tomato seed. However, the handling of the seeds and the detrimental effect of powder in the germination system made difficult the application with agricultural purposes. The plastic seed mats provide a practical system with lower germination, but more homogenous growth of root/shoot is possible. Surprisingly, in this methodology the carvacrol presents a detrimental effect on germination due to less interaction with the seeds. The handling of seeds and recover of the nanomaterials and its reuse are advantages of the plastic seed mats, which together with less wastage of seeds suggest a potential use in agriculture. The as-synthetized TSO NPs, together with the functionalization of triethanolamine and carvacrol used to promote the health germination of the seeds, allows the control of the time for seed germination, germination %, and length for the root/shoot of seed tomato germination. The immobilization of mesoporous materials results in an alternative to help the germination and early growth of agricultural plants searching to avoid the lixiviation of nanomaterials to the environment.

Comparative effect of mesoporous carbon doping on the adsorption of pharmaceutical drugs in water: Theoretical calculations and mechanism study.

In this study, mesoporous doped-carbons were synthesized from sucrose, a natural source, boric acid and cyanamide as precursors, generating B- or N-doped carbon. These materials were characterized by FTIR, XRD, TGA, Raman, SEM, TEM, BET, and XPS, confirming the preparation of a tridimensional doped porous structure. B-MPC and N-MPC showed a high surface specific area above 1000 m2/g. The effect of B and N doping on mesoporous carbon was evaluated on the adsorption of emerging pollutants from water. Diclofenac sodium and paracetamol were used in adsorption assays, reaching removal capacities of 78 and 101 mg.g-1, respectively. Kinetic and isothermal studies indicate the chemical nature of adsorption controlled by external and intraparticle diffusion and multilayer formation due to strong adsorbent/adsorbate interactions. DFT-based calculations and adsorption assays infer that the main attractive forces are hydrogen bonds and Lewis acid-base interactions.

Cinnamon Oil Encapsulated with Silica Nanoparticles: Chemical Characterization and Evaluation of Insecticidal Activity Against the Rice Moth, Corcyra cephalonica.

Cinnamon (Cinnamomum zeylanicum Blume) essential oil has vast potential as an antimicrobial but is limited by its volatility and rapid degradation. To decrease its volatility and prolong the efficacy of the biocide, cinnamon essential oil was encapsulated into mesoporous silica nanoparticles (MSNs). The characterization of MSNs and cinnamon oil encapsulated with silica nanoparticles (CESNs) was estimated. Additionally, their insecticidal activity against the rice moth Corcyra cephalonica (Stainton) larvae was evaluated. The MSN surface area decreased from 893.6 to 720 m2 g-1 and the pore volume also decreased from 0.824 to 0.7275 cc/g after loading with cinnamon oil. X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX), and N2 sorption by Brunauer-Emmett-Teller (BET) confirmed the successful formation and evolution of the synthesized MSNs and CESN structures. The surface characteristics of MSNs and CESNs were analyzed by scanning and transmission electron microscopy. Compared with the sub-lethal activity values, the order of toxicity after 6 days of exposure was MSNs ˃ CESN ˃ cinnamon oil ˃ silica gel ˃ peppermint oil. The efficacy of CESNs gradually increases its toxicity more than MSN after the 9th day of exposure.

Hierarchical Biobased Macroporous/Mesoporous Carbon: Fabrication, Characterization and Electrochemical/Ion Exchange Properties.

With the goal of improving the mechanical properties of porous hierarchical carbon, cellulosic fiber fabric was incorporated into the resorcinol/formaldehyde (RF) precursor resins. The composites were carbonized in an inert atmosphere, and the carbonization process was monitored by TGA/MS. The mechanical properties, evaluated by nanoindentation, show an increase in the elastic modulus due to the reinforcing effect of the carbonized fiber fabric. It was found that the adsorption of the RF resin precursor onto the fabric stabilizes its porosity (micro and mesopores) during drying while incorporating macropores. The textural properties are evaluated by N2 adsorption isotherm, which shows a surface area (BET) of 558 m2g-1. The electrochemical properties of the porous carbon are evaluated by cyclic voltammetry (CV), chronocoulometry (CC), and electrochemical impedance spectroscopy (EIS). Specific capacitances (in 1 M H2SO4) of up to 182 Fg-1 (CV) and 160 Fg-1 (EIS) are measured. The potential-driven ion exchange was evaluated using Probe Bean Deflection techniques. It is observed that ions (protons) are expulsed upon oxidation in acid media by the oxidation of hydroquinone moieties present on the carbon surface. In neutral media, when the potential is varied from values negative to positive of the potential of zero charge, cation release, followed by anion insertion, is found.

A mechanothermal approach for the synthesis of Fe3O4 nanoparticles as dopant on mesoporous TiO2 for electrochemical determination of catechol.

The subject of water contamination and how it gets defiled to the society and humans is confabulating from the past decades. Phenolic compounds widely exist in the water sources and it is emergent to determine the toxicity in natural and drinking water, because it is hazardous to the humans. Among these compounds, catechol has sought a strong concern because of its rapid occurrence in nature and its potential toxicity to humans. The present work aims to develop an effective electrochemical sensing of catechol using mesoporous structure of Fe3O4-TiO2 decorated on glassy carbon (GC) electrode. The creation of pure TiO2 using the sol-gel technique was the first step in the synthesis protocol for binary nanocomposite, which was then followed by the loading of Fe3O4 nanoparticles on the surface of TiO2 using the thermal decomposition method. The resultant Fe3O4-TiO2 based nanocomposite exhibited mesoporous structure and the cavities were occupied with highly active magnetite nanoparticles (Fe3O4) with high specific surface area (90.63 m2/g). When compared to pure TiO2, catechol showed a more prominent electrochemical response for Fe3O4-TiO2, with a significant increase in anodic peak current at a lower oxidation potential (0.387 V) with a detection limit of 45 µM. Therefore, the prepared magnetite binary nanocomposite can serve as an efficient electroactive material for sensing of catechol, which could also act as a promising electrocatalyst for various electrocatalytic applications.