Microwave-Assisted Silanization of Magnetite Nanoparticles Pre-Synthesized by a 3D Microfluidic Platform.

Magnetite nanoparticles (Fe3O4 NPs) are among the most investigated nanomaterials, being recognized for their biocompatibility, versatility, and strong magnetic properties. Given that their applicability depends on their dimensions, crystal morphology, and surface chemistry, Fe3O4 NPs must be synthesized in a controlled, simple, and reproducible manner. Since conventional methods often lack tight control over reaction parameters and produce materials with unreliable characteristics, increased scientific interest has been directed to microfluidic techniques. In this context, the present paper describes the development of an innovative 3D microfluidic platform suitable for synthesizing uniform Fe3O4 NPs with fine-tuned properties. On-chip co-precipitation was performed, followed by microwave-assisted silanization. The obtained nanoparticles were characterized from the compositional and microstructural perspectives by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Moreover, supplementary physicochemical investigations, such as Fourier Transform Infrared Spectroscopy (FT-IR), Kaiser Test, Ultraviolet-Visible (UV-Vis) Spectrophotometry, Dynamic Light Scattering (DLS), and Thermogravimetry and Differential Scanning Calorimetry (TG-DSC) analyses, demonstrated the successful surface modification. Considering the positive results, the presented synthesis and functionalization method represents a fast, reliable, and effective alternative for producing tailored magnetic nanoparticles.

Mesoporous Composite Bioactive Compound Delivery System for Wound-Healing Processes.

Currently, the treatment of wounds is still a challenge for healthcare professionals due to high complication incidences and social impacts, and the development of biocompatible and efficient medicines remains a goal. In this regard, mesoporous materials loaded with bioactive compounds from natural extracts have a high potential for wound treatment due to their nontoxicity, high loading capacity and slow drug release. MCM-41-type mesoporous material was synthesized by using sodium trisilicate as a silica source at room temperature and normal pressure. The synthesized mesoporous silica was characterized by using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), N2 absorption-desorption (BET), Dynamic Light Scattering (DLS) and Fourier transform infrared spectroscopy (FT-IR), revealing a high surface area (BET, 1244 m2/g); pore diameter of approx. 2 nm; and a homogenous, ordered and hexagonal geometry (TEM images). Qualitative monitoring of the desorption degree of the Salvia officinalis (SO) extract, rich in ursolic acid and oleanolic acid, and Calendula officinalis (CO) extract, rich in polyphenols and flavones, was performed via the continuous recording of the UV-VIS spectra at predetermined intervals. The active ingredients in the new composite MCM-41/sage and marigold (MCM-41/SO&CO) were quantified by using HPLC-DAD and LC-MS-MS techniques. The evaluation of the biological composites' activity on the wound site was performed on two cell lines, HS27 and HaCaT, naturally involved in tissue-regeneration processes. The experimental results revealed the ability to stimulate collagen biosynthesis, the enzymatic activity of the main metalloproteinases (MMP-2 and MMP-9) involved in tissue remodeling processes and the migration rate in the wound site, thus providing insights into the re-epithelializing properties of mesoporous composites.

Synergistic Antimicrobial Activity of Magnetite and Vancomycin-Loaded Mesoporous Silica Embedded in Alginate Films.

The aim of the present study was to obtain a hydrogel-based film as a carrier for the sustained and controlled release of vancomycin, an antibiotic commonly used in various types of infections. Considering the high-water solubility of vancomycin (>50 mg/mL) and the aqueous medium underlying the exudates, a prolonged release of vancomycin from an MCM-41 carrier was sought. The present work focused on the synthesis of malic acid coated magnetite (Fe3O4/malic) by co-precipitation, synthesis of MCM-41 by a sol-gel method and loading of MCM-41 with vancomycin, and their use in alginate films for wound dressing. The nanoparticles obtained were physically mixed and embedded in the alginate gel. Prior to incorporation, the nanoparticles were characterized by XRD, FT-IR and FT-Raman spectroscopy, TGA-DSC and DLS. The films were prepared by a simple casting method and were further cross-linked and examined for possible heterogeneities by means of FT-IR microscopy and SEM. The degree of swelling and the water vapor transmission rate were determined, considering their potential use as wound dressings. The obtained films show morpho-structural homogeneity, sustained release over 48 h and a strong synergistic enhancement of the antimicrobial activity as a consequence of the hybrid nature of these films. The antimicrobial efficacy was tested against S. aureus, two strains of E. faecalis (including vancomycin-resistant Enterococcus, VRE) and C. albicans. The incorporation of magnetite was also considered as an external triggering component in case the films were used as a magneto-responsive smart dressing to stimulate vancomycin diffusion.

Low Release Study of Cefotaxime by Functionalized Mesoporous Silica Nanomaterials.

As a third-generation ß-lactam antibiotic, cefotaxime shows a broad-spectrum with Gram-positive and Gram-negative bacteria activity and is included in WHO's essential drug list. In order to obtain new materials with sustained release properties, the present research focuses on the study of cefotaxime absorption and desorption from different functionalized mesoporous silica supports. The MCM-41-type nanostructured mesoporous silica support was synthesized by sol-gel technique using a tetraethyl orthosilicate (TEOS) route and cetyltrimethylammonium bromide (CTAB) as a surfactant, at room temperature and normal pressure. The obtained mesoporous material (MCM-41 class) was characterized through nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), N2 absorption-desorption (BET) and Fourier transform infrared spectroscopy (FT-IR), proving a good micro-structured homogeneity (SEM images), a high surface area (BET, 1029 m2/g) correlated with high silanolic activity (Q3/Q4 peak ratio from 29Si MAS-NMR), and an expected uniform hexagonal structure (2-3 nm, HRTEM). In order to non-destructively link the antibiotic compound on the solid phase, MCM-41 was further functionalized in two steps: with aminopropyl trimethoxysilane (APTMS) and glutaraldehyde (GA). Three cefotaxime-loaded materials were comparatively studied for low release capacity: the reference material with adsorbed cefotaxime on MCM-41, MCM-41/APS (aminopropyl silyl surface functionalization) adsorbed cefotaxime material, and APTMS-GA bounded MCM-41-cefotaxime material. The slow-release profiles were obtained by using an on-flow modified HPLC system. A significant improved release capacity was identified in the case of MCM-41/APS/GA-cefotaxime due to the covalent surface grafting of the biological active compound, recommending this class of materials as an effective carrier of bioactive compounds in wound dressing, anti-biofilm coatings, advanced drugs, and other related applications.

A Comparative Loading and Release Study of Vancomycin from a Green Mesoporous Silica.

Since its first use as a drug delivery system, mesoporous silica has proven to be a surprisingly efficient vehicle due to its porous structure. Unfortunately, most synthesis methods are based on using large amounts of surfactants, which are then removed by solvent extraction or heat treatment, leading to an undesired environmental impact because of the generated by-products. Hence, in the present study, we followed the synthesis of a silica material with a wormhole-like pore arrangement, using two FDA-approved substances as templates, namely Tween-20 and starch. As far as we know, it is the first study using the Tween-20/starch combo as a template for mesoporous silica synthesis. Furthermore, we investigated whether the obtained material using this novel synthesis had any potential in using it as a DDS. The material was further analyzed by XRD, TEM, FT-IR, N2 adsorption/desorption, and DLS to investigate its physicochemical features. Vancomycin was selected as the active molecule based on the extensive research engaged towards improving its bioavailability for oral delivery. The drug was loaded onto the material by using three different approaches, assuming its full retention in the final system. Thermal analysis confirmed the successful loading of vancomycin by all means, and pore volume significantly decreased upon loading, especially in the case of the vacuum-assisted method. All methods showed a slower release rate compared to the same amount of the pure drug. Loadings by physical mixing and solvent evaporation released the whole amount of the drug in 140 min, and the material loaded by the vacuum-assisted method released only 68.2% over the same period of time, leading us to conclude that vancomycin was adsorbed deeper inside the pores. The kinetic release of the three systems followed the Higuchi model for the samples loaded by physical mixing and vacuum-assisted procedures, while the solvent evaporation loading method was in compliance with the first-order model.

Microwave-Assisted Sol-Gel Preparation of the Nanostructured Magnetic System for Solid-Phase Synthesis.

This work describes a new synthesis method for core-shell magnetite nanoparticles with a secondary silica shell, functionalized with a linker system (Fe3O4-PABA-SiO2-linker) using a microwave-assisted heating technique. The functionalized solid nanomaterial was used for the nanophase synthesis of peptides (Fmoc route) as a solid support. The co-precipitation method was selected to obtain magnetite nanoparticles and sol-gel technique for silica coating using a microwave-assisted (MW) procedure. The magnetic properties of the nanoparticle core offer the advantage of a quick and easy alternative for the magnetic separation of the product from the reaction mixture, facilitating all the intermediary washing and separation operations. The intermediate and final materials were analyzed by advanced characterization methods. The effectiveness of the nanophase peptide synthesis using this nanostructured material as solid support was demonstrated for a short peptide sequence.

Sulpho-Salicylic Acid Grafted to Ferrite Nanoparticles for n-Type Organic Semiconductors.

A disadvantage of the use of pentacene and typical organic materials in electronics is that their precursors are toxic for manufacturers and the environment. To the best of our knowledge, this is the first report of an n-type non-toxic semiconductor for organic transistors that uses sulpho-salicylic acid-a stable, electron-donating compound with reduced toxicity-grafted on a ferrite core-shell and a green synthesis method. The micro-physical characterization indicated a good dispersion stability and homogeneity of the obtained nanofilms using the dip-coating technique. The in-situ electrical characterization was based on a point-contact transistor configuration, and the increase in the drain current as the positive gate voltage increased proved the functionality of the n-type semiconductor.

Functionalized magnetic nanoparticles for biomedical applications.

Functionalized magnetic nanoparticles followed two main directions in the field of biomedical applications: one direction is as image enhancing agents for magnetic resonance imaging (MRI) and the other is as drugdelivery devices for various biologically-active substances. A third field which just emerges in nanomedicine is the field of the so-called theranostic devices which combines in the same delivery vehicle both the therapeutic agent and the contrast substance. The advantages of using nanoparticles instead of larger carriers for delivery of both drug and image contrast enhancing agents will be highlighted throughout this review article. Despite the ever increasing number of articles reporting both in vitro and in vivo studies carried out on functionalized magnetic nanoparticles and envisaging their potential biomedical applications, only few formulations reached the phase of clinical trials and even fewer became marketed products. The perspectives in the field are open, since new drugs require new delivery devices and possibly new means of functionalization. At the same time, the field of nanomedicine also provides the opportunity to better exploit drugs that are already in clinical use by improving their bioavailability through appropriate nanoformulations.