Search Results (21)

The development and application of antimicrobial coatings has become increasingly important in both medical and industrial settings due to the rising threat of microbial contamination and antibiotic resistance. This paper focuses on the formulation, characterization, and investigation of coatings based on quaternized polysulfone, which are designed to encapsulate two broad-spectrum antimicrobial drugs with complementary activity, amphotericin B (AmB) and norfloxacin (NFX), with the primary aim of inhibiting pathogen colonization on surgical instruments. Structural characterization using FTIR, ¹H-NMR, and UV-Vis spectroscopy, along with supramolecular analysis via X-ray diffraction and polarized optical microscopy (POM), revealed strong physical interactions between the drugs and the quaternized polysulfone matrix. Scanning electron microscopy (SEM) confirmed a uniform distribution of the antimicrobial agents within the polymeric matrix. Surface wettability, assessed through water contact angle measurements, indicated moderate hydrophilicity (70–90°). The coatings also exhibited notable antioxidant activity, showing a 12-fold increase in DPPH radical inhibition compared to the control. Furthermore, all formulations demonstrated strong antimicrobial efficacy against three reference strains frequently associated with hospital-acquired infections, S. aureus, E. coli, and C. albicans, with inhibition zones ranging from 32 to 39.67 mm for bacterial strains and 13.86 to 20.86 mm for C. albicans. These data points indicate that these materials may be useful as antimicrobial coatings. Full article

The stability of cement slurries under high-temperature conditions poses a significant engineering challenge in cementing operations. This study explored the development of a novel tetrameric thermosensitive thickening polymer (TTSTC) as a solution to this problem. Aqueous free radical polymerization was employed to synthesize the polymer. The base monomers 2-acrylamido-2-methylpropanesulfonic acid (AMPS) and acrylamide (AM) were employed, in conjunction with the long-chain thermosensitive monomers octadecyldimethylallylammonium chloride (C18DMAAC) and N-vinylpyrrolidone (NVP). The optimal synthesis conditions were determined by orthogonal experiments as follows: monomer molar ratio (AM:AMPS:C18DMAAC:NVP) = 15:10:5:5, initiator concentration of 16 wt%, cross-linker concentration of 0.45 wt%, pH 6, and polymerization temperature of 60 °C. The chemical structure of TTSTC was characterized by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance (1H-NMR), gel permeation chromatography, scanning electron microscopy, Zeta potential, and particle size measurement. The results verified the successful synthesis of the target polymer. Its thermal stability, thermosensitive thickening behavior, and salinity resistance were systematically investigated. Furthermore, the impact of TTSTC on the settling stability, rheological characteristics, and compressive strength of cement paste was assessed. The experimental findings demonstrated that TTSTC displayed noteworthy thermosensitive thickening properties at temperatures up to 279 °C, pH values ranging from 11 to 13, and NaCl/CaCl₂ concentrations between 0.05 and 0.5 g/L. The optimal performance of TTSTC was observed at mass fractions ranging from 0.6 to 0.8 wt%. When incorporated into the slurry at 0.6–1.0 wt%, TTSTC significantly improved the slurry settling stability, thickening properties, and 28d compressive strength at elevated temperatures compared with the control. When comparing the temperature-sensitive thickening performance of the newly developed treatment agent with that of the commercially available xanthan gum thickener, the results showed that for the cement slurry system containing the new treatment agent at a mass fraction of 0.6%, the reduction in consistency was 30.9% less than that of the cement slurry system with xanthan gum at a mass fraction of 0.6%. These findings indicate that TTSTC has the potential to function as a highly effective additive in cementing operations conducted in extreme environments, thereby enhancing the stability and dependability of such operations. Full article

This study investigates the stability and application of trithiocarbonate-based chain transfer agents (CTAs) in reversible addition–fragmentation chain transfer (RAFT) radical polymerization under harsh conditions. We evaluated the stability of 4-cyano-4-(2-carboxyethylthiothioxomethylthio) pentanoic acid (Rtt-17) and 4-cyano-4-(dodecylsulfanylthiocarbonyl) sulfanylpentanoic acid (Rtt-05) at 60 °C under basic conditions using ¹H NMR and UV–vis absorption spectra, showing that Rtt-05 is more stable than Rtt-17. The greater stability of Rtt-05 is attributed to the hydrophobic dodecyl group, which allows it to form micelles in water, thereby protecting the trithiocarbonate group from the surrounding aqueous phase. In contrast, hydrophilic Rtt-17, without long alkyl chains, cannot form micelles in water. Following the stability assessment, Rtt-17 and Rtt-05 were employed for RAFT polymerization of hydrophilic monomers, such as N,N-dimethylacrylamide (DMA) and 2-(methacryloyloxy)ethyl phosphorylcholine (MPC). DMA can dissolve in both water and organic solvents, and MPC can dissolve in water and polar solvents. Both CTAs successfully controlled the polymerization of DMA, producing polymers with narrow molecular weight distributions (M_w/M_n) less than 1.2. Also, Rtt-17 demonstrated effective control of MPC polymerization, yielding M_w/M_n values of around 1.2. However, during the polymerization of MPC, Rtt-05 failed to maintain control, resulting in a broad M_w/M_n (≥1.9). The inability of Rtt-05 to control MPC polymerization is due to the formation of micelles, which disrupts the interaction between the hydrophilic MPC propagating radicals and the trithiocarbonate group in the hydrophobic core of Rtt-05 micelles. The findings provide critical insights into designing CTAs for specific applications, particularly for biomedical and industrial uses of hydrophilic polymers, highlighting the potential for precise molecular weight control and tailored polymer properties. Full article

Smart materials for drug delivery are designed to offer a precise and controlled release of therapeutic agents. By responding to specific physiological stimuli, such as changes in temperature and pH, these materials improve treatment efficacy and minimize side effects, paving the way for personalized therapeutic solutions. In this study, we present the fabrication of dual-responsive alginate/poly(N-isopropylacrylamide) (PNIPAM) microspheres, having the ability to respond to both pH and temperature variations and embedding the lipophilic bioactive compound Ozoile. Ozoile^® Stable Ozonides is obtained from extra virgin olive oil and acts as an inducer, interacting with major biological pathways by means of modulating the systemic redox balance. The dual-responsive microspheres are prepared by electrospray technique without the use of organic solvents. PNIPAM is synthesized by radical polymerization using the APS/TEMED redox initiators. The microspheres are further optimized with a chitosan coating to enhance their stability and modulate the degradation kinetics of the gel matrix. A comprehensive morphological analysis, Fourier transform infrared (FTIR) spectroscopy, and degradation assays are conducted to confirm the structural stability and pH-responsive behavior of the hydrogel microspheres. A study of the volume phase transition temperature (VPTT) by differential scanning calorimetry (DSC) is used to assess the microsphere thermal response. This research introduces a promising methodology for the development of targeted drug delivery systems, which are particularly useful in the context of oxidative stress modulation and inflammation management. Full article

Polymeric composites for manipulating the sustained release of an encapsulated active ingredient are highly sought after for many practical applications; particularly, water-insoluble polymers and core–shell structures are frequently explored to manipulate the release behaviors of drug molecules over an extended time period. In this study, electrospun core–shell nanostructures were utilized to develop a brand-new strategy to tailor the spatial distributions of both an insoluble polymer (ethylcellulose, EC) and soluble polymer (polyvinylpyrrolidone, PVP) within the nanofibers, thereby manipulating the extended-release behaviors of the loaded active ingredient, ferulic acid (FA). Scanning electron microscopy and transmission electron microscopy assessments revealed that all the prepared nanofibers had a linear morphology without beads or spindles, and those from the coaxial processes had an obvious core–shell structure. X-ray diffraction and attenuated total reflectance Fourier transform infrared spectroscopic tests confirmed that FA had fine compatibility with EC and PVP, and presented in all the nanofibers in an amorphous state. In vitro dissolution tests indicated that the radical distributions of EC (decreasing from shell to core) and PVP (increasing from shell to core) were able to play their important role in manipulating the release behaviors of FA elaborately. On one hand, the core–shell nanofibers F3 had the advantages of homogeneous composite nanofibers F1 with a higher content of EC prepared from the shell solutions to inhibit the initial burst release and provide a longer time period of sustained release. On the other hand, F3 had the advantages of nanofibers F2 with a higher content of PVP prepared from the core solutions to inhibit the negative tailing-off release. The key element was the water permeation rates, controlled by the ratios of soluble and insoluble polymers. The new strategy based on core–shell structure paves a way for developing a wide variety of polymeric composites with heterogeneous distributions for realizing the desired functional performances. Full article

The primary objective of this study was to assess the potential utility of quince seed mucilage as an excipient within a graft copolymer for the development of an oral-controlled drug delivery system. The Cydonia oblonga-mucilage-based graft copolymer was synthesized via a free radical polymerization method, employing potassium per sulfate (KPS) as the initiator and N, N-methylene bisacrylamide (MBA) as the crosslinker. Various concentrations of monomers, namely acrylic acid (AA) and methacrylic acid (MAA), were used in the graft copolymerization process. Metoprolol tartarate was then incorporated into this graft copolymer matrix, and the resultant drug delivery system was subjected to comprehensive characterization using techniques such as Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The swelling behavior of the drug delivery system was evaluated under different pH conditions, and in vitro drug release studies were conducted. Furthermore, pharmacokinetic parameters including the area under the curve (AUC), maximum plasma concentration (Cmax), time to reach Cmax (Tmax), and half-life (t1/2) were determined for metoprolol-loaded hydrogel formulations in rabbit plasma, and these results were compared with those obtained from a commercially available product. The key findings from the study include observations that higher concentrations of acrylic acid (AA) and Cydonia oblonga mucilage (CM) in the graft copolymer enhanced swelling, while the opposite trend was noted at elevated concentrations of methacrylic acid (MAA) and N, N-methylene bisacrylamide (MBA). FTIR analysis confirmed the formation of the graft copolymer and established the compatibility between the drug and the polymer. SEM imaging revealed a porous structure in the prepared formulations. Additionally, the swelling behavior and drug release profiles indicated a pH-sensitive pattern. The pharmacokinetic assessment revealed sustained release patterns of metoprolol from the hydrogel network system. Notably, the drug-loaded formulation exhibited a higher Cmax (156.48 ng/mL) compared to the marketed metoprolol product (96 ng/mL), and the AUC of the hydrogel-loaded metoprolol was 2.3 times greater than that of the marketed formulation. In conclusion, this study underscores the potential of quince seed mucilage as an intelligent material for graft-copolymer-based oral-controlled release drug delivery systems. Full article

Purpose: Numerous carbohydrate polymers are frequently used in wound-dressing films because they are highly effective materials for promoting successful wound healing. In this study, we prepared amikacin (AM)-containing hydrogel films through the cross-linking of chitosan (CS) with folic acid along with methacrylic acid (MA), ammonium peroxodisulfate (APS), and methylenebisacrylamide (MBA). In the current studies, an effort has been made to look at the possibilities of these materials in developing new hydrogel film wound dressings meant for a slow release of the antibiotic AM and to enhance the potential for wound healing. Methods: Free-radical polymerization was used to generate the hydrogel film, and different concentrations of the CS polymer were used. Measurements were taken of the film thickness, weight fluctuation, folding resistance, moisture content, and moisture uptake. HPLC, FTIR, SEM, DSC, and AFM analyses were some of the different techniques used to confirm that the films were successfully developed. Results: The AM release profile demonstrated regulated release over a period of 24 h in simulated wound media at pH 5.5 and 7.4, with a low initial burst release. The antibacterial activity against gram-negative bacterial strains exhibited substantial effectiveness, with inhibitory zones measuring approximately 20.5 ± 0.1 mm. Additionally, in vitro cytocompatibility assessments demonstrated remarkable cell viability, surpassing 80%, specifically when evaluated against human skin fibroblast (HFF-1) cells. Conclusions: The exciting findings of this study indicate the promising potential for further development and testing of these hydrogel films, offering effective and controlled antibiotic release to enhance the process of wound healing. Full article

The production of customized polymeric hydrogels in the form of 3D scaffolds with application in bone tissue engineering is currently a topic of great interest. Based on gelatin methacryloyl (GelMa) as one of the most popular used biomaterials, GelMa with two different methacryloylation degrees (DM) was obtained, to achieve crosslinked polymer networks by photoinitiated radical polymerization. In this work, we present the obtention of new 3D foamed scaffolds based on ternary copolymers of GelMa with vinylpyrrolidone (VP) and 2-hydroxyethylmethacrylate (HEMA). All biopolymers obtained in this work were characterized by infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA), whose results confirm the presence of all copolymers in the crosslinked biomaterial. In addition, scanning electron microscopy (SEM) pictures were obtained verifying the presence of the porosity created by freeze-drying process. In addition, the variation in its swelling degree and its enzymatic degradation in vitro was analyzed as a function of the different copolymers obtained. This has allowed us to observe good control of the variation in these properties described above in a simple way by varying the composition of the different comonomers used. Finally, with these concepts in mind, biopolymers obtained were tested through assessment of several biological parameters such as cell viability and differentiation with MC3T3-E1 pre-osteoblastic cell line. Results obtained show that these biopolymers maintain good results in terms of cell viability and differentiation, along with tunable properties in terms of hydrophilic character, mechanical properties and enzymatic degradation. Full article

In this work, a commercial SBS was functionalized with the 2,2,6,6-tetramethylpiperidin-N-oxyl stable radical (TEMPO) via free-radical activation initiated with benzoyl peroxide (BPO). The obtained macroinitiator was used to graft both vinylbenzyl chloride (VBC) and styrene/VBC random copolymer chains from SBS to create g-VBC-x and g-VBC-x-co-Sty-z graft copolymers, respectively. The controlled nature of the polymerization as well as the use of a solvent allowed us to reduce the extent of the formation of the unwanted, non-grafted (co)polymer, thereby facilitating the graft copolymer’s purification. The obtained graft copolymers were used to prepare films via solution casting using chloroform. The –CH₂Cl functional groups of the VBC grafts were then quantitatively converted to –CH₂(CH₃)₃N⁺ quaternary ammonium groups via reaction with trimethylamine directly on the films, and the films, therefore, were investigated as anion exchange membranes (AEMs) for potential application in a water electrolyzer (WE). The membranes were extensively characterized to assess their thermal, mechanical, and ex situ electrochemical properties. They generally presented ionic conductivity comparable to or higher than that of a commercial benchmark as well as higher water uptake and hydrogen permeability. Interestingly, the styrene/VBC-grafted copolymer was found to be more mechanically resistant than the corresponding graft copolymer not containing the styrene component. For this reason, the copolymer g-VBC-5-co-Sty-16-Q with the best balance of mechanical, water uptake, and electrochemical properties was selected for a single-cell test in an AEM-WE. Full article

The aim of this work was to assess the limiting rate of eugenol (Eg) and eugenyl-glycidyl methacrylate (EgGMA) at which the ideal degree of conversion (DC) of resin composites is achieved. For this, two series of experimental composites, containing, besides reinforcing silica and a photo-initiator system, either EgGMA or Eg molecules at 0–6.8 wt% per resin matrix, principally consisting of urethane dimethacrylate (50 wt% per composite), were prepared and denoted as UGx and UEx, where x refers to the EgGMA or Eg wt% in the composite, respectively. Disc-shaped specimens (5 × 1 mm) were fabricated, photocured for 60 s, and analyzed for their Fourier transform infrared spectra before and after curing. The results revealed concentration-dependent DC, increased from 56.70% (control; UG0 = UE0) to 63.87% and 65.06% for UG3.4 and UE0.4, respectively, then dramatically decreased with the concentration increase. The insufficiency in DC due to EgGMA and Eg incorporation, i.e., DC below the suggested clinical limit (>55%), was observed beyond UG3.4 and UE0.8. The mechanism behind such inhibition is still not fully determined; however, radicals generated by Eg may drive its free radical polymerization inhibitory activity, while the steric hindrance and reactivity of EgGMA express its traced effect at high percentages. Therefore, while Eg is a severe inhibitor for radical polymerization, EgGMA is safer and can be used to benefit resin-based composites when used at a low percentage per resin. Full article

Environment-responsive-cum-site-specific delivery of therapeutic drugs into tumor cells is a foremost challenge for chemotherapy. In the present work, Moringa oleifera gum–based pH-responsive nanogel (MOGN) was functionalized as a doxorubicin (DOX) carrier. It was synthesized via free radical polymerization through the γ-irradiation method using acrylamide and N,N’-MBA followed by hydrolysis, sonication, and ultracentrifugation. The swelling behavior of MOGN as a function of pH was assessed using a gravimetric method that revealed its superabsorbent nature (365.0 g/g). Furthermore, MOGN showed a very high loading efficiency (98.35 %L) of DOX by MOGN. In vitro release studies revealed that DOX release from DOX-loaded MOGN was 91.92% at pH 5.5 and 12.18% at 7.4 pH, thus favorable to the tumor environment. The drug release from nanogel followed Korsmeyer–Peppas model at pH 5.5 and 6.8 and the Higuchi model at pH 7.4. Later, the efficient DOX release at the tumor site was also investigated by cytotoxicity study using Rhabdomyosarcoma cells. Thus, the synthesized nanogel having high drug loading capacity and excellent pH-triggered disintegration and DOX release performance in a simulated tumor environment could be a promising candidate drug delivery system for the targeted and controlled release of anticancer drugs. Full article

Rosmarinic acid (RA), a caffeic acid derivative, has been loaded in polymeric nanoparticles made up of poly(lactic-co-glycolic acid) (PLGA) through a nano-emulsion templating process using the phase-inversion composition (PIC) method at room temperature. The obtained RA-loaded nanoparticles (NPs) were colloidally stable exhibiting average diameters in the range of 70–100 nm. RA was entrapped within the PLGA polymeric network with high encapsulation efficiencies and nanoparticles were able to release RA in a rate-controlled manner. A first-order equation model fitted our experimental data and confirmed the prevalence of diffusion mechanisms. Protein corona formation on the surface of NPs was assessed upon incubation with serum proteins. Protein adsorption induced an increase in the hydrodynamic diameter and a slight shift towards more negative surface charges of the NPs. The radical scavenging activity of RA-loaded NPs was also studied using the DPPH·assay and showed a dose–response relationship between the NPs concentration and DPPH inhibition. Finally, RA-loaded NPs did not affect the cellular proliferation of the human neuroblastoma SH-SY5Y cell line and promoted efficient cellular uptake. These results are promising for expanding the use of O/W nano-emulsions in biomedical applications. Full article

Polymer–liposome complexes (PLCs) can be efficiently applied for the treatment and/or diagnosis of several types of diseases, such as cancerous, dermatological, neurological, ophthalmic and orthopedic. In this work, temperature-/pH-sensitive PLC-based systems for controlled release were developed and characterized. The selected hydrophilic polymeric setup consists of copolymers of Pluronic^®-poly(acrylic acid) (PLU-PAA) and Pluronic^®-poly(N,N-dimethylaminoethyl methacrylate) (PLU-PD) synthesized by atom transfer radical polymerization (ATRP). The copolymers were incorporated into liposomes formulated from soybean lecithin, with different copolymer/phospholipid ratios (2.5, 5 and 10%). PLCs were characterized by evaluating their particle size, polydispersity, surface charge, capacity of release and encapsulation efficiency. Their cytotoxic potential was assessed by determining the viability of human epithelial cells exposed to them. The results showed that the incorporation of the synthesized copolymers positively contributed to the stabilization of the liposomes. The main accomplishments of this work were the innovative synthesis of PLU-PD and PLU-PAA by ATRP, and the liposome stabilization by their incorporation. The formulated PLCs exhibited relevant characteristics, notably stimuli-responsive attributes upon slight changes in pH and/or temperature, with proven absence of cellular toxicity, which could be of interest for the treatment or diagnosis of all diseases that cause some particular pH/temperature change in the target area. Full article

Ketorolac tromethamine is a non-steroidal anti-inflammatory drug used in the management of severe pain. The half-life of Ketorolac tromethamine is within the range of 2.5–4 h. Hence, repeated doses of Ketorolac tromethamine are needed in a day to maintain the therapeutic level. However, taking several doses of Ketorolac tromethamine in a day generates certain complications, such as acute renal failure and gastrointestinal ulceration. Therefore, a polymeric-controlled drug delivery system is needed that could prolong the release of Ketorolac tromethamine. Therefore, in the current study, pH-responsive carbopol 934/sodium polystyrene sulfonate-co-poly(acrylic acid) (CP/SpScPAA) hydrogels were developed by the free radical polymerization technique for the controlled release of Ketorolac tromethamine. Monomer acrylic acid was crosslinked with the polymers carbopol 934 and sodium polystyrene sulfonate by the cross-linker N’,N’-methylene bisacrylamide. Various studies were conducted to evaluate and assess the various parameters of the fabricated hydrogels. The compatibility of the constituents used in the preparation of hydrogels was confirmed by FTIR analysis, whereas the thermal stability of the unreacted polymers and developed hydrogels was analyzed by TGA and DSC, respectively. A smooth and porous surface was indicated by SEM. The crystallinity of carbopol 934, sodium polystyrene sulfonate, and the prepared hydrogels was evaluated by PXRD, which revealed a reduction in the crystallinity of reactants for the developed hydrogels. The pH sensitivity of the polymeric hydrogel networks was confirmed by dynamic swelling and in vitro release studies with two different pH media i.e., pH 1.2 and 7.4, respectively. Maximum swelling was exhibited at pH 7.4 compared to pH 1.2 and, likewise, a greater percent drug release was perceived at pH 7.4. Conclusively, we can demonstrate that the developed pH-sensitive hydrogel network could be employed as a suitable carrier for the controlled delivery of Ketorolac tromethamine. Full article

Different combinations of polymers, aspartic acid (ASP), alginic acid (AL), and monomer acrylic acid (AA) were crosslinked in the presence of an initiator ammonium peroxodisulfate (APS) and cross-linker ethylene glycol dimethacrylate (EGDMA) to develop aspartic acid/alginic acid-co-poly(acrylic acid) (ASP/ALPAA) (semi-interpenetrating polymer network (SIPN)) hydrogels by the free radical polymerization technique for the controlled delivery of ibuprofen (IBP). Various studies such as dynamic swelling studies, drug loading, in vitro drug release and sol−gel analysis were carried out for the hydrogels. Higher swelling was observed at higher pH 7.4 as compared to lower pH 1.2, due to the presence of carboxylic groups of polymers and the monomer. Hence, pH-dependent swelling was exhibited by the developed hydrogels which led to a pH-dependent drug release and vice versa. The structural properties of the hydrogels were assessed by FTIR, PXRD, TGA, DSC, and SEM which confirmed the fabrication and stability of the developed structure. FTIR analysis revealed the reaction of both polymers with the monomer during the polymerization process and confirmed the overlapping of the monomer on the backbone of the both polymers. The disappearance of high intense crystalline peaks and the encapsulation of the drug by the hydrogel network was confirmed by PXRD. TGA and DSC showed that the developed hydrogels were thermally more stable than their basic ingredients. Similarly, the surface morphology of the hydrogels was analyzed by SEM and showed a smooth surface with few pores. Conclusively, ASP/ALPAA hydrogels have the potential to deliver IBP for a long period of time in a controlled way. Full article