Amphiphilic polymers have attracted significant interest due to their versatile applications in the biomedical, pharmaceutical, and cosmetic fields. In this work, we report the synthesis of novel cationic comb-shaped polymers derived from N, N-dimethylaminoethyl acrylate (MDMAEA) through free radical polymerization. The obtained polymers were thoroughly characterized using Fourier-transform infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H NMR), and viscosimetric analysis to confirm their structural features and evaluate their solution behavior. In aqueous and hydro-alcoholic media, amphiphilic polymers are known to undergo self-assembly processes driven by the balance between hydrophilic and hydrophobic interactions. To investigate this phenomenon, a detailed viscosimetric study was performed on the synthesized polymers. The results revealed that the reduced viscosity of polymer solutions decreases as the concentration increases, indicating the predominance of intramolecular associations. This behavior is attributed to the hydrophobic interactions of the side alkyl chains, which induce polymer chain folding and reduce intermolecular entanglements. Such behavior is consistent with the general characteristics of polysoaps, highlighting their ability to form micelle-like structures in selective solvents. The findings of this study provide valuable insights into the self-organization of comb-shaped polymers in solution, which is essential for tailoring their physicochemical properties and optimizing their performance in drug delivery, surface modification, and other advanced applications.Based on the optical spectra, the composite has an optical bandgap energy, Eg = 3.15 eV. The energy gap results can confirm the behavior of a semiconductor. The polymers PDMAEAC6 and PDMAEAC10 exhibited strong antimicrobial activity against both bacteria and fungi, likely through membrane disruption via electrostatic interactions, making them promising candidates for biomedical and topical use.
Several research works place significant emphasis on the versatile strategy of combining multiple polymerization methods for the synthesis of amphiphilic block copolymers. Many interesting structures can be prepared through the combinations of ring-opening polymerization and living radical polymerization techniques. Herein, we report a successful synthesis of amphiphilic block copolymers of acrylic acid with 2-ethyl-2-oxazoline and 2-phenyl-2-oxazoline monomers by combining two polymerization methods, including iodine transfer polymerization and cationic ring-opening polymerization. The synthesized copolymers were characterized using Nuclear Magnetic Resonance, Fourier Transform Infrared Spectroscopy and Gel Permeation Chromatography analysis. The morphology and the structure of the copolymers were investigated by optical microscopy. The finding results reveal that the reaction medium exhibits an interesting arrangement of the polymer chains, and indicates that the synthesized copolymers possess remarkable self-assembly properties in aqueous solution. This combinatorial approach could pave the way for the preparation of more complex supramolecular structures. In fact, these copolymers can be easily modified, thereby enhancing their properties.
Inflammation is a significant physiological response of the body to various stimuli, necessitating effective therapeutic interventions. This study focuses on the formulation and evaluation of an emulgel using clove oil, known for its important anti-inflammatory properties. The emulgel was developed by incorporating clove oil into a gel based on the presence of alginate, aiming to enhance its topical delivery and therapeutic efficacy. The formulation process involved optimizing the oil-to-gel ratio for a good consistency, stability and skin permeability. The emulgel was characterized by various physicochemical evaluations, including pH, viscosity, spreadability and stability studies, to ensure its suitability for topical application. In vitro and in vivo anti-inflammatory activity was assessed using clove oil as the active agent in the emulgel in comparison with 1
The present work investigates, for the first time, the synthesis of a composite film based on glutaraldehyde-cross-linked chitosan (GA-CS) and a natural zeolite (H-ZSM-5) and its application for the removal of hexavalent chromium (Cr(VI)) from aqueous solutions under wide experimental conditions. The composite film (GA-CS-ZEO) characterization by using various analytical techniques confirms its successful production with promising physical, chemical, and thermal properties. The use of the response surface methodology (RSM) for the optimization of the Cr(VI) adsorption by this composite shows that that the maximum removal efficiency (82.39
Due to their strong molecular hyperpolarizability, organic push–pull materials are gaining interest for nonlinear optical applications. We were able to characterize the intramolecular charge transfer and the distribution of the electron cloud within the molecular unit by exciting these materials under the influence of an electric field. The series products of conjugated monomers derived from acrylo–azobenzene containing in the para position the attracting groups (–H, –NO2, –COOC2H5, –SO3H and –COOH) exhibit good nonlinear optical activity. We computed the nonlinear optical characteristics of these compounds as well as exploiting the theoretical calculations of DFT and AM1 to determine their hyperpolarizabilities. Besides, we investigated the increase in hyperpolarizability in the push–pull model of organic compounds under the effect of the strength of attracting groups, the existence of the conjugated [Formula: see text]-electron and the azo bridge.
Active and intelligent films with antioxidant, antimicrobial, and pH-responsive properties were developed by incorporating betacyanins-rich weed amaranth (A. hybridus) extract (AE) into chitosan/gelatin (Cs/Gn) and arginine-modified chitosan/gelatin (MCs/Gn) blend films. The microstructures, physical and functional properties of Cs/Gn, MCs/Gn, Cs/Gn-AE, and MCs/Gn-AE films were compared. Results showed the addition of AE into MCs/Gn film produced a compact inner microstructure through H-bonding and electrostatic interactions. Meanwhile, AE remarkably changed the colors of the film under alkaline pH mediums. However, AE significantly reduced the water vapor permeability of the films. By comparing different films, MCs/Gn-AE film presented the best UV-vis light and barrier ability as well as the highest mechanical strength. Moreover, MCs/Gn and MCs/Gn-AE films showed stronger microbial growth inhibition than Cs/Gn and Cs/Gn-AE films. Cs/Gn-AE and MCs/Gn-AE films possessed more potent free radical scavenging activity than Cs/Gn and MCs/Gn. Notably, MCs/Gn-AE film is suitable to monitor fish freshness and could be used as novel multifunctional packaging in the seafood industry.
In this present study, a series of copolymers with diverse compositions were produced using bulk ring-opening polymerization of glycolide and ?-caprolactone, using stannous(II) octoate as initiator. 1H, 13C NMR, and FTIR spectroscopy were used to characterize the resultant copolymers. After-wards, the oil/water emulsion evaporation technique was used to create blend microspheres of poly (glycolide-co-?-caprolactone) and ethylcellulose in order to investigate the controlled release of 5-fluorouracil, an anticancer drug. The size distribution of the microspheres was studied by optical microscope, which confirmed their spherical nature with sizes ranging from 112 to 186?m, FTIR and X-ray diffraction were used to confirm the polymer blend compatibility and to confirm the absence of drug-polymer interactions. Moreover, in vitro release experiments were performed at 37?C in simulated buffer medium of the stomach (pH=1.2) for 2h, and simulated intestinal medium (pH=7.4). It was found that the release of 5-fluorouracil from blend microspheres followed pH-independent release as compared to that of plain poly(?-caprolactone) and ethylcellulose microspheres for more than 10h. Furthermore, to better understand the nature of the drug release profiles, release data was fitted to empirical models.
We presents in this work the preparation of several formulations, based on biocompatible biodegradable polymers: polycaprolactone (PCL) and poly(lactic-co-glycolic) acid (PLGA) loaded with Erythromycin (ERYT) antibiotic. These biocompatible materials were used to prepare microspheres with and without immobilized ERYT via simple evaporation method by simple emulsion. The particle size was determined by scanning electron microscopy and the absence of the interaction with ERYT was confirmed via X-ray diffraction and infrared spectroscopy. The release kinetics of ERYT were studied and then, ERYT loaded PCL and PLGA blends microspheres were used for the inhibition of gram-positive S. aureus strain. The microbial activity was carried-out by Agar diffusion disc method. The results show that PCL/PLGA blend and PCL alone inhibited the strain by ERYT present in kinetic aliquots with the complementary effect of the polymers. A numerical model was proposed for modeling the kinetics reported in our study.
Polyacrylamide (Poly (AAm)) and poly(acrylamide-co-methyl methacrylate) (poly (AAm-co-MMA)) hydrogels were synthesized by solution free radical polymerization initiated by Potassium persulfate initiator (KPS) at different feed mol monomer ratios and N,N-methylene bisacrylamide (BIS) as a crosslinking agent. The obtained hydrogels were characterized by FTIR, scanning electron microscopy (SEM) and swelling behaviour. The swelling properties of Poly (AAm) and poly (AAm-co-MMA) hydrogels were studied in distilled water at different pH. The effect of temperature on swelling behaviour of these hydrogels has been analysed by variation from 25 to 50?C. Poly(AAm-co-MMA) hydrogels were considered for the removal of Red Erionyl textile dyes from aqueous solutions. Two kinetics models were applied; the first and the second order kinetics as well as the Freundlich and Langmuir isotherms were tested. The result confirms that the adsorption process of Red Erionyl dye follows second-order kinetics and their equilibrium data were fitted well to the linear Langmuir model.
In the present study, microparticles loading amoxicillin have been prepared and characterized. These particles were carried out by solvent evaporation method (o/w) using beta-cyclodextrin (beta-CD) and cellulose acetate phthalate (CAP) as matrix. This study is carried out in order to investigate its effect on encapsulation efficiency and drug release kinetics. Scanning Electron Microscopy (SEM) micrographs showed that microspheres were smooth, rigid and porous with different shapes. The encapsulation efficiency varied between 71 and 86 % and the mean diameter d10 was varied between 184 to 250 mu m. Microspheres were also characterized by FTIR and XRD. The release kinetics was studied in pH 1.2 medium at and 37 +/- 0.5 degrees C and their data base were analyzed by different mathematical methods as Fick and Higuchi laws. The prepared microspheres were exposed to two bacterial strains at different concentrations and the inhibition zones have been determined.
This paper describes the synthesis of novel amphiphilic diblock copolymer composed of polystyrene (PS) as the hydrophobic block and Poly(N-[3-(dimethylamino)propyl] methacrylamide) (PDMAPMA) as hydrophilic block by reverse-mode iodine transfer controlled radical polymerization (RITP). Initially, homopolymer based on activated monomers (styrene) was synthesized by RITP. Thereafter, amphiphilic diblock copolymer was synthesized. The diblock copolymer obtained was characterized by spectroscopic methods: FTIR, 1H NMR, 13C NMR, Energy-dispersive X-ray spectroscopy (EDX) to analyze the elemental composition. Their thermal behaviour was investigated by thermogravimetric analysis (TGA). Study of the self-organization in aqueous phase of the amphiphilic copolymer revealed that formation of micelles for concentrations was higher than critical aggregation concentration (CAC) which their values were determined by tensiometry. The self-assembly behaviors of this copolymer was studied in aqueous solution at different concentrations, PH and temperatures using Dynamic light scattering (DLS).
In this paper, Single and dual modification with etherification and Cross-linking of Zea mays starch were homo-geneously carried out and in [BMIM]Cl ionic liquid media (IL), an excellent solvent for the starch modification using sodium monochloroacetic acid and sodium trimetaphosphate in different sequences. Characteristics analyzed indicated modification of starch which was further confirmed by determining a high degree of etherification (0.79) and Cross-linking (91.2%) could be achieved at short time scale in [BMIM]Cl, which is apparently due to the excellent dissolving capacity and catalytic effect of IL Temperature showed a positive effect on swelling power and water solubility indexes of native and modified starches, however in Cross-linked starch the swelling power decreased. A considerable reduction in amylose content was noticed after modification except for Cross-linked starch. FT-IR and NMR analyses confirmed the modification of starch. Furthermore, the results of XRD and a SEM revealed that the crystallinity and the morphology of the native Zea mays starch was slightly changed throughout its modification in IL and was completely destroyed. Studies on the phase transitions associated with gelatinization using a DSC showed higher enthalpy values for Cross-linked starch and dual modified starches as compared to native and etherified starch. (C) 2018 Elsevier B.V. All rights reserved.
We were interested in this work by the modification of hydrolyzed poly (acrylamide) which allow us to obtain a new copolymer based on acrylamide and p- phenylenediamine (PPD). The properties of the obtained copolymer and its structure and composition were established by H-1 NMR, FTIR spectroscopy's and by TGA analysis. The prepared copolymer was used as a flocculent substance in the aim to remove turbidity from wastewater. Several experimental parameters such as pH of water, initial turbidity, flocculent concentration and dyes concentration, and their effects on the flocculation process were studied. The considered results show that the studied copolymer is good flocculent and efficient at a very low optimum concentration.
Iodine transfer radical homo- and diblock copolymerization of N-[3(dimethylamino)propyl] methacrylamide (DMAPMA) with methyl methacrylate (MMA) were carried out in the presence of iodine I-2 and 2,2'-azobis(isobutyronitrile) (AIBN) as chain transfer agent and initiator, respectively. Using reverse iodine transfer polymerization (RITP) method based on the in situ generation of transfer agents using molecular iodine I-2. The homopolymer and copolymer were characterized by FT-IR and H-1 NMR. The self-assembly behaviours of diblock copolymer in water are studied by viscosity and tensiometry techniques. The water-soluble fraction of P(DMAPMA-b-MMA) block copolymer formed micelles which were investigated at 25 degrees C in water at 0.2 mg.mL(-1) concentration using a tensiometry device. Dynamic light scattering technique (DLS) was performed over a wide range of concentration to determine hydrodynamic size of the aggregates.
Poly (ester-amide) s (PEA) were synthesized via a polycondensation reaction of 1, 3-phenylene bis (2-Oxazoline) carboxylic anhydride, and diol. The polymerization proceeds through the formation of a dicarboxy ester by reaction of two anhydride molecules with one diol molecule and subsequent 2-oxazoline ring opening by attack of the dicarboxy ester. The expected structures of the polymers were confirmed by FTIR and 1 H-NMR. Thermal properties of the poly (ester amide) s were characterized by Differential scanning calorimeter (DSC), X-ray diffraction (XRD) and Thermogravimetric analysis (ATG). Hydrolytic and enzymatic degradations in solid media using Aspergilus Niger of the materials were performed. The biodegradation of polymers were also carried in liquid medium and the source of microorganisms is an inoculum based on activated sludge, by measuring the net biochemical oxygen demand (BOD) under the aerobic conditions. The biodegradation of polymers was observed by changing of BOD a long of 7 days.
Hydrochlorothiazide (HCTZ), which was developed and introduced in the late 1950s, is still one of the most frequently employed drugs in antihypertensive treatments. Its poor aqueous solubility is one of the reasons for its limited bioavailability after oral administration. The present paper provides details of the preparation of HCTZ-loaded microspheres by the solvent evaporation technique. A total of seven formulations were prepared using ethyl cellulose, poly(?-caprolactone) (PCL), ?-cyclodextrin (?-CD) and synthesized poly-(methyl methacrylate) (PMMA) of different molecular weights in different drug-to-carrier ratios in order to investigate their effect on the encapsulation efficiency and drug release kinetics. The prepared formulations were characterized by Fourier transform-infrared (FTIR) spectroscopy, powder X-ray diffractometry, differential scanning calorimetry, yield, drug loading, optical microscopy, surface morphology by scanning electron microscopy (SEM), and in vitro release studies in simulated gastrointestinal tract fluid. The loading efficiency was found in the range from 18?0.34 to 39?0.95 %. The microspheres were spherical, and the mean Sauter diameter (d32) of the obtained microparticles ranged from 26?0.16 to 107?0.58 ?m. The presence of the drug and polymer carriers in the microparticles was confirmed by FTIR spectroscopy and XRD analysis. In vitro dissolution studies showed that the release rate was largely affected by the characteristics of the microparticles, namely the particle size and the nature of the matrix. The release data are best fitted to the Higuchi model with high correlation coefficients (r?).
Introduction: The present paper provides details of preparation of hardcapsules based on microspheres containing 2-aminothiazole as an antithyroidian agent and synthesized poly(butylsuccinate) (PBS) or ethylcellulose(EC10) as biodegradable matrices as well as the study of the drug delivery. Methods: A disintegration tests of these gelatinous capsules were done. The biodegradable synthesized polyester was characterized by infrared spectroscopy, nuclear magnetic resonance (mono and bidimentional H1NMR, 13CNMR) and by Differential Scanning Calorimetry (DSC). A viscosimetric study has been done in order to evaluate viscosimetric PBS's weight wich was calculated from Mark-Houwink equation. The microencapsulation of 2-aminothiazole was done using solvent evaporation technique. Results: Microspheres were spherical and the effects of varying emulsifiers and blades number on microspheres encapsulation efficiency were evaluated. A kinetic studies of releases of 2-aminothiazole in gastric pH were done in order to evaluate the best late effect and then the best formulation.
The synthesis of macromonomers is made by anhydrides to prevent the reducing average molecular weight of synthesized polymers in order to obtain poly alpha, w unsaturated (styrene oxide) more stable, using a proton exchanged montmorillonite clay called Maghnite-H+. For cationic polymerization of the styrene oxide, we have used the Maghnite-H+ as a heterogeneous polymerization catalyst to synthesis poly (styrene oxide), which is performed in solution of dichloromethane with methacrylic anhydride at temperature 20 degrees C. We have investigated the effect of the amount of catalyst and methacrylic anhydride on yield of polymer, and analysed the structures of modified montmorillonite by X-Ray Diffraction (XRD). Also, we have characterized the polymers by infrared spectroscopy (IR) and nuclear magnetic resonance (NMR), gel permeation chromatography (GPC) and differential scanning calorimetry (DSC).