We derivatized low molecular weight chitosan (LMWC) with 3-mercaptopropanoic acid (3-MPA) by a coupling reaction. The chemical modification of LMWC was characterized by Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance,1HNMR. We researched the influence of 3-MPA on the nanoparticles formation by ionic gelation method using sodium tripolyphosphate (TPP) as cross-linker reagent. In order to optimize the nanoparticles formation, we studied the effect of the pH solution and molar ratio on nanoparticles stability. Analyses of particle size, morphology, and surface charge were determined by dynamic light scattering, Atomic Force Microscopy, and zeta potential, respectively. It was found that formation of semispherical and stable nanoparticles was improved due to the chemical modification of chitosan. Optimized semispherical nanoparticles of thiolated chitosan were synthesized with the parameters (pH 4.7, molar ratios 1 : 106). Additionally, we reported the thermodynamic profile of the nanoparticles formation determined by isothermal titration calorimetry (ITC). The aggregation process achieved to form nanoparticles of thiolated and nonmodified chitosan consisted of two stages, considering one binding site model. Gibbs free energy(ΔG)and binding constant (Ka) describe the aggregation process of thiolated chitosan/TPP, which is an initial reaction and followed by an endothermic stage. These results are promising for the possible application of these nanoparticles as nanocarriers and delivery systems.
In this study we describe a mathematical analysis that considers the temperature effects of the controlled drug release process from biodegradable poly-D,L-lactide-co-glycolide (PLGA) nanoparticles.Temperature effects are incorporated and applied to two drug release models. The first one consists of a two-stage release process that considers only simultaneous contributions of initial burst and nanoparticle degradation-relaxation (BR model). The second one is a three release stage model that considers, additionally, a simultaneous drug diffusion (BRD model) step. In these models, the temperature dependency of the release parameters, initial burst constant, k b , the rate of degradationrelaxation constant, k r , time to achieve 50% of release, t max , and effective diffusion coefficient constant (D e ), are determined using mathematical expressions analogous to the Arrhenius equation. The temperature dependent models are used to analyze the release of previously encapsulated Rhodamine 6G dye as a model drug in polyethylene glycol modified PLGA nanoparticles. The experimental data used to develop the mathematical model was obtained from release studies carried out in phosphate buffer pH 7.4 at 37 C, 47 C, and 57 C. Multiphasic release behaviors with an overall increase rate associated with the incubation temperature were observed. The study incorporates a parametrical analysis that can evaluate diverse temperature variation effects of the controlled release parameters for the two models.
Plasmid DNA (pVAX1-NH36) was encapsulated in nanoparticles of poly-dl-lactic-coglycolic (PLGA) functionalized with polyethylene glycol (PEG) and folic acid (PLGA-PEG-FA) without losing integrity. PLGA-PEG-FA nanoparticles loaded with pVAX1-NH36 (pDNA-NPs) were prepared by using a double emulsification-solvent evaporation technique. PLGA-PEG-FA synthesis was verified by FT-IR and spectrophotometry methods. pVAX1-NH36 was replicated in Escherichia coli (E. coli) cell cultures. Atomic force microscopy (AFM) analysis confirmed pDNA-NPs size with an average diameter of 177-229 nm, depending on pVAX1-NH36 loading and zeta potentials were below −24 mV for all preparations. In vitro release studies confirmed a multiphase release profile for the duration of more than 30-days. Plasmid release kinetics were analyzed with a release model that considered simultaneous contributions of initial burst and degradation-relaxation of nanoparticles. Fitting of release model against experimental data presented excellent correlation. This mathematical analysis presents a novel approach to describe and predict the release of plasmid DNA from biodegradable nanoparticles.
Abstract:The handling of metallic nanoparticles often requires their dispersion into several polar and nonpolar solvents. Solid-phase stages or polymer-based ligands are commonly required to complete the transfer. The construction of a thiol ligand based in oleic acid, and its ability to efficiently assist in gold and silver nanoparticle aqueous-organic phase transfer is reported. After the transfer, the particles are completely dispersed in an organic solvent, preserving their diameter and morphology, as confirmed by ultraviolet-visible spectroscopy and scanning transmission electron micrographs.
The interesting properties of stimuli-responsive polymers lead to a wide range of possibilities in design and engineering of functional material for the biomedical application. A systematic approach focused on the evaluation of the physical properties of multiresponse (pH and temperature) PNIPAM was reported in this work. The effect of three different molar ratios of poly(n-isopropylacrylamide): chitosan (1:49, 1:99 and 1:198) were evaluated and labeled correspondingly as PC1F, PC2F, and PC3F. An increase in the lower critical solution temperature (LCST) of sample PC1F (34°C) was observed by differential scanning calorimetry (DSC). The presence of low molecular weight chitosan (LMWC) full-interpenetrating polymer (Full-IPN) segments in poly(n-isopropylacrylamide) was confirmed by Fourier-transform infrared spectroscopy (FT-IR). The hydrogel’s water capture was analyzed by two models of swelling, the power law model and a model that considers the relaxation of polymeric chains of the hydrogel, finding good correlations with experimental data in both cases. Sample PC3F resulted with higher swellability, increasing the weight of the hydrogel around seven times. Hydrogel pH-sensibility was confirmed placing the samples at different pH environments, with an apparent increase in swellability for acidic conditions, confirming the highest swellability for sample PC3F, due to hydrogen bonds boosted by chitosan high molar ratio. Based on these results, the hydrogel obtained has potential as a thermo-pH triggered hydrogel in drug delivery applications.
Here we demonstrate a simple method for the organic sonosynthesis of stable Iron Carbide@Iron Oxide core-shell nanoparticles (ICIONPs) stabilized by oleic acid surface modification. This robust synthesis route is based on the sonochemistry reaction of organometallic precursor like Fe(CO) in octanol using low intensity ultrasonic bath. As obtained, nanoparticles diameter sizes were measured around 6.38 nm ± 1.34 with a hydrodynamic diameter around 25 nm and an estimated polydispersity of 0.27. Core-Shell structure of nanoparticles was confirmed using HR-TEM and XPS characterization tools in which a core made up of iron carbide (FeC) and a shell of magnetite (γ-FeO) was found. The overall nanoparticle presented ferromagnetic behavior at 4 K by SQUID. With these characteristics, the ICIONPs can be potentially used in various applications such as theranostic agent due to their properties obtained from the iron oxides and iron carbide phases.
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