A simple method to generate spontaneous chemisorption of metallic particles mediated by carboxylate groups from silylated oligomeric poly(amide‐imide)s

The present work describes oligomeric poly(amide‐imide)s (PAIs) containing several l ‐amino acidic residues and two silicon atoms in their repeat unit, whose carboxylate terminal group was chemisorbed onto metallic particles (Cu, Ag or Au) previously deposited in controlled conditions via physical vapor deposition. Thus, for each prepared polymer–metallic hybrid, the surface morphology, particle size distribution, and percentage of organic material, silicon and metal were studied using scanning electron microscopy and energy‐dispersive X‐ray spectroscopy. The results show that the hybrids are formed probably via electrostatic interaction between the carboxylate anions of the PAIs and nanoparticle cations. This bridging ligand was visualized using Raman spectroscopy and corroborated with X‐ray diffraction. Optical studies and resistivity measurements (conductivity) of each hybrid were developed using UV‐visible and the four‐point probe method, respectively. X‐ray photoelectron spectroscopy was used to study the oxidation states of the metallic particles at surface level. Thus, a simple and spontaneous protocol is proposed for the preparation of metallic particles stabilized in situ by an oligomer, a procedure that takes place from seconds to a few minutes. Finally, particle diameters were measured using atomic force microscopy in order to study possible agglomeration of the metallic particles with time. © 2017 Society of Chemical Industry     

Preparation and In Vitro Properties of N-Succinylchitosan– or Carboxymethylchitin–Mitomycin C Conjugate Microparticles with Specified Size

The preparation of cross-linked conjugate microparticles of N succinyl-chitosan (Suc) or 6-O-carboxymethylchitin (CM) with mitomycin C (MMC), which showed an adequate size for liver targeting (0.2–3 μm), was attempted by a combination of water-soluble carbodiimide (EDC) coupling and emulsification technique. As for Suc, microparticles with a diameter less than a few micrometers could be obtained easily, while the preparation of CM microparticles (CM-MPs) of the same diameter was not necessarily easy. First, preparation conditions were compared for CM-MPs, and some conditions gave CM-MPs with a diameter less than a few micrometers. As to CM-MMC conjugate microparticles, the method by addition of EDC after emulsification using CM with low molecular weight (CM_L) gave more appropriate microparticles with a mean diameter of 0.97 μm (CM_L-MP-MMC). Suc-MMC conjugate microparticles adequate for liver targeting could be produced by the addition of EDC both before and after emulsification; especially, the conjugate microparticles with a mean diameter of 0.45 μm (Suc-MP-MMC) were derived by the addition of EDC before emulsification. Suc-MP-MMC exhibited a higher drug content than CM_L-MP-MMC. CM_L-MP-MMC and Suc-MP-MMC exhibited 50% drug release times of 2.87 h and 42.1 h, respectively.     

Preparation and Antimicrobial Activityof Gelatin Microparticles Containing Propolis Against Oral Pathogens

ABSTRACT

Gelatin microparticles containing propolis ethanolic extractive solution were prepared by spray-drying technique. Particles with regular morphology, mean diameter ranging of 2.27 μm to 2.48 μm, and good entrapment efficiency for propolis were obtained. The in vitro antimicrobial activity of microparticles was evaluated against microorganisms of oral importance (Enterococcus faecalis, Streptococcus salivarius, Streptococcus sanguinis, Streptococcus mitis, Streptococcus mutans, Streptococcus sobrinus, Candida albicans, and Lactobacillus casei). The utilized techniques were diffusion in agar and determination of minimum inhibitory concentration. The choice of the method to evaluate the antimicrobial activity of microparticles showed be very important. The microparticles displayed activity against all tested strains of similar way to the propolis, showing greater activity against the strains of E. salivarius, S. sanguinis, S. mitis, and C. albicans.     

Mupirocin calcium microencapsulation via spray drying: feed solvent influence on microparticle properties,stability and antimicrobial activity

Objectives: The aim of this research was to design a controlled release, spray dried, mupirocin calcium-loaded microparticles (MP) with acrylic polymer and assess the influence of a feed solvent at preselected drug:polymer proportions (1:5 and 2:1 (w/w)) on the performance and stability of the prepared MP.

Methods: Physicochemical properties of MP were assessed using modulated differential scanning calorimetry (MDSC), and thermogravimetric analyses (TGA), Fourier transformed infrared spectroscopy (FTIR) and X-ray analyses and were correlated with drug release. Morphology and particle size were determined using low-angle laser light scattering and a scanning electron microscope. A time-kill assay was conducted on two strains of Staphylococcus aureus to evaluate the antimicrobial activity of MP.

Results and discussion: The MP formed solid dispersions without apparent drug crystallization. Drug-polymer miscibility, morphology, drug release and consequently antimicrobial activity were dependent on drug loading (DL) and the used solvent. The superior control of drug release from MP was achieved for the higher DL (2:1 (w/w) drug:polymer proportion) using solvents in the following order: methanol ≈ methanol:ethanol (50:50, w/w) > isopropanol:acetone (40:60, w/w). Moreover, a time-kill assay performed on S. aureus (ATCC 29213) and methicillin-resistant S. aureus strains confirmed the prolonged release and preservation of antimicrobial activity of the microencapsulated drug. The physical aging of the solid dispersion after 10 months of storage had negligible impact on the MP performance.

Conclusions: Acrylic-based MP were confirmed as suitable microcarriers for prolonged drug release using a well-established spray drying technique, while solvent influence was strongly related to the DL employed.     

Polymer Crystallization Induced by Biaxial Stretching During Film Manufacture

Abstract

In the manufacture of semicrystalline polymer films, orientation is commonly introduced. This orientation may be uniaxial, unbalanced biaxial, or balanced biaxial. Machine-direction and transverse stretching may be concurrent or sequential; each orienting process is characterized by a trajectory on the biaxial stress plane and the biaxial extension plane. The presence of uniaxial or biaxial tensile stress strongly affects the process of polymer crystallization, influencing the crystal-amorphous equilibrium, crystallization kinetics, and the resulting polymer morphology. Post-solidification alterations in morphology can be imposed by drawing or heat-setting under biaxial tension, below the crystalline melting point.

The machine-direction and transverse properties of a semicrystalline polymer film depend strongly on the crystalline morphology, and hence on the processing history. The dependence of film properties on processing conditions are well recognized and widely exploited; but the morphology of biaxially oriented films and the structure-property relationships involved are only partly understood.     

Micron‐sized membrane reactors: Multicompartment semipermeable polymer particles containing palladium nanoparticles

Multicompartment polymer microparticles are prepared encapsulating palladium nanoparticles within closed‐shell compartments, using a double‐emulsion (W₁/O/W₂), evaporative limited coalescence process. The encapsulation efficiency in some cases is as high as 99%, and very little Pd leaches from the particles. The Pd nanoparticles dispersed in an aqueous environment within the closed‐shell compartments of the microparticles catalyze hydrogenation reactions of low molar mass substrates in water at substantial rates. The microparticle walls serve as semipermeable membranes, permitting diffusion of small molecules into the compartments while retaining the larger metal nanoparticles. The microparticles can be reused after simple filtration. The catalytic activity increases on recycling, possibly because of plasticization of polymer walls by the reactant and products, resulting in increased diffusion. In a second demonstration of catalytic activity, the microparticles efficiently decompose hydrogen peroxide. These nanoparticle‐containing microparticles serve as convenient, reusable catalyst carriers, and prevent inadvertent human and environmental contact with nanoparticles. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42021.     

The effect of process parameters on the size and morphology of poly(D,L‐lactide‐co‐glycolide) micro/nanoparticles prepared by an oil in oil emulsion/solvent evaporation technique

For the past few decades, there has been a considerable research interest in the area of biodegradable polymeric micro‐ and nanoparticles for tissue engineering, regenerative medicine, implants, stents, medical devices, and drug delivery systems. Poly(D,L ‐lactide‐co‐glycolide) (PLGA) is well‐known by its safety in biomedical preparations which has been approved for human use by the FDA. The goal of this study was to evaluate the influence of process parameters on size characteristics of PLGA microparticles prepared by oil in oil (o/o) solvent evaporation technique. This method has been introduced as one of the most appropriate methods for hydrophilic agents. Scanning electron microscopy showed that prepared particles were spherical with smooth surface without aggregation. Particle size varied from 570 nm to 29 μm in different experimental conditions. Stirring speed, polymer concentration, impeller type, and dropping size had a significant effect on the particle size. The polydispersity index of particles showed a strong relationship with the surfactant concentration, impeller type, and dropping size. It was concluded that increasing in temperature up to 50°C or changing in dropping rate has a little effect on reducing the size of PLGA particles. The residual solvent content in the final suspension was less than 0.1 ppm that is in appropriate range for biomedical application. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010