Preparation, characterization and in vitro release study of carvacrol-loaded chitosan nanoparticles

The fabrication of carvacrol-loaded chitosan nanoparticles was achieved by a two-step method, i.e., oil-in-water emulsion and ionic gelation of chitosan with pentasodium tripolyphosphate. The obtained particles possessed encapsulation efficiency (EE) and loading capacity (LC) in the ranges of 14-31% and 3-21%, respectively, when the initial carvacrol content was 0.25-1.25 g/g of chitosan. The individual particles exhibited a spherical shape with an average diameter of 40-80 nm, and a positively charged surface with a zeta potential value of 25-29 mV. The increment of initial carvacrol content caused a reduction of surface charge. Carvacrol-loaded chitosan nanoparticles showed antimicrobial activity against Staphylococcus aureus, Bacillus cereus and Escherichia coli with an MIC of 0.257 mg/mL. The release of carvacrol from chitosan nanoparticles reached plateau level on day 30, with release amounts of 53% in acetate buffer solution with pH of 3, and 23% and 33% in phosphate buffer solutions with pH of 7 and 11, respectively. The release mechanism followed a Fickian behavior. The release rate was superior in an acidic medium to either alkaline or neutral media, respectively.     

Enhancement of dissolution rate of valdecoxib by solid dispersions technique with PVP K 30 & PEG 4000: preparation and in vitro evaluation

Solid dispersions of valdecoxib were prepared with the objective of dissolution enhancement by melt granulation technique using polyvinyl pyrollidone (PVP K 30) and polyethylene glycol (PEG 4000) alone (1:1) and in combination (1:0.5:0.5). Phase solubility studies showed a linear increase in valdecoxib solubility with increase in polymer concentration in both the cases. The FTIR spectroscopic studies showed the stability of valdecoxib and absence of well defined valdecoxib—PVP K 30–PEG 4000 interaction. Powder X-ray diffraction (XRD) and differential scanning calorimeter (DSC) were used to characterize the solid state of the dispersion, indicated a complete transformation of drug from crystalline to amorphous form. In vitro dissolution studies performed in 0.1 N HCl showed a significant enhance in dissolution rate when PEG 4000 and PVP K 30 were used in combination. Improved drug dissolution by both the carriers may be attributed to the improved wettability, reduction in drug crystallinity and solubilizing effects from solid dispersions of valdecoxib. Accelerated stability studies of solid dispersion with PVP K 30 and PEG 4000 does not show any significant change in the drug content and dissolution profile in 6 months study period. This study concluded that the dissolution rate of valdecoxib can be modulated by appropriate levels of hydrophilic carriers.     

Enhancement of solubility, dissolution and bioavailability of ibuprofen in solid dispersion systems

To improve its solubility, dissolution, and bioavailability; Ibuprofen-polyethylene glycol 8000 (PEG 8000) solid dispersions (SDs) with different drug loadings were prepared, characterized by scanning electron microscopy (SEM) and differential scanning calorimetry (DSC), and evaluated for solubility, in-vitro release, and oral bioavailability of ibuprofen in rats. Loss of individual surface properties during melting and solidification as revealed by SEM micrographs indicated the formation of effective SDs. Absence or shifting towards the lower melting temperature of the drug peak in SDs and physical mixtures in DSC study indicated the possibilities of drug-polymer interactions. Quicker release of ibuprofen from SDs in rat intestine resulted in a significant increase in AUC and C(max), and a significant decrease in T(max) over pure ibuprofen. Preliminary results of this study suggested that the preparation of ibuprofen SDs using PEG 8000 as a meltable hydrophilic polymer carrier could be a promising approach to improve solubility, dissolution and bioavailability of ibuprofen.     

单分散壳聚糖微囊的制备与表征

对水溶性壳聚糖和对苯二甲醛在水/油界面发生的交联反应进行了研究,考察了水相溶液的pH值和油相中对苯二甲醛的浓度对该界面交联反应的影响.采用微流控技术制备得到了单分散的壳聚糖微囊:首先通过毛细管同轴聚焦流微流控装置制备得到单分散的O/W/O乳液.乳液制备中,以Pluronic F-127作为水相乳化剂,羟乙基纤维素作为水相增稠剂,水溶性壳聚糖溶于中间水相;交联剂对苯二甲醛溶于内部油相;含乳化剂PGPR 90的大豆油作为外部油相.乳液制备完成后,以乳液为模板,对苯二甲醛通过油/水界面扩散进入水层,与壳聚糖的氨基发生交联反应,生成壳聚糖聚合物凝胶网络,从而构成微囊的囊壁.通过光学显微镜分析和扫描电镜观察发现:微囊具备良好的单分散性和球形度以及尺寸均一的内部空腔,微囊的囊壁致密无孔.所得单分散微囊在药物传递等领域具备潜在的应用价值.     

Enhancing the dissolution of hydrophobic guests using solid state inclusion complexation: characterization and in vitro evaluation

The objectives of the present investigation were to prepare and characterize solid inclusion complexes of Etodolac (ETD) with β-cyclodextrin (β-CD) in order to study the effect of complexation on the dissolution rate of ETD, a hydrophobic guest molecule. Phase solubility curve was classified as a typical A_L-type for the cyclodextrins (CD’s), showing that soluble complex was formed. The inclusion complexes in the molar ratio of 1:1 and 1:2 (β-CD–ETD) were prepared by various methods such as kneading, co-evaporation and in molar ratio of 1:1 by spray dried technique respectively. The molecular behaviors of ETD in all samples were characterized by nuclear magnetic resonance (NMR) spectroscopy, fourier-transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC) and powder X-ray diffraction (PXRD) studies and Scanning Electron microscopy (SEM) analysis. The results of these studies indicated that complexes prepared by kneading, co-evaporation and spray drying techniques showed inclusion of the ETD molecule into the CD’s cavities. The highest improvement in in vitro dissolution profiles was observed in complexes prepared with spray dried technique. Mean in vitro dissolution time indicated significant difference between the release profiles of ETD from complexes and physical mixtures and from pure ETD.     

Preparation, characterization of hydrophilic and hydrophobic drug in combine loaded chitosan/cyclodextrin nanoparticles and in vitro release study

The compound nanoparticles of chitosan (CS) and cyclodextrin (CD) loading with hydrophilic and hydrophobic drug simultaneously were prepared via the cross-linking method. Methotrexate (MTX) and calcium folinate (CaF) were selected as the model drugs. The prepared nanoparticles were characterized by FT-IR spectroscopy to confirm the cross-linking reaction between CS and cross-linking agent. X-ray diffraction (XRD) was performed to reveal the form of the drug after encapsulation. The average size of nanoparticles ranged from 308.4 ± 15.22 to 369.3 ± 30.01 nm. The nanoparticles formed were spherical in shape with high zeta potentials (higher than +30mV). In vitro release studies in phosphate buffer saline (pH 7.4) showed an initial burst effect and followed by a slow drug release. Cumulative release data were fitted to an empirical equation to compute diffusional exponent (n), which indicated the non-Fickian trend for drug release.     

A biomimetic chitosan derivates: preparation, characterization and transdermal enhancement studies of N-arginine chitosan

A novel arginine-rich chitosan (CS) derivates mimicked cell penetration peptides; N-Arginine chitosan (N-Arg-CS) was prepared by two reaction methods involving activated L-arginine and the amine group on the chitosan. FTIR spectra showed that arginine was chemically coupled with CS. Elemental analysis estimated that the degrees of substitution (DS) of arginine in CS were 6%, 31.3% and 61.5%, respectively. The drug adefovir was chosen as model and its permeation flux across excised mice skin was investigated using a Franz diffusion cell. The results showed that the most effective enhancer was 2% (w/v) concentration of 10 kDa N-Arg-CS with 6% DS. At neutral pH, the cumulative amount of adefovir permeated after 12 hours was 2.63 ± 0.19 mg cm(-2) which was 5.83-fold more than adefovir aqueous solution. Meanwhile N-Arg-CS was 1.83, 2.22, and 2.45 times more effective than Azone, eucalyptus and peppermint, respectively. The obtained results suggest that N-Arg-CS could be a promising transdermal enhancer.     

Preparation and characterization of chitosan nanocomposites with vermiculite of different modification

In this study, the biopolymer chitosan/vermiculite (VMT) nanocomposites were prepared by the solution mixing process of the cationic biopolymer chitosan with three different modified VMT (HVMT, NVMT, and OVMT), which was treated by hydrochloride, sodium, and cetyl trimethyl ammonium bromide (CTAB), respectively. Wide-angle X-ray diffraction (WAXD), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) have been employed in the characterization of chitosan/HVMT, chitosan/NVMT, and chitosan/OVMT nanocomposites. Both WAXD data and TEM images of chitosan nanocomposites indicated that the silicate layers were disorderedly dispersed into the chitosan matrix in nano scale. The thermal stability of chitosan/HVMT nanocomposites have the greatest improvements compared to that of neat chitosan, chitosan/NVMT and chitosan/OVMT nanocomposites. It provides a potential approach to prepare high performance and low-cost chitosan nanocomposite.     

Nanocrystalline cuprous oxide in chitosan membrane: Preparation,characterization, and photocatalytic properties

Crystalline Cu₂O nanoparticles were synthesized via the templating method by taking advantage of the chelation of chitosan with copper ions. Experimental data indicated that Cu₂O-embedded film exhibited higher photocatalytic activity toward methhyl orange degradation under visible light irradiation.     

Preparation, characterization and adhesive properties of di- and tri-hydroxy benzoyl chitosan nanoparticles

Modified chitosans with 3,4-di-hydroxy benzoyl groups (CS-DHBA) and 3,4,5-tri-hydroxy benzoyl groups (CS-THBA) were synthesized and their nanoparticles were prepared via ionic crosslinking by tripolyphosphate (TPP). The chemical structure and degree of substitution (DS) of di-and tri-hydroxy benzoyl chitosans are determined by FTIR and 1H-NMR spectroscopy. The morphology of particles, size distribution and zeta potential of nanoparticles were studied using transmission electron microscopy (TEM) and dynamic light scattering (DLS), respectively. The mean diameters of particles of CS-DHBA and CS-THBA nanoparticles were 144 nm and 112 nm, respectively. It was found that the particles size decreased slightly with decreasing the degree of substitution and increasing degree of deacetylation (DD), due to increasing of ionic crosslinking of ammonium ions and polyanions of tripolyphosphate. The TEM photographs of CS-DHBA show that these particles are spherical in shape, but the particles of CS-THBA show some aggregation. In addition, the solubility and the mechanical properties of the prepared modified chitosans and their nanoparticles were evaluated for bio-adhesive and biomedical application. The results of solubility tests indicated that, the CS-DHBA and CS-THBA have higher solubility at pH > 7 comparing to CS. Also the CS-DHBA, CS-THBA and their nanoparticles showed a significant adhesive capacity and enhanced tensile strength and tensile modulus.     

Porous-conductive chitosan scaffolds for tissue engineering, 1. Preparation and characterization

Novel porous-conductive chitosan scaffolds were fabricated by incorporating conductive polypyrrole (PPy) particles into a chitosan matrix and employing a phase separation technique to build pores inside the scaffolds. Conductive polypyrrole particles were prepared with a microemulsion method using FeCl3 as a dopant. The preparation conditions were optimized to obtain scaffolds with controlled pore size and porosity. The conductivity of the scaffolds was investigated using a standard four-point probe technique. It was found that several kinds of scaffolds showed a conductivity close to 10(-3) S.cm(-1) with a low polypyrrole loading of around 2 wt.-%. The main mechanical properties, such as tensile strength, breaking elongation and Young's modulus of the scaffolds, were examined both in the dry and in the hydrated states. The results indicated that a few different kinds of scaffolds exhibited the desired mechanical strength for some tissue engineering applications. The miscibility of polypyrrole and chitosan was also evaluated using a dynamic mechanical method. The presence of significant phase separation was detected in non-porous PPy/chitosan scaffolds but enhanced miscibility in porous PPy/chitosan scaffolds was observed.     

Preparation,characterization, and antibacterial activity of organo-sepiolite/chitosan/silver bionanocomposites

Bionanocomposites with different loadings of silver (Ag) were prepared via synthesis of Ag nanoparticles (AgNPs) using the wet chemical reduction method in the lamellar space layer of the organo-sepiolite/chitosan (O-SEP/CS). The prepared O-SEP/CS/Ag bionanocomposites were characterized using various analysis methods for their structure, morphology, and optical properties. The characteristic absorption bands from the UV–visible absorption spectrum confirmed the formation of AgNPs. The antibacterial activities of O-SEP/CS/Ag bionanocomposites were investigated against gram-positive and gram-negative bacteria using the disc diffusion method. The results suggest that O-SEP/CS/Ag bionanocomposites can be useful in wide range of bio-medical applications because of high antibacterial activity.     

Preparation and characterization of polymer electrolyte membrane from chloroacetate chitosan/chitosan blended with epoxidized natural rubber

Chitosan-based membranes are among the most effective and efficient PEMs for fuel cells, however their low proton conductivity needs to be improved. In this study, chitosan, chloroacetate chitosan (CCS), chitosan blend with epoxidized natural rubber (ENR), and CCS with ENR blend based membranes were prepared by solution casting, crosslinked with NaOH and H₂SO₄, and investigated for physical, chemical, electrical and ionic properties. The functional groups were identified by ATR-FTIR spectroscopy and the peaks matched improved membrane properties. The surface roughness of the membranes was determined by AFM, and it increased with the amount of ENR. The electrical properties measured with an LCR meter showed that the CCS, CS and CS-B had the highest conductance, conductivity, capacitance and dielectric constant, while the CCS10/ENR8, CS10/ENR8 and CS15/ENR3 showed the highest resistance and resistivity. Furthermore, the CCS gave the lowest dissipation factor, which indicates its suitability for use in a PEM. In addition, the contact angle was relatively high for CS-B, CS and CCS.     

Preparation and characterization of temperature response molecularly imprinted membrane with chitosan and methylmethacrylate

In this study, a novel temperature controlled molecularly imprinted membrane (Temp-Ctrl-MIM) made of chitosan and methyl methacrylate was fabricated with bovine serum albumin (BSA) as template molecule. The film was characterized by infrared spectroscopy (IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and the permeation experiment. The results revealed that the porous structure of the film was as similar as the BSA. Moreover, the membrane had advanced molecular imprinting capability to BSA comparing to pepsin and casein at any temperature and the film demonstrated an excellent ability to identify specific template molecule (BSA) at the synthesis temperature comparing to other temperatures.     

Physico-chemical characterization and dissolution properties of nifluminic acid-cyclodextrin-PVP ternary systems

In view of the poor aqueous solubility of nifluminic acid (NIF), the aim of this article was to improve its solubility and dissolution rate through the preparation of formulations based on hydroxypropyl β-cyclodextrin (HPβCD) and polyvinylpyrrolidone K25 (PVP K25), a combination of carriers which has been advantageously used for a similar purpose with various hydrophobic drugs. Ternary systems of NIF, HPβCD, and PVP K25 were prepared in different drug to CD to PVP ratios by physical mixing, kneading, microwave irradiation, and co-evaporation. Differential scanning calorimetry, thermogravimetric analysis, hot stage microscopy, Fourier transform infrared spectroscopy, and X-ray powder diffractometry were used to investigate the resulting solid-state interactions. The results showed that the solid state of the drug in the amorphous or crystalline ternary combinations influenced both the solubility and the dissolution rate of NIF.     

Preparation and characterization of multilayered structures with polyconjugated systems

Soluble poly(3-alkylthiophenes) can be conveniently tailored by the introduction of polar groups in the side chain with the aim of obtaining structures able to give multilayered films with the Langmuir Blodgett technique. The films, uniform in thickness, show orientation of the polyenic backbone in the dipping direction as detected by UV-visible measurements in polarised light. These materials can be conveniently used in electronic device preparation.