Development of a novel nanocomposite consisting of 3-(4-methoxyphenyl)propionic acid and magnesium layered hydroxide for controlled-release formulation

ABSTRACT

Magnesium layered hydroxide (MLH) intercalated with anionic 3-(4-methoxyphenyl)propionic acid (MPP) was synthesised by a direct reaction method using magnesium oxide and MPP as precursors. A further coating of chitosan was applied on the external surface of MLH–MPP nanocomposite to form a new material, named MLH–MPP/chitosan nanocomposite. The XRD pattern showed an intense and sharp peak at basal spacing 18.9 Å, proving that MPP anions were successfully intercalated into the interlayer gallery of MLH in a monolayer arrangement. The XRD pattern of the MLH–MPP/chitosan nanocomposite shows similar peaks with the MLH–MPP nanocomposite. The result was also supported by FTIR spectra and elemental analysis. TGA/DTG spectra showed that the thermal stabilities of the guest anion in the both nanocomposites were markedly enhanced. A controlled-release study of the MPP ion from the MLH–MPP/chitosan nanocomposite showed a slower release compared to MLH–MPP nanocomposite with an initial rapid release and slow release thereafter. Meanwhile, the release behaviours of MPP ions from both nanocomposites were governed by pseudo-second order kinetics. This result highlights the potential of the nanocomposite as an encapsulated material for the controlled-release formulation of MPP anions.     

Stacking of lamellae in Mg/Al hydrotalcites: Effect of metal ion concentrations on morphology

A hybrid nanocomposite based on the intercalation of carbonate anion has been synthesized through co-precipitation technique. Powder X-ray diffraction patterns (PXRD) showed pure layered double hydroxide (LDH) phases having crystallite size around 20 and 13 nm in ‘a’ and ‘c’ crystallographic directions, respectively. Fourier transform infrared and Raman spectroscopy measurements exhibit shifting of bands with increase of divalent metal ion concentration and it further suggests the presence of carbonate anions. Differential scanning calorimetry (DSC) and thermogravimetry analysis (TGA) exhibit the three stages of thermal degradation, which is characteristic behaviour of layered double hydroxide. CHN and energy dispersive X-ray analysis support the PXRD and spectroscopy results. The nature of charge observed through Zeta potential analyzer is positive. Transmission electron microscope (TEM) exhibits the characteristic LDH platelet morphology with the platelets stacked one above the other.     

Green synthesis of biocidal silver-activated charcoal nanocomposite for disinfecting water

We report for the first time the green synthesis of silver nanoparticles using West Indian cherry (Malpighia emarginata) extract known for its high vitamin C content. UV–visible spectroscopy, powder X ray diffraction (PXRD), dynamic light scattering (DLS), scanning electron microscopy (SEM) and energy dispersive X ray spectroscopy (EDX) analysis were used to characterise silver nanoparticles. Silver nanoparticles thus synthesised exhibit antimicrobial activity against gram-negative bacteria such as Pseudomonas aeruginosa, Escherichia coli, and gram-positive bacteria such as Bacillus subtilis and Staphylococcus aureus. The antimicrobial property of nanoparticles thus synthesised was applied in the production of silver-activated charcoal nanocomposite towards fabrication of antimicrobial water filtration columns. The microbial filtration efficiency of the nanocomposite was found to be higher compared to virgin activated charcoal even with reusage.     

Synthesis and characterization of a clay/waterborne polyurethane nanocomposite

A novel clay/waterborne polyurethane (WPU) nanocomposite was synthesized from polyurethane and organoclay. The clay was organically modified with a swelling agent, namely, 1,12-diaminododecane. The nanocomposite was characterized using Fourier transform infrared (FT-IR) and gel permeation chromatography (GPC). The d-spacing of clay was determined by X-ray diffraction (XRD) and confirmed by transmission electron microscopy (TEM). XRD and TEM analyses indicated that clay retains a layer structure in the clay/waterborne polyurethane (WPU) nanocomposite. Consequently, these materials are an intercalated nanocomposite with a d-spacing of around 4 to 5 nm. FT-IR revealed that adding clay does not affect the synthesis of the waterborne polyurethane. GPC results indicated that molecular weight decreased as the clay content increased. The thermal properties of the nanocomposite were examined using a thermogravimetric analyzer (TGA). Results showed that adding clay increased the temperature of thermal degradation by 15°C.     

Mechanical properties of natural fibre reinforced polymer composites

During the last few years, natural fibres have received much more attention than ever before from the research community all over the world. These natural fibres offer a number of advantages over traditional synthetic fibres. In the present communication, a study on the synthesis and mechanical properties of new series of green composites involving Hibiscus sabdariffa fibre as a reinforcing material in urea-formaldehyde (UF) resin based polymer matrix has been reported. Static mechanical properties of randomly oriented intimately mixed Hibiscus sabdariffa fibre reinforced polymer composites such as tensile, compressive and wear properties were investigated as a function of fibre loading. Initially urea-formaldehyde resin prepared was subjected to evaluation of its optimum mechanical properties. Then reinforcing of the resin with Hibiscus sabdariffa fibre was accomplished in three different forms: particle size, short fibre and long fibre by employing optimized resin. Present work reveals that mechanical properties such as tensile strength, compressive strength and wear resistance etc of the urea-formaldehyde resin increases to considerable extent when reinforced with the fibre. Thermal (TGA/DTA/DTG) and morphological studies (SEM) of the resin and biocomposites have also been carried out.     

Preparation and characterization of zinc-exchanged montmorillonite and its effectiveness as aflatoxin B1 adsorbent

A zinc-exchanged montmorillonite (Zn-MONT) was prepared from a natural montmorillonite (MONT) and the adsorption of aflatoxin B₁ (AFB₁) was investigated at pH 3 and 7. Characterization of Zn-MONT was done by determination of chemical composition, the point of the zero charge (pH_pzc), thermal (DTA/TGA/DTG) and X-ray powder diffraction (XRPD) analysis.     

Fabrication of silver nanocomposite films impregnated with curcumin for superior antibacterial applications

Silver nanocomposite films are found to be very effective material for anti-bacterial application. In the present work, sodium carboxylmethyl cellulose silver nanocomposite films (SCMC SNCF) were tried for antibacterial applications. To enhance their applicability novel film-silver nanoparticle-curcumin composites have been developed. SCMC SNCF are developed from sodium carboxylmethyl cellulose (SCMC), N,N ¹ -methylenebisacrylamide (MBA) and silver nitrate solution. These films were characterized by FTIR, UV–visible, XRD, TGA, DSC and TEM techniques. The formed silver nanoparticles have an average particle size of ~15 nm as observed by transmission electron microscopy (TEM). Curcumin loading into SCMC SNCF is achieved by diffusion mechanism. The UV–Visible analysis indicated that higher encapsulation of curcumin in the films with higher SCMC content. Further, it was observed that the presence of silver nanoparticles in the films enhanced the encapsulation of curcumin indicating an interaction between them. Moreover, the antibacterial activity showed that the SCMC films generated with silver nanoparticles have a synergistic effect in the antimicrobial activity against Escherichia coli (E. coli). In order improve the healing efficacy as antibacterial agents, curcumin loaded with SCMC SNCFs were developed which showed significant inhibition of E. coli growth than the silver nanoparticles and curcumin alone film. Therefore, the present study clearly provides novel antimicrobial films which are potentially useful in preventing/treating infections.     

Intercalation of methylene blue into layered potassium titanoniobate KTiNbO5: characterization and electrochemical investigation

Methylene blue (MB) was intercalated into layered potassium titanoniobate (KTiNbO₅) through a guest–guest exchange method by use of the intercalation compound n-C₄H₉NH₃ ⁺–TiNbO₅ as a precursor. The MB⁺/H⁺–TiNbO₅ nanocomposite has been characterized by XRD, SEM, IR, TGA, UV, elemental analysis, and electrochemical cyclic voltammetric measurements. From the XRD and elemental analysis results, we proposed that the MB⁺ cations formed a single layer standing vertically to the titanoniobate nanosheets together with H⁺. The CV curves of the MB⁺/H⁺–TiNbO₅ nanocomposite thin film exhibited a fine diffusion-controlled redox process, which hints the possibility of being utilized as an electrode modifying material.     

A pH-sensitive nanocomposite microsphere based on chitosan and montmorillonite with in vitro reduction of the burst release effect

Objective: The aim of this study was to prepare pH-sensitive ofloxacin (OFL)/montmorillonite (MMT)/chitosan (CTS) nanocomposite microspheres that improve the burst release effect of the drug by the solution intercalation technique and emulsification cross-linking techniques. Methods: First, OFL/MMT hybrids were prepared through the solution intercalation technique. Then, OFL/MMT-intercalated OFL/MMT/CTS nanocomposite microspheres were obtained through emulsification cross-linking technology. The intercalated nanocomposite was confirmed by Fourier-transform infrared spectroscopy and X-ray diffraction. Finally, in vitro release of OFL from the microspheres was performed in simulated gastric fluids and simulated intestinal fluids. The effect of MMT content on drug encapsulation efficiency and the drug release of the nanocomposite microspheres were investigated. Results: The results showed that the release rate of OFL from the nanocomposite microspheres at pH 7.4 was higher than that at pH 1.2. Compared with pure CTS microspheres, the incorporation of certain amount of MMT in the nanocomposite microspheres can enhance the drug encapsulation efficiency and reduce the burst release. Conclusion: A sustained release particulate system can be obtained by incorporating MMT into the nanocomposite microspheres and can improve the burst release effect of the drug.     

A study of the influence of crystallite size on the electrical and magnetic properties of CuFe2O4

An attempt has been made to clarify the fundamental assumption that the properties of materials change as the crystallite size of the material is reduced below 100 nm. CuFe₂O₄ samples of different crystallite sizes were prepared by the sol–gel and combustion methods and then analyzed by X-ray diffraction (XRD), thermal analyses (TGA/DTG) and scanning electron microscopy (SEM) techniques. The magnetic properties were studied by measuring the AC magnetic susceptibility (χ) and the Mössbauer spectroscopy. The DC electrical resistivity, dielectric constant, dielectric loss tangent, Curie temperature and hyperfine splitting of the samples change with the crystallite size. The change in the electrical properties is attributed to the formation of discrete energy levels instead of the bands. However, the magnetic parameters change due to the existence of non magnetic surface layers. The isomer shift and the hyperfine splitting show gradual increase with the increase in crystallite sizes.     

Preparation of UV-curable intercalated/exfoliated epoxide/acrylateclays nanocomposite resins

Preparation of UV-curable intercalated/exfoliated epoxide/acrylateclays nanocomposite resins with the addition of specific monomers and solvent via the consideration of solubility parameter and chemical reactivity was carried out in this work. Due to the good compatibility with surfactant in acrylateclays and the cationic oligomer in resin matrix, the two additive monomers dispersed uniformly in resin matrix with the swollen acrylateclays before UV curing. As revealed by conversion ratio and DTG analyses, chemical bonds between the two additive monomers, the cationic oligomers and surfactant in acrylateclays were formed during UV irradiation. This, in turn, generated a hybrid acrylate-based/epoxy network and effectively enlarged the lamellae spacing of inorganic clays in nanocomposite resins prepared in this work. The XRD and TEM characterizations revealed that the intercalated clay domains containing exfoliated lamellae about 1 nm in thickness uniformly disperse in polymeric matrix. The nanocomposite resin containing 5 wt.% inorganic filler possessed the physical properties as follows: T _d-5% = 213 °C, CTE = 80.5 ppm/°C, moisture absorption = 6.12%, average optical transmittance = 83.17%, and adhesion strength on glass substrate = 43.8 kgf/cm². The analyses above indicated that the formation of polymeric interpenetrating networks and nanometer-scale exfoliation of clay lamellae not only improve the thermal properties and resistance to moisture permeation, but also retain highly optical transmittance and satisfactory adhesion strength of nanocomposite resins prepared in this work. A better device lifetime property was hence achieved when the nanocomposite resins were applied to the packaging of OLEDs.     

Acenes adducts with C70 fullerene: Anthracene,tetracene and pentacene

The mono-adducts of C₇₀ fullerene with pentacene, tetracene and antracene were synthesized. The C₇₀/acene adducts were studied with FT-IR and the electronic absorption spectroscopy. Thermogravimetric analysis (TGA) in combination with derivative thermogravimetry (DTG) and differential thermal analysis (DTA) were employed to determine the quantitative composition of the adducts and their relative thermal stability. Differential scanning calorimetry (DSC) was employed as well for the determination of the stability of the adducts. It was found that the C₇₀/acene adducts decompose with endothermal reactions. The enthalpy of the decomposition reaction and the decomposition temperatures were determined and found in agreement with the DTG and DTA results.     

Powder X-ray diffraction method for the quantification of cocrystals in the crystallization mixture

Context: The solid state purity of cocrystals critically affects their performance. Thus, it is important to accurately quantify the purity of cocrystals in the final crystallization product.

Objective: The aim of this study was to develop a powder X-ray diffraction (PXRD) quantification method for investigating the purity of cocrystals. The method developed was employed to study the formation of indomethacin-saccharin (IND-SAC) cocrystals by mechanochemical methods.

Materials and methods: Pure IND-SAC cocrystals were geometrically mixed with 1:1 w/w mixture of indomethacin/saccharin in various proportions. An accurately measured amount (550?mg) of the mixture was used for the PXRD measurements. The most intense, non-overlapping, characteristic diffraction peak of IND-SAC was used to construct the calibration curve in the range 0–100% (w/w). This calibration model was validated and used to monitor the formation of IND-SAC cocrystals by liquid-assisted grinding (LAG).

Results: The IND-SAC cocrystal calibration curve showed excellent linearity (R²?=?0.9996) over the entire concentration range, displaying limit of detection (LOD) and limit of quantification (LOQ) values of 1.23% (w/w) and 3.74% (w/w), respectively. Validation results showed excellent correlations between actual and predicted concentrations of IND-SAC cocrystals (R²?=?0.9981).

Discussion: The accuracy and reliability of the PXRD quantification method depend on the methods of sample preparation and handling. The crystallinity of the IND-SAC cocrystals was higher when larger amounts of methanol were used in the LAG method.

Conclusion: The PXRD quantification method is suitable and reliable for verifying the purity of cocrystals in the final crystallization product.     

Influences of MonoSilanolIsobutyl-POSS on thermal stability of polymethylsilxoane

Incorporation of polyhedral oligomeric silsesquioxane (POSS) molecules into polymer matrix resulted in increased used and decomposition temperatures. Polymethylsiloxane (PMS)/MonoSilanolIsobutyl-POSS hybrid copolymers containing various proportions of MonoSilanolIsobutyl-POSS were prepared. The structures and thermal properties of the obtained products were characterized with Gel Permeation Chromatography (GPC), Fourier transform infrared (FTIR), thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG) and X-ray photoelectron spectroscopy (XPS). The GPC and FTIR spectra suggested successful bonding of MonoSilanolIsobutyl-POSS and PMS. TGA, DTG and XPS analysis revealed that MonoSilanoIsobutyl-POSS reinforced PMS are thermally more stable than the original PMS, primarily by the elimination of SiOH effects, the nanoreinforcement effect of POSS, the retardation of polymer chain motion and the formation of SiO₂ protective layer.     

Dielectric relaxation studies on [PEO–SiO<Subscript>2</Subscript>]:NH<Subscript>4</Subscript>SCN nanocomposite polymer electrolyte films

Present work deals with findings on dielectric relaxation behaviour and a.c. conduction in a SiO₂-doped polymer nanocomposite electrolyte system, namely, [(100 − x)PEO + xSiO₂]:yNH₄SCN. The formation of nanocomposite has been ascertained by XRD measurements. The effect of salt and filler (SiO₂) on conductivity response of PEO-based nanocomposite polymer electrolyte has been investigated by impedance spectroscopy. The variation of dielectric permittivity, dielectric loss and modulus spectra with frequency and temperature was carried out from impedance spectroscopy data. The a.c. conductivity seems to follow the universal power law.     

Preparation of the acidic PVA/MMT nanocomposite polymer membrane for the direct methanol fuel cell (DMFC)

A novel nanocomposite polymer electrolyte membrane composed of PVA polymer matrix and nanosized Montmorillonite (MMT) filler, was prepared by a solution casting method. The characteristic properties of the PVA/MMT nanocomposite polymer membrane were investigated using thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), atomic force microscopy (AFM), micro-Raman spectroscopy, and the AC impedance method. The PVA polymer directly blended with nanosized MMT filler (2-20 wt.%) showed good ionic conductivity, thermal, and mechanical properties. The highest ionic conductivity value for the acidic PVA/10 wt.%MMT nanocomposite polymer membrane was around 0.0368 S cm^− 1 at 30 °C. The methanol permeability (P) value was 3-4 × 10^− 6 cm² s^− 1. It was revealed that the addition of nanosized MMT fillers into the PVA matrix could markedly improve the electrochemical properties of the PVA/MMT nanocomposite membrane. In fact, the PVA/MMT nanocomposite polymer membrane appears to be a good candidate for the DMFC applications.     

Fabrication and characterization of carbon fiber reinforced clay/epoxy composite

In this study, dynamic mechanical analysis (DMA), thermogravimetric analysis (TGA), and flexural tests were performed on unfilled, 1, 2, 3, and 4 wt% clay filled SC-15 epoxy to identify the effect of clay weight fraction on thermal and mechanical properties of the epoxy matrix. The flexural results indicate that 2.0 wt% clay filled epoxy showed the highest improvement in flexural strength. DMA studies also revealed that 2.0 wt% system exhibit the highest storage modulus and T _g as compared to neat and other weight fraction. However, TGA results show that thermal stability of composite is insensitive to the clay content. Based on these results, the nanophased epoxy with 2 wt% clay was then utilized in a vacuum assisted resin transfer molding set up with carbon fabric to fabricate laminated composites. The effectiveness of clay addition on thermal and mechanical properties of composites has been evaluated by TGA, DMA, tensile, flexural, and fatigue test. 5 °C increase in glass transition temperature was found in nanocomposite, and the tensile and flexural strengths improved by 5.7 and 13.5 %, respectively as compared to the neat composite. The fatigue strength was also improved significantly. Based on the experimental result, a linear damage model combined with the Weibull distribution function has been established to describe static failure processing of neat and nanophased carbon/epoxy. The simulated stress–strain curves from the model are in good agreement with the test data. Simulated results show that damage processing of neat and nanophased carbon/epoxy described by bimodal Weibull distribution function.     

The Influence of Potassium Clavulanate on the Rate of Amoxicillin Sodium Degradation in Phosphate and Acetate Buffers in the Liquid State

The stability of aqueous admixtures of amoxicillin sodium and potassium clavulanate was studied in the liquid state at selected pH values. Potassium clavulanate was found to catalyze the rate of degradation of amoxicillin sodium under the conditions of this study. In phosphate buffer (at pH 7.0) both amoxicillin sodium and potassium clavulanate showed first-order degradation when stored separately. However, when combined the rate of amoxicillin degradation increased and t₉₀ values for amoxicillin decreased from 69.6 min for amoxicillin alone to 10.8 min for amoxicillin in the combination at 55°C. A kinetic model was developed that explained the catalytic behavior of potassium clavulanate and phosphate buffer. In acetate buffer the rate of degradation of amoxicillin sodium followed first-order kinetics, but the catalytic effect of clavulanate caused curvature in the rate plots at higher temperatures and clavulanate concentrations. This catalytic effect was less than that occurred in phosphate buffer (where the t₉₀ value of amoxicillin decreased from 137.3 min for amoxicillin alone to 52.5 min for amoxicillin in combination at 55°C). First-order bi-exponential decay occurred with amoxicillin degradation, which explained this change in rate.     

Poly(vinyl phosphonic acid) (PVPA)–BaFe12O19 Nanocomposite

We present a method for the fabrication of PVPA/BaFe₁₂O₁₉ nanocomposite by in-situ polymerization of vinyl phosphonic acid, VPA in the presence of synthesized BaFe₁₂O₁₉ NPs. Nanoparticles and the nanocomposite were analyzed by XRD, FTIR, TGA, SEM, TEM, VSM, and conductivity techniques for structural and physicochemical characteristics. Nanoparticles, identified as BaFe₁₂O₁₉ from XRD analysis, were successfully coated with PVPA and the linkage was assessed to be via P?CO bonds. Electron microscopy analysis revealed aggregation of BaFe₁₂O₁₉ particles and dominantly platelet morphology upon composite formation. TGA analysis revealed the composition of the nanocomposite as 65% BaFe₁₂O₁₉ and 35% polymer. Magnetic evaluation revealed that adsorption of PVPA anions during the preparation of the nanocomposite strongly influenced the magnetic properties resulting in much lower saturation magnetization values. DC conductivity measurements were used to calculate activation energy of PVPA/BaFe₁₂O₁₉ nanocomposite and it was obtained as 0.37?eV.     

Synthesis and ferrimagnetic properties of novel Sm-substituted LiNi ferrite–polyaniline nanocomposite

Polyaniline (PANI)–LiNi_0.5Sm_0.08Fe_1.92O₄ nanocomposite was synthesized by an in situ polymerization of aniline in the presence of LiNi_0.5Sm_0.08Fe_1.92O₄ ferrite. The products were characterized by powder X-ray diffractometer (XRD), Fourier transform infrared (FTIR) and UV–visible absorption spectrometer, thermogravimetric analyser (TGA), atomic force microscope (AFM) and vibrating sample magnetometer (VSM). The results of XRD, FTIR and UV–visible spectra confirmed the formation of PANI–LiNi_0.5Sm_0.08Fe_1.92O₄ composite. AFM study showed that ferrite particles had an effect on the morphology of the composite. TGA revealed that the incorporation of ferrite improved the thermal stability of PANI. The nanocomposite under applied magnetic field exhibited the hysteresis loops of ferrimagnetic nature at room temperature. The bonding interaction between ferrite and PANI in the nanocomposite had been studied.