Search results for: calorimetry

Authors: Qing Liu, Jean-fabien Capsal, Claude Richard

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In this current contribution, authors are dedicated to investigate influence of the crystal lamellae orientation on electromechanical behaviors of relaxor ferroelectric Poly (vinylidene fluoride –trifluoroethylene -chlorotrifluoroethylene) (P(VDF-TrFE-CTFE)) films by control of polymer microstructure, aiming to picture the full map of structure-property relationship. In order to define their crystal orientation films, terpolymer films were fabricated by solution-casting, stretching and hot-pressing process. Differential scanning calorimetry, impedance analyzer, and tensile strength techniques were employed to characterize crystallographic parameters, dielectric permittivity, and elastic Young’s modulus respectively. In addition, large electrical induced out-of-plane electrostrictive strain was obtained by cantilever beam mode. Consequently, as-casted pristine films exhibited surprisingly high electrostrictive strain 0.1774% due to considerably small value of elastic Young’s modulus although relatively low dielectric permittivity. Such reasons contributed to large mechanical elastic energy density. Instead, due to 2 folds increase of elastic Young’s modulus and less than 50% augmentation of dielectric constant, fully-crystallized film showed weak electrostrictive behavior and mechanical energy density as well. And subjected to mechanical stretching process, Film C exhibited stronger dielectric constant and out-performed electrostrictive strain over Film B because edge-on crystal lamellae orientation induced by uniaxially mechanical stretch. Hot-press films were compared in term of cooling rate. Rather large electrostrictive strain of 0.2788% for hot-pressed Film D in quenching process was observed although its dielectric permittivity equivalent to that of pristine as-casted Film A, showing highest mechanical elastic energy density value of 359.5 J/m^3. In hot-press cooling process, dielectric permittivity of Film E saw values at 48.8 concomitant with ca.100% increase of Young’s modulus. Films with intermediate mechanical energy density were obtained.

Keywords: crystal orientation, electrostroctive strain, mechanical energy density, permittivity, relaxor ferroelectric

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Authors: Hussein M. Etmimi, Peter E. Mallon

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Electrospinning uses an electrical charge to draw very fine fibers (typically on the micro or nano scale) from a liquid or molten precursor. Over the years, this method has become a widely used and a successful technique to process polymer materials and their composites into nanofibers. The main focus of this work is to study the electrospinning of multi-phase amphiphilic copolymers and their nanocomposites, which contain graphene as the nanofiller material. In such amphiphilic materials, the constituents segments are incompatible and thus the solid state morphology will be determined by the composition of the various constituents as well as the method of preparation. In this study, amphiphilic block copolymers of poly(dimethyl siloxane) and poly(methyl methacrylate) (PDMS-b-PMMA) with well-defined structures were synthesized and the solution electrospinning of these materials and their properties were investigated. Atom transfer radical polymerization (ATRP) was used to obtain the controlled block copolymers with relatively high molar masses and narrow dispersity. First, PDMS macroinitiators with different chain length of 1000, 5000 and 10000 g/mol were synthesized by the reaction of monocarbinol terminated PDMS with α-bromoisobutyryl bromide initiator. The obtained macroinitiators were used for the polymerization of methyl methacrylate monomer to obtain the desired block copolymers using the ATRP process. Graphene oxide (GO) of different loading was then added to the copolymer solution and the resultant nanocomposites were successfully electrospun into nanofibers. The electrospinning was achieved using dimethylformamide/chloroform mixture (60:40 vl%) as electrospinning solution medium. Scanning electron microscopy (SEM) showed the successful formation of the electrospun fibers with dimensions in the nanometer range. X-ray diffraction indicated that the GO nanosheets were of an exfoliated structure, irrespective of the filler loading. Thermogravimetric analysis also showed that the thermal stability of the nanofibers was improved in the presence of GO, which was not a function of the filler loading. Differential scanning calorimetry also showed that the mechanical properties (measured as glass transition temperature) of the nanofibers was improved significantly in the presence of GO, which was a function of the filler loading.

Keywords: elctrospinning, graphene oxide, nanofibers, polymethyl methacrylate (PMMA)

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Authors: Rawia M. Khalil, Ghada Abd-Elbary, Mona Basha, Ghada E. A. Awad, Hadeer A. Elhashemy

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Background: Bacterial infections of the eye are the clinical conditions responsible for ocular morbidity and blindness. Conjunctivitis is an inflammation of the conjunctiva, due to Staphylococcus aureus. Lomefloxacin HCl (LXN) is a third generation flouroquinolone antibiotic with a broad spectrum against wide range of bacteria and very effective against Staph infections especially in conjunctiva (conjunctivitis). The present study aims to develop and evaluate novel ocular proniosomal gels of Lomefloxacin Hcl (LXN); in order to improve its ocular bioavailability for the management of bacterial conjunctivitis. Materials and methods: Proniosomes were prepared by coacervation phase separation method using different types of nonionic surfactants (Span 60,40,20,Tween 20,40,60,80,Brij 35,98,72) solely and as mixtures with Span® 60. The formed gels were characterized for entrapment efficiency, vesicle size and in vitro drug release. The optimum proniosomal gel; P-LXN 7 were characterized for pH measurement, transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) as well as Stability study and microbiological evaluation .The results revealed that only Span 60 was able to form stable LXN proniosomal gel when used individually while the other nonionic surfactants formed gels only in combination with Span 60 at different ratios. The optimum proniosomal gel; P-LXN 7 (Span60:Tween60, 9:1) appeared as spherical shaped vesicles having high entrapment efficiency (>80 %), appropriate vesicle size (187 nm) as well as controlled drug release over 12h. DSC confirmed the amorphous nature and the uniformity of LXN inclusion within the vesicles. Physical stability study did not show any significant changes in appearance or entrapment efficiency or vesicle size after storage for 3 months at 4°C. Ocular irritancy test revealed that P-LXN 7 was safe, well tolerable and suitable for ocular delivery. In vivo antibacterial activity of P-LXN 7 evaluated using the susceptibility test and topical therapy of induced ocular conjunctivitis confirmed the enhanced antibacterial therapeutic efficacy of the LXN-proniosomal gel compared to the commercially available LXN eye drops; Orchacin®. Conclusions: Our results suggest that proniosomal gels could provide a promising carrier of LXN for efficient ocular treatment of bacterial conjunctivitis.

Keywords: bacterial conjunctivitis, lomefloxacin HCl, ocular drug delivery, proniosomes

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Authors: F. Elhaouzi, H. Lahlali, M. Zaghrioui, I. El Aboudi A. BelfKira, A. Mdarhri

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The effect of physico chemical properties of solvents on the transport process and mechanical properties in elastomeric nano composite materials is reported. The investigated samples are formed by a semi-crystalline ethylene-co-butyl acrylate polymer filled with hard spherical carbon black (CB) nano particles. The swelling behavior was studied by immersion the dried samples in selected solvents at room temperature during 2 days. For this purpose, two chemical compounds methyl derivatives of aromatic hydrocarbons of benzene, i.e. toluene and xylene, are used to search for the mass and molar volume dependence on the absorption kinetics. Mass gain relative to the mass of dry material at specific times was recorded to probe the absorption kinetics. The transport of solvent molecules in these filled elastomeric composites is following a Fickian diffusion mechanism. Additionally, the swelling ratio and diffusivity coefficient deduced from the Fickian law are found to decrease with the CB concentration. These results indicate that the CB nano particles increase the effective path length for diffusion and consequently limit the absorption of the solvent by occupation free volumes in the material. According to physico chemical properties of the two used solvents, it is found that the diffusion is more important for the toluene molecules solvent due to their low values of the molecular weight and volume molar compared to those for the xylene. Differential Scanning Calorimetry (DSC) and X-ray photo electron (XPS) were also used to probe the eventual change in the chemical composition for the swollen samples. Mechanically speaking, the stress-strain curves of uniaxial tensile tests pre- and post- swelling highlight a remarkably decrease of the strength and elongation at break of the swollen samples. This behavior can be attributed to the decrease of the load transfer density between the matrix and the CB in the presence of the solvent. We believe that the results reported in this experimental investigation can be useful for some demanding applications e.g. tires, sealing rubber.

Keywords: nanocomposite, absorption kinetics, mechanical behavior, diffusion, modelling, XPS, DSC

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Authors: A. Atli, K. Candelier, J. Alteyrac

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Environmental and sustainability concerns push the industries to manufacture alternative materials having less environmental impact. The Wood Plastic Composites (WPCs) produced by blending the biopolymers and natural fillers permit not only to tailor the desired properties of materials but also are the solution to meet the environmental and sustainability requirements. This work presents the elaboration and characterization of the fully green WPCs prepared by blending a biopolymer, BIOPLAST® GS 2189 and spruce sawdust used as filler with different amounts. Since both components are bio-based, the resulting material is entirely environmentally friendly. The mechanical, thermal, structural properties of these WPCs were characterized by different analytical methods like tensile, flexural and impact tests, Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and X-ray Diffraction (XRD). Their water absorption properties and resistance to the termite and fungal attacks were determined in relation with different wood filler content. The tensile and flexural moduli of WPCs increased with increasing amount of wood fillers into the biopolymer, but WPCs became more brittle compared to the neat polymer. Incorporation of spruce sawdust modified the thermal properties of polymer: The degradation, cold crystallization, and melting temperatures shifted to higher temperatures when spruce sawdust was added into polymer. The termite, fungal and water absorption resistance of WPCs decreased with increasing wood amount in WPCs, but remained in durability class 1 (durable) concerning fungal resistance and quoted 1 (attempted attack) in visual rating regarding to the termites resistance except that the WPC with the highest wood content (30 wt%) rated 2 (slight attack) indicating a long term durability. All the results showed the possibility to elaborate the easy injectable composite materials with adjustable properties by incorporation of BIOPLAST® GS 2189 and spruce sawdust. Therefore, lightweight WPCs allow both to recycle wood industry byproducts and to produce a full ecologic material.

Keywords: biodegradability, color measurements, durability, mechanical properties, melt flow index, MFI, structural properties, thermal properties, wood-plastic composites, WPCs

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Authors: Fakhreldin O. Suliman, Alia H. Al-Battashi

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This work explored the interaction of three different imidazoline drugs, naphazoline nitrate (NPH), oxymetazoline hydrochloride (OXY) and xylometazoline hydrochloride (XYL) with two different synthesized cucurbit[n]urils CB[n], cucurbit[7]uril (CB[7]) and cucuribit[8]uril (CB[8]). Three binary inclusion complexes have been investigated in solution and in the solid state. The solid complexes were obtained by lyophilization, whereas the physical mixtures of guests and hosts at a stoichiometric ratio of 1:1 were obtained for each drug. 1HNMR, electrospray ionization mass spectrometry (ESI-MS), and matrix-assisted laser desorption-ionization time-of-flight (MALDI-TOF) mass spectrometry was used to study the complexes prepared in aqueous media. The lyophilized solid complexes were characterized by Fourier transform-infrared spectroscopy (FT-IR), powder X-ray diffractometry (PXRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). MS, FT-IR and PXRD experimental results established in this work reveal that NPH, OXY and XYL molecules form stable inclusion complexes with the two hosts. The TGA and DSC confirmed the enhancement of the thermal stability of each drug and the production of a thermally stable solid complex. The 1HNMR has shown that the protons of the guests faced shifting in ppm and broadening of their peaks upon the formation of inclusion complexes with the selected CB[n]. The aromatic protons of the guest exhibited the highest changes in the chemical shifts and shape of the NMR peaks, suggesting their inclusion into the cavity of the CB[n]. The diffusion coefficients (D), developed from the diffusion-controlled NMR Spectroscopy (DOSY) measurements, for the complexation of the selected imidazoline drugs with CB[7] and CB[8], were decreased in the presence of hosts compared to the free guests indicating the formation of the guest-host adduct. Furthermore, we conducted molecular dynamic simulations and quantum mechanics calculations on these complexes. The results of the theoretical study corroborate the experimental findings and have also shed light on the mechanism of inclusion of the guests into the two hosts. This study generates initial data for potential drug delivery or drug formulation systems for these three selected imidazoline drug compounds based on their inclusion into the CB[n] cavities.

Keywords: cucurbit[n]urils, imidazoline, inclusion complexes, molecular dynamics, DFT calculations, mass spectrometry

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Authors: Hana Hanaee-Ahvaz, Monika Cserjan-Puschmann, Christopher Tauer, Gerald Striedner

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Incorporation of noncanonical amino acids (ncAA) into proteins has become an interesting topic as proteins featured with ncAAs offer a wide range of different applications. Nowadays, technologies and systems exist that allow for the site-specific introduction of ncAAs in vivo, but the efficient production of proteins modified this way is still a big challenge. This is especially true for 'hard-to-express' proteins where low yields are encountered even with the native sequence. In this study, site-specific incorporation of azido-ethoxy-carbonyl-Lysin (azk) into an anti-tumor-necrosis-factor-α-Fab (FTN2) was investigated. According to well-established parameters, possible site positions for ncAA incorporation were determined, and corresponding FTN2 genes were constructed. Each of the modified FTN2 variants has one amber codon for azk incorporated either in its heavy or light chain. The expression level for all variants produced was determined by ELISA, and all azk variants could be produced with a satisfactory yield in the range of 50-70% of the original FTN2 variant. In terms of expression yield, neither the azk incorporation position nor the subunit modified (heavy or light chain) had a significant effect. We confirmed correct protein processing and azk incorporation by mass spectrometry analysis, and antigen-antibody interaction was determined by surface plasmon resonance analysis. The next step is to characterize the effect of azk incorporation on protein stability and aggregation tendency via differential scanning calorimetry and light scattering, respectively. In summary, the incorporation of ncAA into our Fab candidate FTN2 worked better than expected. The quantities produced allowed a detailed characterization of the variants in terms of their properties, and we can now turn our attention to potential applications. By using click chemistry, we can equip the Fabs with additional functionalities and make them suitable for a wide range of applications. We will now use this option in a first approach and develop an assay that will allow us to follow the degradation of the recombinant target protein in vivo. Special focus will be laid on the proteolytic activity in the periplasm and how it is influenced by cultivation/induction conditions.

Keywords: degradation, FTN2, hard-to-express protein, non-canonical amino acids

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Authors: Matthias Walluch, José Alberto Rodríguez, Christopher Giehl, Gunther Arnold, Daniela Ehgartner

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Dynamic mechanical analysis (DMA) is a powerful method to characterize viscoelastic properties and phase transitions for a wide range of materials. It is often used to characterize polymers and their temperature-dependent behavior, including thermal transitions like the glass transition temperature Tg, via determination of storage and loss moduli in tension (Young’s modulus, E) and shear or torsion (shear modulus, G) or other testing modes. While production and application temperatures for polymers are often limited to several hundred degrees, material properties of glasses usually require characterization at temperatures exceeding 600 °C. This contribution highlights a high temperature setup for rotational and oscillatory rheometry as well as for DMA in different modes. The implemented standard convection oven enables the characterization of glass in different loading modes at temperatures up to 950 °C. Three-point bending, tension and torsional measurements on different glasses, with E and G moduli as a function of frequency and temperature, are presented. Additional tests include superimposing several frequencies in a single temperature sweep (“multiwave”). This type of test results in a considerable reduction of the experiment time and allows to evaluate structural changes of the material and their frequency dependence. Furthermore, DMA in torsion and tension was performed to determine the complex Poisson’s ratio as a function of frequency and temperature within a single test definition. Tests were performed in a frequency range from 0.1 to 10 Hz and temperatures up to the glass transition. While variations in the frequency did not reveal significant changes of the complex Poisson’s ratio of the glass, a monotonic increase of this parameter was observed when increasing the temperature. This contribution outlines the possibilities of DMA in bending, tension and torsion for an extended temperature range. It allows the precise mechanical characterization of material behavior from room temperature up to the glass transition and the softening temperature interval. Compared to other thermo-analytical methods, like Dynamic Scanning Calorimetry (DSC) where mechanical stress is neglected, the frequency-dependence links measurement results (e.g. relaxation times) to real applications

Keywords: dynamic mechanical analysis, oscillatory rheometry, Poisson's ratio, solid glass, viscoelasticity

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Authors: Danilo A. F. Fontes, Magaly A. M.Lyra, Maria L. C. Moura, Leslie R. M. Ferraz, Salvana P. M. Costa, Amanda C. Q. M. Vieira, Larissa A. Rolim, Giovanna C. R. M. Schver, Ping I. Lee, Severino Alves-Júnior, José L. Soares-Sobrinho, Pedro J. Rolim-Neto

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Efavirenz (EFV) is a first-choice drug in antiretroviral therapy with high efficacy in the treatment of infection by Human Immunodeficiency Virus, which causes Acquired Immune Deficiency Syndrome (AIDS). EFV has low solubility in water resulting in a decrease in the dissolution rate and, consequently, in its bioavailability. Among the technological alternatives to increase solubility, the Lamellar Double Hydroxides (LDH) have been applied in the development of systems with poorly water-soluble drugs. The use of analytical techniques such as X-Ray Diffraction (XRD), Infrared Spectroscopy (IR) and Differential Scanning Calorimetry (DSC) allowed the elucidation of drug interaction with the lamellar compounds. The objective of this work was to characterize and develop the binary systems with EFV and LDH in order to increase the solubility of the drug. The LDH-CaAl was synthesized by the method of co-precipitation from salt solutions of calcium nitrate and aluminum nitrate in basic medium. The systems EFV-LDH and their physical mixtures (PM) were obtained at different concentrations (5-60% of EFV) using the solvent technique described by Takahashi & Yamaguchi (1991). The characterization of the systems and the PM’s was performed by XRD techniques, IR, DSC and dissolution test under non-sink conditions. The results showed improvements in the solubility of EFV when associated with LDH, due to a possible change in its crystal structure and formation of an amorphous material. From the DSC results, one could see that the endothermic peak at 173°C, temperature that correspond to the melting process of EFZ in the crystal form, was present in the PM results. For the EFZ-LDH systems (with 5, 10 and 30% of drug loading), this peak was not observed. XRD profiles of the PM showed well-defined peaks for EFV. Analyzing the XRD patterns of the systems, it was found that the XRD profiles of all the systems showed complete attenuation of the characteristic peaks of the crystalline form of EFZ. The IR technique showed that, in the results of the PM, there was the appearance of one band and overlap of other bands, while the IR results of the systems with 5, 10 and 30% drug loading showed the disappearance of bands and a few others with reduced intensity. The dissolution test under non-sink conditions showed that systems with 5, 10 and 30% drug loading promoted a great increase in the solubility of EFV, but the system with 10% of drug loading was the only one that could keep substantial amount of drug in solution at different pHs.

Keywords: Efavirenz, Lamellar Double Hydroxides, Pharmaceutical Techonology, Solubility

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Authors: Ahmed. Abdel Bary, Omneya. Khowessah, Mojahed. al-jamrah

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Introduction: The major challenge with the design of oral dosage forms lies with their poor bioavailability. The most frequent causes of low oral bioavailability are attributed to poor solubility and low permeability. The aim of this study was to develop solid nanodispersed tablet formulation of Glimepiride for the enhancement of the solubility and bioavailability. Methodology: Solid nanodispersions of Glimepiride (GMP) were prepared using two different ratios of 2 different carriers, namely; PEG6000, pluronic F127, and by adopting two different techniques, namely; solvent evaporation technique and fusion technique. A full factorial design of 2 3 was adopted to investigate the influence of formulation variables on the prepared nanodispersion properties. The best chosen formula of nanodispersed powder was formulated into tablets by direct compression. The Differential Scanning Calorimetry (DSC) analysis and Fourier Transform Infra-Red (FTIR) analysis were conducted for the thermal behavior and surface structure characterization, respectively. The zeta potential and particle size analysis of the prepared glimepiride nanodispersions was determined. The prepared solid nanodispersions and solid nanodispersed tablets of GMP were evaluated in terms of pre-compression and post-compression parameters, respectively. Results: The DSC and FTIR studies revealed that there was no interaction between GMP and all the excipients used. Based on the resulted values of different pre-compression parameters, the prepared solid nanodispersions powder blends showed poor to excellent flow properties. The resulted values of the other evaluated pre-compression parameters of the prepared solid nanodispersion were within the limits of pharmacopoeia. The drug content of the prepared nanodispersions ranged from 89.6 ± 0.3 % to 99.9± 0.5% with particle size ranged from 111.5 nm to 492.3 nm and the resulted zeta potential (ζ ) values of the prepared GMP-solid nanodispersion formulae (F1-F8) ranged from -8.28±3.62 mV to -78±11.4 mV. The in-vitro dissolution studies of the prepared solid nanodispersed tablets of GMP concluded that GMP- pluronic F127 combinations (F8), exhibited the best extent of drug release, compared to other formulations, and to the marketed product. One way ANOVA for the percent of drug released from the prepared GMP-nanodispersion formulae (F1- F8) after 20 and 60 minutes showed significant differences between the percent of drug released from different GMP-nanodispersed tablet formulae (F1- F8), (P<0.05). Conclusion: Preparation of glimepiride as nanodispersed particles proven to be a promising tool for enhancing the poor solubility of glimepiride.

Keywords: glimepiride, solid Nanodispersion, nanodispersed tablets, poorly water soluble drugs

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Authors: Florent Cerdan, Anne-Gaëlle Denay, Annette Roy, Jean-Claude Grandidier, Éric Laine

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The insulation of MarkIII membrane of the Liquid Natural Gas Carriers (LNGC) consists of a load- bearing system made of panels in reinforced polyurethane foam (R-PUF). During the shipping, the cargo containment shall be potentially subject to risk events which can be water leakage through the wall ballast tank. The aim of these present works is to further develop understanding of water transfer mechanisms and water effect on properties of R-PUF. This multi-scale approach contributes to improve the durability. Macroscale / Mesoscale Firstly, the use of the gravimetric technique has allowed to define, at room temperature, the water transfer mechanisms and kinetic diffusion, in the R-PUF. The solubility follows a first kinetic fast growing connected to the water absorption by the micro-porosity, and then evolves linearly slowly, this second stage is connected to molecular diffusion and dissolution of water in the dense membranes polyurethane. Secondly, in the purpose of improving the understanding of the transfer mechanism, the study of the evolution of the buoyant force has been established. It allowed to identify the effect of the balance of total and partial pressure of mixture gas contained in pores surface. Mesoscale / Microscale The differential scanning calorimetry (DSC) and Dynamical Mechanical Analysis (DMA), have been used to investigate the hydration of the hard and soft segments of the polyurethane matrix. The purpose was to identify the sensitivity of these two phases. It been shown that the glass transition temperatures shifts towards the low temperatures when the solubility of the water increases. These observations permit to conclude to a plasticization of the polymer matrix. Microscale The Fourier Transform Infrared (FTIR) study has been used to investigate the characterization of functional groups on the edge, the center and mid-way of the sample according the duration of submersion. More water there is in the material, more the water fix themselves on the urethanes groups and more specifically on amide groups. The pic of C=O urethane shifts at lower frequencies quickly before 24 hours of submersion then grows slowly. The intensity of the pic decreases more flatly after that.

Keywords: porous materials, water sorption, glass transition temperature, DSC, DMA, FTIR, transfer mechanisms

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Authors: I. Irska, S. Paszkiewicz, D. Pawlikowska, E. Piesowicz, A. Linares, T. A. Ezquerra

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Due to the number of advantages such as high tensile strength, sensitivity to hydrolytic degradation, and biocompatibility poly(lactic acid) (PLA) is one of the most common polyesters for biomedical and pharmaceutical applications. However, PLA is a rigid, brittle polymer with low heat distortion temperature and slow crystallization rate. In order to broaden the range of PLA applications, it is necessary to improve these properties. In recent years a number of new strategies have been evolved to obtain PLA-based materials with improved characteristics, including manipulation of crystallinity, plasticization, blending, and incorporation into block copolymers. Among the other methods, synthesis of aliphatic-aromatic copolyesters has been attracting considerable attention as they may combine the mechanical performance of aromatic polyesters with biodegradability known from aliphatic ones. Given the need for highly flexible biodegradable polymers, in this contribution, a series of aromatic-aliphatic based on poly(butylene terephthalate) and poly(lactic acid) (PBT-b-PLA) copolyesters exhibiting superior mechanical properties were copolymerized with an additional poly(tetramethylene oxide) (PTMO) soft block. The structure and properties of both series were characterized by means of attenuated total reflectance – Fourier transform infrared spectroscopy (ATR-FTIR), nuclear magnetic resonance spectroscopy (¹H NMR), differential scanning calorimetry (DSC), wide-angle X-ray scattering (WAXS) and dynamic mechanical, thermal analysis (DMTA). Moreover, the related changes in tensile properties have been evaluated and discussed. Lastly, the viscoelastic properties of synthesized poly(ester-ether) copolymers were investigated in detail by step cycle tensile tests. The block lengths decreased with the advance of treatment, and the block-random diblock terpolymers of (PBT-ran-PLA)-b-PTMO were obtained. DSC and DMTA analysis confirmed unambiguously that synthesized poly(ester-ether) copolymers are microphase-separated systems. The introduction of polyether co-units resulted in a decrease in crystallinity degree and melting temperature. X-ray diffraction patterns revealed that only PBT blocks are able to crystallize. The mechanical properties of (PBT-ran-PLA)-b-PTMO copolymers are a result of a unique arrangement of immiscible hard and soft blocks, providing both strength and elasticity.

Keywords: aliphatic-aromatic copolymers, multiblock copolymers, phase behavior, thermoplastic elastomers

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Authors: M. R. Vijayakumar, K. Priyanka, Ramoji Kosuru, Lakshmi, Sanjay Singh

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Trans resveratrol (RES) is a non-flavonoid poly-phenolic compound proved for its therapeutic and preventive effect against various types of cancer. However, the practical application of RES in cancer treatment is limited because of its higher dose (up to 7.5 g/day in humans), low biological half life, rapid metabolism and faster elimination in mammals. PEGylated core-shell type lipid polymer hybrid nanoparticles are the novel drug delivery systems for long circulation and improved anti cancer effect of its therapeutic payloads. Therefore, the main objective of this study is to extend the biological half life (long circulation) and improve the therapeutic efficacy of RES through core shell type of nanoparticles. D-α-tocopheryl polyethylene glycol 1000 succinate (vitamin E TPGS), a novel surfactant is applied for the preparation of PEGylated lipid polymer hybrid nanoparticles. The prepared nanoparticles were evaluated by various state of the art techniques such as dynamic light scattering (DLS) technique for particle size and zeta potential, TEM for shape, differential scanning calorimetry (DSC) for interaction analysis and XRD for crystalline changes of drug. Entrapment efficiency and invitro drug release were determined by ultracentrifugation method and dialysis bag method, respectively. Cancer cell viability studies were performed by MTT assay, respectively. Pharmacokinetic studies after i.v administration were performed in sprague dawley rats. The prepared NPs were found to be spherical in shape with smooth surfaces. Particle size and zeta potential of prepared NPs were found to be in the range of 179.2±7.45 to 266.8±9.61 nm and -0.63 to -48.35 mV, respectively. DSC revealed absence of potential interaction. XRD study revealed presence of amorphous form in nanoparticles. Entrapment efficiency was found to be 83.7 % and drug release was found to be in controlled manner. MTT assay showed low MEC and pharmacokinetic studies showed higher AUC of nanoformulaition than its pristine drug. All these studies revealed that the RES loaded PEG modified core-shell type lipid polymer hybrid nanoparticles can be an alternative tool for chemopreventive and therapeutic application of RES in cancer.

Keywords: trans resveratrol, cancer nanotechnology, long circulating nanoparticles, bioavailability enhancement, core shell nanoparticles, lipid polymer hybrid nanoparticles

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Authors: Ana Carolina Kogawa, Selma Gutierrez Antonio, Hérida Regina Nunes Salgado

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Rifaximin is an oral antimicrobial, gut - selective and not systemic with adverse effects compared to placebo. It is used for the treatment of hepatic encephalopathy, travelers diarrhea, irritable bowel syndrome, Clostridium difficile, ulcerative colitis and acute diarrhea. The crystalline form present in the rifaximin with minimal systemic absorption is α, being the amorphous form significantly different. Regulators are increasingly attention to polymorphisms. Polymorphs can change the form by altering the drug characteristics compromising the effectiveness and safety of the finished product. International Conference on Harmonization issued the ICH Guidance Q6A, which aim to improve the control of polymorphism in new and existing pharmaceuticals. The objective of this study was to obtain polymorphic forms of rifaximin employing recrystallization processes and characterize them by thermal analysis (thermogravimetry - TG and differential scanning calorimetry - DSC), X-ray diffraction, scanning electron microscopy and solubility test. Six polymorphic forms of rifaximin, designated I to VI were obtained by the crystallization process by evaporation of the solvent. The profiles of the TG curves obtained from polymorphic forms of rifaximin are similar to rifaximin and each other, however, the DTG are different, indicating different thermal behaviors. Melting temperature values of all the polymorphic forms were greater to that shown by the rifaximin, indicating the higher thermal stability of the obtained forms. The comparison of the diffractograms of the polymorphic forms of rifaximin with rifaximin α, β and γ constant in patent indicate that forms III, V and VI are formed by mixing polymorph β and α and form III is formed by polymorph β. The polymorphic form I is formed by polymorph β, but with a significant amount of amorphous material. Already, the polymorphic form II consists of polymorph γ, amorphous. In scanning electron microscope is possible to observe the heterogeneity of morphological characteristics of crystals of polymorphic forms among themselves and with rifaximin. The solubility of forms I and II was greater than the solubility of rifaximin, already, forms III, IV and V presented lower solubility than of rifaximin. Similarly, the bioavailability of the amorphous form of rifaximin is considered significantly higher than the form α, the polymorphic forms obtained in this work can not guarantee the excellent tolerability of the reference medicine. Therefore, studies like these are extremely important and they point to the need for greater requirements by the regulatory agencies competent about polymorphs analysis of the raw materials used in the manufacture of medicines marketed globally. These analyzes are not required in the majority of official compendia. Partnerships between industries, research centers and universities would be a viable way to consolidate researches in this area and contribute to improving the quality of solid drugs.

Keywords: electronic microscopy, polymorphism, rifaximin, solubility, X-ray diffraction

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Authors: Alberto A. Escobar Puentes, G. Adriana García, Luis F. Cuevas G., Alejandro P. Zepeda, Fernando B. Martínez, Susana A. Rincón

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Snack foods are usually classified as ‘junk food’ because have little nutritional value. However, due to the increase on the demand and third generation (3G) snacks market, low price and easy to prepare, can be considered as carriers of compounds with certain nutritional value. Resistant starch (RS) is classified as a prebiotic fiber it helps to control metabolic problems and has anti-cancer colon properties. The active compound can be developed by chemical cross-linking of starch with phosphate salts to obtain a type 4 resistant starch (RS4). The chemical reaction can be achieved by extrusion, a process widely used to produce snack foods, since it's versatile and a low-cost procedure. Starch is the major ingredient for snacks 3G manufacture, and the seeds of sorghum contain high levels of starch (70%), the most drought-tolerant gluten-free cereal. Due to this, the aim of this research was to develop a snack (3G), with RS4 in optimal conditions extrusion (previously determined) from sorghum starch, and carry on a sensory, chemically and structural characterization. A sample (200 g) of sorghum starch was conditioned with 4% sodium trimetaphosphate/ sodium tripolyphosphate (99:1) and set to 28.5% of moisture content. Then, the sample was processed in a single screw extruder equipped with rectangular die. The inlet, transport and output temperatures were 60°C, 134°C and 70°C, respectively. The resulting pellets were expanded in a microwave oven. The expansion index (EI), penetration force (PF) and sensory analysis were evaluated in the expanded pellets. The pellets were milled to obtain flour and RS content, degree of substitution (DS), and percentage of phosphorus (% P) were measured. Spectroscopy [Fourier Transform Infrared (FTIR)], X-ray diffraction, differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) analysis were performed in order to determine structural changes after the process. The results in 3G were as follows: RS, 17.14 ± 0.29%; EI, 5.66 ± 0.35 and PF, 5.73 ± 0.15 (N). Groups of phosphate were identified in the starch molecule by FTIR: DS, 0.024 ± 0.003 and %P, 0.35±0.15 [values permitted as food additives (<4 %P)]. In this work an increase of the gelatinization temperature after the crosslinking of starch was detected; the loss of granular and vapor bubbles after expansion were observed by SEM; By using X-ray diffraction, loss of crystallinity was observed after extrusion process. Finally, a snack (3G) was obtained with RS4 developed by extrusion technology. The sorghum starch was efficient for snack 3G production.

Keywords: extrusion, resistant starch, snack (3G), Sorghum

Procedia PDF Downloads 281

Authors: Devi Eka Septiyani Arifin, Jrjeng Ruan

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As an approach to manipulate the performance of polymer thin film, epitaxy crystallization within polymer blends of poly(vinylidene fluoride) (PVDF) and its copolymer poly(vinylidene fluoride-trifluoroethylene) P(VDF-TrFE) was studied in this research, which involves the competition between phase separation and crystal growth of constitutive semicrystalline polymers. The unique piezoelectric feature of poly(vinylidene fluoride) crystalline phase is derived from the packing of molecular chains in all-trans conformation, which spatially arranges all the substituted fluorene atoms on one side of the molecular chain and hydrogen atoms on the other side. Therefore, the net dipole moment is induced across the lateral packing of molecular chains. Nevertheless, due to the mutual repulsion among fluorene atoms, this all-trans molecular conformation is not stable, and ready to change above curie temperature, where thermal energy is sufficient to cause segmental rotation. This research attempts to explore whether the epitaxial interactions between piezoelectric crystals and crystal lattice of hexamethylbenzene (HMB) crystalline platelet is able to stabilize this metastable all-trans molecular conformation or not. As an aromatic crystalline compound, the melt of HMB was surprisingly found able to dissolve the poly(vinylidene fluoride), resulting in homogeneous eutectic solution. Thus, after quenching this binary eutectic mixture to room temperature, subsequent heating or annealing processes were designed to explore the involve phase separation and crystallization behavior. The phase transition behaviors were observed in-situ by X-ray diffraction and differential scanning calorimetry (DSC). The molecular packing was observed via transmission electron microscope (TEM) and the principles of electron diffraction were brought to study the internal crystal structure epitaxially developed within thin films. Obtained results clearly indicated the occurrence of heteroepitaxy of PVDF/PVDF-TrFE on HMB crystalline platelet. Both the concentration of poly(vinylidene fluoride) and the mixing ratios of these two constitutive polymers have been adopted as the influential factors for studying the competition between the epitaxial crystallization of PVDF and P(VDF-TrFE) on HMB crystalline. Furthermore, the involved epitaxial relationship is to be deciphered and studied as a potential factor capable of guiding the wide spread of piezoelectric crystalline form.

Keywords: epitaxy, crystallization, crystalline platelet, thin film and mixing ratio

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Authors: Z. Terzopoulou, I. Koliakou, D. Bikiaris

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Tissue engineering offers a new approach to regenerate diseased or damaged tissues such as bone. Great effort is devoted to eliminating the need of removing non-degradable implants at the end of their life span, with biodegradable polymers playing a major part. Poly(ε-caprolactone) (PCL) is one of the best candidates for this purpose due to its high permeability, good biodegradability and exceptional biocompatibility, which has stimulated extensive research into its potential application in the biomedical fields. However, PCL degrades much slower than other known biodegradable polymers and has a total degradation of 2-4 years depending on the initial molecular weight of the device. This is due to its relatively hydrophobic character and high crystallinity. Consequently, much attention has been given to the tunable degradation of PCL to meet the diverse requirements of biomedicine. Poly(ε-caprolactone) (PCL) is a biodegradable polyester that lacks bioactivity, so when used in bone tissue engineering, new bone tissue cannot bond tightly on the polymeric surface. Therefore, it is important to incorporate reinforcing fillers into PCL matrix in order to result in a promising combination of bioactivity, biodegradability, and strength. Natural clay halloysite nanotubes (HNTs) were incorporated into PCL polymeric matrix, via in situ ring-opening polymerization of caprolactone, in concentrations 0.5, 1 and 2.5 wt%. Both unmodified and modified with aminopropyltrimethoxysilane (APTES) HNTs were used in this study. The effect of nanofiller concentration and functionalization with end-amino groups on the physicochemical properties of the prepared nanocomposites was studied. Mechanical properties were found enhanced after the incorporation of nanofillers, while the modification increased further the values of tensile and impact strength. Thermal stability of PCL was not affected by the presence of nanofillers, while the crystallization rate that was studied by Differential Scanning Calorimetry (DSC) and Polarized Light Optical Microscopy (POM) increased. All materials were subjected to enzymatic hydrolysis in phosphate buffer in the presence of lipases. Due to the hydrophilic nature of HNTs, the biodegradation rate of nanocomposites was higher compared to neat PCL. In order to confirm the effect of hydrophilicity, contact angle measurements were also performed. In vitro biomineralization test confirmed that all samples were bioactive as mineral deposits were detected by X-ray diffractometry after incubation in SBF. All scaffolds were tested in relevant cell culture using osteoblast-like cells (MG-63) to demonstrate their biocompatibility

Keywords: biomaterials, nanocomposites, scaffolds, tissue engineering

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Authors: Elmira Ghanbari, Jan Van Esch, Stephen J. Picken, Sahil Aggarwal

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Low-molecular-weight organogelators form gels by self-assembly into the crystalline network which immobilizes the organic solvent. For single bisamide organogelator systems, the effect of the molecular structure on the molecular interaction and their self-assembly behavior has been explored. The spatial arrangement of bisamide molecules in the gel-state is driven by a combination of hydrogen bonding and Van der Waals interactions. The hydrogen-bonding pattern between the amide groups of bisamide molecules is regulated by the number of methylene spacers; the even number of methylene spacers between two amide groups, in even-spaced bisamides, leads to the antiparallel position of amide groups within a molecule. An even-spaced bisamide molecule with antiparallel amide groups can make two pairs of hydrogen bonding with the molecules on the same plane. The odd-spaced bisamide with a parallel directionality of amide groups can form four independent hydrogen bonds with four other bisamide molecules on different planes. The arrangement of bisamide molecules in the crystalline state and the interaction of these molecules depends on the molecular structure, particularly the parity of the spacer length between the amide groups in the bisamide molecule. In this study, the directionality of amide groups has been exploited as a structural characteristic to affect the arrangement of molecules in the crystalline state and produce different binary bisamide gelators with different degrees of crystallinities. Single odd- and even-spaced single bisamides were synthesized and blended to produce binary bisamide organogelators to be characterized in order to understand the effect of the different directionality of amide groups on the molecular interaction in the crystalline state. The pattern of molecular interactions between these blended molecules, mixing or phase separation, has been monitored via differential scanning calorimetry (DSC) and crystallography techniques; X-ray powder diffraction (XRD) and Small-angle X-ray scattering (SAXS). The formation of lamellar structures for odd- and even-spaced bisamide gelators was confirmed by using SAXS and XRD techniques. DSC results have shown that binary bisamide organogelators with different parity of methylene spacers (odd-even binary blends) have a higher tendency for phase separation compared to the binary bisamides with the same parity (odd-odd or even-even binary blends). Phase separation in binary odd-even bisamides was confirmed by the presence of individual (100) reflections of odd and even lamellar structures. The structural characteristic of bisamide organogelators, the parity of spacer length in binary systems, is a promising tool to control the arrangement of molecules and their crystalline structure.

Keywords: binary bisamide organogelators, crystalline structure, phase separation, self-assembly behavior

Procedia PDF Downloads 160

Authors: Weiliang Gong, Lissa Gomes, Lucile Raymond, Hui Xu, Werner Lutze, Ian L. Pegg

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Alkali-activated materials, particularly geopolymers, have attracted much interest in academia. Commercial applications are on the rise, as well. Geopolymers are produced typically by a reaction of one or two aluminosilicates with an alkaline solution at room temperature. Fly ash is an important aluminosilicate source. However, using low-Ca fly ash, the byproduct of burning hard or black coal reacts and sets slowly at room temperature. The development of mechanical durability, e.g., compressive strength, is slow as well. The use of fly ashes with relatively high contents ( > 6%) of unburned carbon, i.e., high loss on ignition (LOI), is particularly disadvantageous as well. This paper will show to what extent these impediments can be mitigated by mixing the fly ash with one or two more aluminosilicate sources. The fly ash used here is generated at the Orlando power plant (Florida, USA). It is low in Ca ( < 1.5% CaO) and has a high LOI of > 6%. The additional aluminosilicate sources are metakaolin and blast furnace slag. Binary fly ash-metakaolin and ternary fly ash-metakaolin-slag geopolymers were prepared. Properties of geopolymer pastes before and after setting have been measured. Fresh mixtures of aluminosilicates with an alkaline solution were studied by Vicat needle penetration, rheology, and isothermal calorimetry up to initial setting and beyond. The hardened geopolymers were investigated by SEM/EDS and the compressive strength was measured. Initial setting (fluid to solid transition) was indicated by a rapid increase in yield stress and plastic viscosity. The rheological times of setting were always smaller than the Vicat times of setting. Both times of setting decreased with increasing replacement of fly ash with blast furnace slag in a ternary fly ash-metakaolin-slag geopolymer system. As expected, setting with only Orlando fly ash was the slowest. Replacing 20% fly ash with metakaolin shortened the set time. Replacing increasing fractions of fly ash in the binary system by blast furnace slag (up to 30%) shortened the time of setting even further. The 28-day compressive strength increased drastically from < 20 MPa to 90 MPa. The most interesting finding relates to the calorimetric measurements. The use of two or three aluminosilicates generated significantly more heat (20 to 65%) than the calculated from the weighted sum of the individual aluminosilicates. This synergetic heat contributes or may be responsible for most of the increase of compressive strength of our binary and ternary geopolymers. The synergetic heat effect may be also related to increased incorporation of calcium in sodium aluminosilicate hydrate to form a hybrid (N,C)A-S-H) gel. The time of setting will be correlated with heat release and maximum heat flow.

Keywords: alkali-activated materials, binary and ternary geopolymers, blends of fly ash, metakaolin and blast furnace slag, rheology, synergetic heats

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Authors: Tamara Romero, Manuel Romero-Huelva, Jose V. Segarra, Jose Castro, Carlos Fernandez

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Many foods resulting from processing and manufacturing end up as waste, most of which is burned, dumped into landfills or used as compost, which leads to wasted resources, and environmental problems due to unsuitable disposal. Using residues of the crop and food processing industries to feed livestock has the advantage to obviating the need for costly waste management programs. The main residue generated in citrus cultivations and rice crop are pruning waste and rice straw, respectively. Within Spain, the Valencian Community is one of the world's oldest citrus and rice production areas. The objective of this experiment found out the effects of including orange leaves and rice straw as ingredients in the concentrate diets of goats, on milk production and methane (CH₄) emissions. Ten Murciano-Granadina dairy goats (45 kg of body weight, on average) in mid-lactation were selected in a crossover design experiment, where each goat received two treatments in 2 periods. Both groups were fed with 1.7 kg pelleted mixed ration; one group (n= 5) was a control (C) and the other group (n= 5) used orange leaves and rice straw (OR). The forage was alfalfa hay, and it was the same for the two groups (1 kg of alfalfa was offered by goat and day). The diets employed to achieve the requirements during lactation period for caprine livestock. The goats were allocated to individual metabolism cages. After 14 days of adaptation, feed intake and milk yield were recorded daily over a 5 days period. Physico-chemical parameters and somatic cell count in milk samples were determined. Then, gas exchange measurements were recorded individually by an open-circuit indirect calorimetry system using a head box. The data were analyzed by mixed model with diet and digestibility as fixed effect and goat as random effect. No differences were found for dry matter intake (2.23 kg/d, on average). Higher milk yield was found for C diet than OR (2.3 vs. 2.1 kg/goat and day, respectively) and, greater milk fat content was observed for OR than C (6.5 vs. 5.5%, respectively). The cheese extract was also greater in OR than C (10.7 vs. 9.6%). Goats fed OR diet produced significantly fewer CH₄ emissions than C diet (27 vs. 30 g/d, respectively). These preliminary results (LIFE Project LOWCARBON FEED LIFE/CCM/ES/000088) suggested that the use of these waste by-products was effective in reducing CH₄ emission without detrimental effect on milk yield.

Keywords: agricultural waste, goat, milk production, methane emission

Procedia PDF Downloads 118

Authors: Sara R. Knigge, Sugat R. Tuladhar, Hans-Klaus HöFfler, Tobias Schilling, Tim Kaufeld, Axel Haverich

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Tissue engineered (TE) heart valves based on degradable electrospun fiber scaffold represent a promising approach to overcome the known limitations of mechanical or biological prostheses. But the mechanical stress in the high-pressure system of the human circulation is a severe challenge for the delicate materials. Hence, the prediction of the scaffolds` in vivo degradation kinetics must be as accurate as possible to prevent fatal events in future animal or even clinical trials. Therefore, this study investigates whether long-term testing in full blood provides more meaningful results regarding the degradation behavior than conventional tests in simulated body fluids (SBF) or Phosphate Buffered Saline (PBS). Fiber mats were produced from a polycaprolactone (PCL)/tetrafluoroethylene solution by electrospinning. The morphology of the fiber mats was characterized via scanning electron microscopy (SEM). A maximum physiological degradation environment utilizing a test set-up with porcine full blood was established. The set-up consists of a reaction vessel, an oxygenator unit, and a roller pump. The blood parameters (pO2, pCO2, temperature, and pH) were monitored with an online test system. All tests were also carried out in the test circuit with SBF and PBS to compare conventional degradation media with the novel full blood setting. The polymer's degradation is quantified by SEM picture analysis, differential scanning calorimetry (DSC), and Raman spectroscopy. Tensile and cyclic loading tests were performed to evaluate the mechanical integrity of the scaffold. Preliminary results indicate that PCL degraded slower in full blood than in SBF and PBS. The uptake of water is more pronounced in the full blood group. Also, PCL preserved its mechanical integrity longer when degraded in full blood. Protein absorption increased during the degradation process. Red blood cells, platelets, and their aggregates adhered on the PCL. Presumably, the degradation led to a more hydrophilic polymeric surface which promoted the protein adsorption and the blood cell adhesion. Testing degradable implants in full blood allows for developing more reliable scaffold materials in the future. Material tests in small and large animal trials thereby can be focused on testing candidates that have proven to function well in an in-vivo-like setting.

Keywords: Electrospun scaffold, full blood degradation test, long-term polymer degradation, tissue engineered aortic heart valve

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Authors: Raj Kumar, Prem Felix Siril

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The poor aqueous solubility of many pharmaceutical drugs and potential drug candidates is a big challenge in drug development. Nanoformulation of such candidates is one of the major solutions for the delivery of such drugs. We initially developed the evaporation assisted solvent-antisolvent interaction (EASAI) method. EASAI method is use full to prepared nanoparticles of poor water soluble drugs with spherical morphology and particles size below 100 nm. However, to further improve the effect formulation to reduce number of dose and side effect it is important to control the delivery of drugs. However, many drug delivery systems are available. Among the many nano-drug carrier systems, solid lipid nanoparticles (SLNs) have many advantages over the others such as high biocompatibility, stability, non-toxicity and ability to achieve controlled release of drugs and drug targeting. SLNs can be administered through all existing routes due to high biocompatibility of lipids. SLNs are usually composed of lipid, surfactant and drug were encapsulated in lipid matrix. A number of non-steroidal anti-inflammatory drugs (NSAIDs) have poor bioavailability resulting from their poor aqueous solubility. In the present work, SLNs loaded with NSAIDs such as Nabumetone (NBT), Ketoprofen (KP) and Ibuprofen (IBP) were successfully prepared using different lipids and surfactants. We studied and optimized experimental parameters using a number of lipids, surfactants and NSAIDs. The effect of different experimental parameters such as lipid to surfactant ratio, volume of water, temperature, drug concentration and sonication time on the particles size of SLNs during the preparation using hot-melt sonication was studied. It was found that particles size was directly proportional to drug concentration and inversely proportional to surfactant concentration, volume of water added and temperature of water. SLNs prepared at optimized condition were characterized thoroughly by using different techniques such as dynamic light scattering (DLS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and differential scanning calorimetry and Fourier transform infrared spectroscopy (FTIR). We successfully prepared the SLN of below 220 nm using different lipids and surfactants combination. The drugs KP, NBT and IBP showed 74%, 69% and 53% percentage of entrapment efficiency with drug loading of 2%, 7% and 6% respectively in SLNs of Campul GMS 50K and Gelucire 50/13. In-vitro drug release profile of drug loaded SLNs is shown that nearly 100% of drug was release in 6 h.

Keywords: nanoparticles, delivery, solid lipid nanoparticles, hot-melt sonication, poor water soluble drugs, solubility, bioavailability

Procedia PDF Downloads 288

Authors: Osman Adiguzel

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Shape memory effect is a peculiar property exhibited by certain alloy systems and based on martensitic transformation, and shape memory properties are closely related to the microstructures of the material. Shape memory effect is linked with martensitic transformation, which is a solid state phase transformation and occurs with the cooperative movement of atoms by means of lattice invariant shears on cooling from high-temperature parent phase. Lattice twinning and detwinning can be considered as elementary processes activated during the transformation. Thermally induced martensite occurs as martensite variants, in self-accommodating manner and consists of lattice twins. Also, this martensite is called the twinned martensite or multivariant martensite. Deformation of shape memory alloys in martensitic state proceeds through a martensite variant reorientation. The martensite variants turn into the reoriented single variants with deformation, and the reorientation process has great importance for the shape memory behavior. Copper based alloys exhibit this property in metastable β- phase region, which has DO3 –type ordered lattice in ternary case at high temperature, and these structures martensiticaly turn into the layered complex structures with lattice twinning mechanism, on cooling from high temperature parent phase region. The twinning occurs as martensite variants with lattice invariant shears in two opposite directions, <110 > -type directions on the {110}- type plane of austenite matrix. Lattice invariant shear is not uniform in copper based ternary alloys and gives rise to the formation of unusual layered structures, like 3R, 9R, or 18R depending on the stacking sequences on the close-packed planes of the ordered lattice. The unit cell and periodicity are completed through 18 atomic layers in case of 18R-structure. On the other hand, the deformed material recovers the original shape on heating above the austenite finish temperature. Meanwhile, the material returns to the twinned martensite structures (thermally induced martensite structure) in one way (irreversible) shape memory effect on cooling below the martensite finish temperature, whereas the material returns to the detwinned martensite structure (deformed martensite) in two-way (reversible) shape memory effect. Shortly one can say that the microstructural mechanisms, responsible for the shape memory effect are the twinning and detwinning processes as well as martensitic transformation. In the present contribution, x-ray diffraction, transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) studies were carried out on two copper-based ternary alloys, CuZnAl, and CuAlMn.

Keywords: shape memory effect, martensitic transformation, twinning and detwinning, layered structures

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Authors: Adriana Garcia G., Alberto A. Escobar P., Amira D. Calvo L., Gabriel Lizama U., Alejandro Zepeda P., Fernando Martínez B., Susana Rincón A.

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Different studies have recently been focused on the use of antioxidants such as polyphenols because of to its anticarcinogenic capacity. However, these compounds are highly sensible to environmental factors such as light and heat, so lose its long-term stability, besides possess an astringent and bitter taste. Nevertheless, the polyphenols can be protected by microcapsule formulation. In this sense, a rich source of polyphenols is sorghum, besides presenting a high starch content. Due to the above, the aim of this work was to obtain modified starches from sorghum by extrusion to encapsulate polyphenols the sorghum by spray drying. Polyphenols were extracted by ethanol solution from sorghum (Pajarero/red) and determined by the method of Folin-Ciocalteu, obtaining GAE at 30 mg/g. Moreover, was extracted starch of sorghum (Sinaloense/white) through wet milling (yield 32 %). The hydrolyzed starch was modified with three treatments: acetic anhydride (2.5g/100g), sodium tripolyphosphate (4g/100g), and sodium tripolyphosphate/ acetic anhydride (2g/1.25g by each 100 g) by extrusion. Processing conditions of extrusion were as follows: barrel temperatures were of 60, 130 and 170 °C at the feeding, transition, and high-pressure extrusion zones, respectively. Analysis of Fourier Transform Infrared spectroscopy (FTIR), showed bands exhibited of acetyl groups (1735 cm-1) and phosphates (1170 cm-1, 910 cm-1 and 525 cm-1), indicating the respective modification of starch. Besides, all modified starches not developed viscosity, which is a characteristic required for use in the encapsulation of polyphenols using the spray drying technique. As result of the modification starch, was obtained a water solubility index (WSI) from 33.8 to 44.8 %, and crystallinity from 8 to 11 %, indicating the destruction of the starch granule. Afterwards, microencapsulation of polyphenols was developed by spray drying, with a blend of 10 g of modified starch, 60 ml polyphenol extract and 30 ml of distilled water. Drying conditions were as follows: inlet air temperature 150 °C ± 1, outlet air temperature 80°C ± 5. As result of the microencapsulation: were obtained yields of 56.8 to 77.4 % and an efficiency of encapsulation from 84.6 to 91.4 %. The FTIR analysis showed evidence of microcapsules loaded with polyphenols in bands 1042 cm-1, 1038 cm-1 and 1148 cm-1. Analysis Differential scanning calorimetry (DSC) showed transition temperatures from 144.1 to 173.9 °C. For the order hand, analysis of Scanning Electron Microscopy (SEM), were observed rounded surfaces with concavities, typical feature of microcapsules produced by spray drying, how result of rapid evaporation of water. Finally, the modified starches were obtained by extrusion with good characteristics for use as cover materials by spray drying, where the phosphorylated starch was the best treatment in this work, according to the encapsulation yield, efficiency, and transition temperature.

Keywords: encapsulation, extrusion, modified starch, polyphenols, spray drying

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Authors: A. J. Cobley, L. Krishnan

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The demand for multi-functional lightweight materials in sectors such as automotive, aerospace, electronics is growing, and for this reason fibre-reinforced, epoxy polymer composites are being widely utilized. The fibre reinforcing material is mainly responsible for the strength and stiffness of the composites whilst the main role of the epoxy polymer matrix is to enhance the load distribution applied on the fibres as well as to protect the fibres from the effect of harmful environmental conditions. The superior properties of the fibre-reinforced composites are achieved by the best properties of both of the constituents. Although factors such as the chemical nature of the epoxy and how it is cured will have a strong influence on the properties of the epoxy matrix, the method of mixing and degassing of the resin can also have a significant impact. The production of a fibre-reinforced epoxy polymer composite will usually begin with the mixing of the epoxy pre-polymer with a hardener and accelerator. Mechanical methods of mixing are often employed for this stage but such processes naturally introduce air into the mixture, which, if it becomes entrapped, will lead to voids in the subsequent cured polymer. Therefore, degassing is normally utilised after mixing and this is often achieved by placing the epoxy resin mixture in a vacuum chamber. Although this is reasonably effective, it is another process stage and if a method of mixing could be found that, at the same time, degassed the resin mixture this would lead to shorter production times, more effective degassing and less voids in the final polymer. In this study the effect of four different methods for mixing and degassing of the pre-polymer with hardener and accelerator were investigated. The first two methods were manual stirring and magnetic stirring which were both followed by vacuum degassing. The other two techniques were ultrasonic mixing/degassing using a 40 kHz ultrasonic bath and a 20 kHz ultrasonic probe. The cured cast resin samples were examined under scanning electron microscope (SEM), optical microscope, and Image J analysis software to study morphological changes, void content and void distribution. Three point bending test and differential scanning calorimetry (DSC) were also performed to determine the thermal and mechanical properties of the cured resin. It was found that the use of the 20 kHz ultrasonic probe for mixing/degassing gave the lowest percentage voids of all the mixing methods in the study. In addition, the percentage voids found when employing a 40 kHz ultrasonic bath to mix/degas the epoxy polymer mixture was only slightly higher than when magnetic stirrer mixing followed by vacuum degassing was utilized. The effect of ultrasonic mixing/degassing on the thermal and mechanical properties of the cured resin will also be reported. The results suggest that low frequency ultrasound is an effective means of mixing/degassing a pre-polymer mixture and could enable a significant reduction in production times.

Keywords: degassing, low frequency ultrasound, polymer composites, voids

Procedia PDF Downloads 273

Authors: Franciele L. Bernard, Felipe Dalla Vecchia, Barbara B. Polesso, Jose A. Donato, Marcus Seferin, Rosane Ligabue, Jailton F. do Nascimento, Sandra Einloft

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The increasing level of carbon dioxide concentration in the atmosphere related to fossil fuels processing and utilization are contributing to global warming phenomena considerably. Carbon capture and storage (CCS) technologies appear as one of the key technologies to reduce CO2 emissions mitigating the effects of climate change. Absorption using amines solutions as solvents have been extensively studied and used in industry for decades. However, solvent degradation and equipment corrosion are two of the main problems in this process. Poly (ionic liquid) (PIL) is considered as a promising material for CCS technology, potentially more environmentally friendly and lesser energy demanding than traditional material. PILs possess a unique combination of ionic liquids (ILs) features, such as affinity for CO2, thermal and chemical stability and adjustable properties, coupled with the intrinsic properties of the polymer. This study investigated new Poly (ionic liquid) (PIL) based on polyurethanes with different ionic liquids cations and its potential for CO2 capture. The PILs were synthesized by the addition of diisocyante to a difunctional polyol, followed by an exchange reaction with the ionic Liquids 1-butyl-3-methylimidazolium chloride (BMIM Cl); tetrabutylammonium bromide (TBAB) and tetrabutylphosphonium bromide (TBPB). These materials were characterized by Fourier transform infrared spectroscopy (FTIR), Proton Nuclear Magnetic Resonance (1H-NMR), Atomic force microscopy (AFM), Tensile strength analysis, Field emission scanning electron microscopy (FESEM), Thermogravimetric analysis (TGA), Differential scanning calorimetry (DSC). The PILs CO2 sorption capacity were gravimetrically assessed in a Magnetic Suspension Balance (MSB). It was found that the ionic liquids cation influences in the compounds properties as well as in the CO2 sorption. The best result for CO2 sorption (123 mgCO2/g at 30 bar) was obtained for the PIL (PUPT-TBA). The higher CO2 sorption in PUPT-TBA is probably linked to the fact that the tetraalkylammonium cation having a higher positive density charge can have a stronger interaction with CO2, while the imidazolium charge is delocalized. The comparative CO2 sorption values of the PUPT-TBA with different ionic liquids showed that this material has greater capacity for capturing CO2 when compared to the ILs even at higher temperature. This behavior highlights the importance of this study, as the poly (urethane) based PILs are cheap and versatile materials.

Keywords: capture, CO2, ionic liquids, ionic poly(urethane)

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Authors: Sudhir Kumar, V. R. Sinha

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Background: The topical and systemic toxicity associated with present nonmelanoma skin cancer (NMSC) treatment therapy using 5-Fluorouracil (5-FU) make it necessary to develop a novel delivery system having lesser toxicity and better control over drug release. Solid lipid nanoparticles offer many advantages like: controlled and localized release of entrapped actives, nontoxicity, and better tolerance. Aim:-To investigate safety and efficacy of 5-FU loaded solid lipid nanoparticles as a topical delivery system for the treatment of nonmelanoma skin cancer. Method: Topical solid lipid nanoparticles of 5-FU were prepared using Compritol 888 ATO (Glyceryl behenate) as lipid component and pluronic F68 (Poloxamer 188), Tween 80 (Polysorbate 80), Tyloxapol (4-(1,1,3,3-Tetramethylbutyl) phenol polymer with formaldehyde and oxirane) as surfactants. The SLNs were prepared with emulsification method. Different formulation parameters viz. type and ratio of surfactant, ratio of lipid and ratio of surfactant:lipid were investigated on particle size and drug entrapment efficiency. Results: Characterization of SLNs like–Transmission Electron Microscopy (TEM), Differential Scannig calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), Particle size determination, Polydispersity index, Entrapment efficiency, Drug loading, ex vivo skin permeation and skin retention studies, skin irritation and histopathology studies were performed. TEM results showed that shape of SLNs was spherical with size range 200-500nm. Higher encapsulation efficiency was obtained for batches having higher concentration of surfactant and lipid. It was found maximum 64.3% for SLN-6 batch with size of 400.1±9.22 nm and PDI 0.221±0.031. Optimized SLN batches and marketed 5-FU cream were compared for flux across rat skin and skin drug retention. The lesser flux and higher skin retention was obtained for SLN formulation in comparison to topical 5-FU cream, which ensures less systemic toxicity and better control of drug release across skin. Chronic skin irritation studies lacks serious erythema or inflammation and histopathology studies showed no significant change in physiology of epidermal layers of rat skin. So, these studies suggest that the optimized SLN formulation is efficient then marketed cream and safer for long term NMSC treatment regimens. Conclusion: Topical and systemic toxicity associated with long-term use of 5-FU, in the treatment of NMSC, can be minimized with its controlled release with significant drug retention with minimal flux across skin. The study may provide a better alternate for effective NMSC treatment.

Keywords: 5-FU, topical formulation, solid lipid nanoparticles, non melanoma skin cancer

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Authors: Patrícia Severino, Luciana Nalone, Daniele Martins, Marco Chaud, Classius Ferreira, Cristiane Bani, Ricardo Albuquerque

Abstract:

Hydrogels produced with polymers have been used in the development of dressings for wound treatment and tissue revitalization. Our study on polymer nanocomposites containing silver nanoparticles shows antimicrobial activity and applications in wound healing. The effects are linked with the slow oxidation and Ag⁺ liberation to the biological environment. Furthermore, bacterial cell membrane penetration and metabolic disruption through cell cycle disarrangement also contribute to microbial cell death. The silver antimicrobial activity has been known for many years, and previous reports show that low silver concentrations are safe for human use. This work aims to develop a hydrogel using natural polymers (sodium alginate and gelatin) combined with silver nanoparticles for wound healing and with antimicrobial properties in cutaneous lesions. The hydrogel development utilized different sodium alginate and gelatin proportions (20:80, 50:50 and 80:20). The silver nanoparticles incorporation was evaluated at the concentrations of 1.0, 2.0 and 4.0 mM. The physico-chemical properties of the formulation were evaluated using ultraviolet-visible (UV-Vis) absorption spectroscopy, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric (TG) analysis. The morphological characterization was made using transmission electron microscopy (TEM). Human fibroblast (L2929) viability assay was performed with a minimum inhibitory concentration (MIC) assessment as well as an in vivo cicatrizant test. The results suggested that sodium alginate and gelatin in the (80:20) proportion with 4 mM of AgNO₃ in the (UV-Vis) exhibited a better hydrogel formulation. The nanoparticle absorption spectra of this analysis showed a maximum band around 430 - 450 nm, which suggests a spheroidal form. The TG curve exhibited two weight loss events. DSC indicated one endothermic peak at 230-250 °C, due to sample fusion. The polymers acted as stabilizers of a nanoparticle, defining their size and shape. Human fibroblast viability assay L929 gave 105 % cell viability with a negative control, while gelatin presented 96% viability, alginate: gelatin (80:20) 96.66 %, and alginate 100.33 % viability. The sodium alginate:gelatin (80:20) exhibited significant antimicrobial activity, with minimal bacterial growth at a ratio of 1.06 mg.mL⁻¹ in Pseudomonas aeruginosa and 0.53 mg.mL⁻¹ in Staphylococcus aureus. The in vivo results showed a significant reduction in wound surface area. On the seventh day, the hydrogel-nanoparticle formulation reduced the total area of injury by 81.14 %, while control reached a 45.66 % reduction. The results suggest that silver-hydrogel nanoformulation exhibits potential for wound dressing therapeutics.

Keywords: nanocomposite, wound healing, hydrogel, silver nanoparticle

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Authors: Joanna Gerszon, Aleksandra Rodacka

Abstract:

In the pathogenesis of neurodegenerative diseases such as Alzheimer's disease and Parkinson's disease, protein and peptide aggregation processes play a vital role in contributing to the formation of intracellular and extracellular protein deposits. One of the major components of these deposits is the oxidatively modified glyceraldehyde-3-phosphate dehydrogenase (GAPDH). Therefore, the purpose of this research was to answer the question whether piceatannol, a stilbene derivative, counteracts and/or slows down oxidative stress-induced GAPDH aggregation. The study also aimed to determine if this natural occurring compound prevents unfavorable nuclear translocation of GAPDH in hippocampal cells. The isothermal titration calorimetry (ITC) analysis indicated that one molecule of GAPDH can bind up to 8 molecules of piceatannol (7.3 ± 0.9). As a consequence of piceatannol binding to the enzyme, the loss of activity was observed. Parallel with GAPDH inactivation the changes in zeta potential, and loss of free thiol groups were noted. Nevertheless, the ligand-protein binding does not influence the secondary structure of the GAPDH. Precise molecular docking analysis of the interactions inside the active center allowed to presume that these effects are due to piceatannol ability to assemble a covalent binding with nucleophilic cysteine residue (Cys149) which is directly involved in the catalytic reaction. Molecular docking also showed that simultaneously 11 molecules of ligand can be bound to dehydrogenase. Taking into consideration obtained data, the influence of piceatannol on level of GAPDH aggregation induced by excessive oxidative stress was examined. The applied methods (thioflavin-T binding-dependent fluorescence as well as microscopy methods - transmission electron microscopy, Congo Red staining) revealed that piceatannol significantly diminishes level of GAPDH aggregation. Finally, studies involving cellular model (Western blot analyses of nuclear and cytosolic fractions and confocal microscopy) indicated that piceatannol-GAPDH binding prevents GAPDH from nuclear translocation induced by excessive oxidative stress in hippocampal cells. In consequence, it counteracts cell apoptosis. These studies demonstrate that by binding with GAPDH, piceatannol blocks cysteine residue and counteracts its oxidative modifications, that induce oligomerization and GAPDH aggregation as well as it prevents hippocampal cells from apoptosis by retaining GAPDH in the cytoplasm. All these findings provide a new insight into the role of piceatannol interaction with GAPDH and present a potential therapeutic strategy for some neurological disorders related to GAPDH aggregation. This work was supported by the by National Science Centre, Poland (grant number 2017/25/N/NZ1/02849).

Keywords: glyceraldehyde-3-phosphate dehydrogenase, neurodegenerative disease, neuroprotection, piceatannol, protein aggregation

Procedia PDF Downloads 138

Authors: Ojas Chaudhari, Ali Nejad Ghafar, Giedrius Zirgulis, Marjan Mousavi, Tommy Ellison, Sandra Pousette, Patrick Fontana

Abstract:

In Swedish tunnel construction, a critical issue that has been repeatedly acknowledged is corrosion and, consequently, failure of the rock bolts in rock support systems. The defective installation of rock bolts results in the formation of cavities in the cement mortar that is regularly used to fill the area under the dome plates. These voids allow for water-ingress to the rock bolt assembly, which results in corrosion of rock bolt components and eventually failure. In addition, the current installation technique consists of several manual steps with intense labor works that are usually done in uncomfortable and exhausting conditions, e.g., under the roof of the tunnels. Such intense tasks also lead to a considerable waste of materials and execution errors. Moreover, adequate quality control of the execution is hardly possible with the current technique. To overcome these issues, a non-shrinking/expansive cement-based mortar filled in the paper packaging has been developed in this study which properly fills the area under the dome plates without or with the least remaining cavities, ultimately that diminishes the potential of corrosion. This article summarizes the development process and the experimental evaluation of this technique for the installation of rock bolts. In the development process, the cementitious mortar was first developed using specific cement and shrinkage reducing/expansive additives. The mechanical and flow properties of the mortar were then evaluated using compressive strength, density, and slump flow measurement methods. In addition, isothermal calorimetry and shrinkage/expansion measurements were used to elucidate the hydration and durability attributes of the mortar. After obtaining the desired properties in both fresh and hardened conditions, the developed dry mortar was filled in specific permeable paper packaging and then submerged in water bath for specific intervals before the installation. The tests were enhanced progressively by optimizing different parameters such as shape and size of the packaging, characteristics of the paper used, immersion time in water and even some minor characteristics of the mortar. Finally, the developed prototype was tested in a lab-scale rock bolt assembly with various angles to analyze the efficiency of the method in real life scenario. The results showed that the new technique improves the performance of the rock bolts by reducing the material wastage, improving environmental performance, facilitating and accelerating the labor works, and finally enhancing the durability of the whole system. Accordingly, this approach provides an efficient alternative for the traditional way of tunnel bolt installation with considerable advantages for the Swedish tunneling industry.

Keywords: corrosion, durability, mortar, rock bolt

Procedia PDF Downloads 87