Search results for: non aqueous solvent

Authors: Abdel Ghany F. Shoair, Mai M. A. H. Shanab

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The basic aqueous systems NiSO4.6H₂O / K₂S₂O₈ (PH= 14) or NiSO₄.6H₂O / KBrO₃ (PH = 11.5) were ‎investigated ‎for the ‎catalytic conversion benzyl alcohol and ‎some para-substituted benzyl ‎alcohols to their ‎corresponding ‎acids in 75-97 % yield at room ‎temperature. The active species ‎was isolated and characterized by scanning ‎electron ‎microscopy (SEM), ‎‎transmission electron microscopy (TEM), X-ray ‎powder diffraction, EDX and ‎‎FT-IR ‎techniques and identified as NiO₂ nanoparticles (NPNPs). The SEM and ‎TEM images of nickel peroxide samples show a fine spherical-like ‎aggregation of ‎NiO₂ molecules with a nearly homogeneous partial size and confirm the ‎aggregation's size ‎to ‎be in the range of 2-3 nm. The yields, turnover (TO) and turn ‎over frequencies (TOF) were calculated. ‎It was noticed ‎that the aromatic alcohols ‎containing para-substituted electron donation groups gave better ‎‎yields than ‎those having electron-withdrawing groups. The optimum conditions for this ‎‎catalytic reaction ‎were studied using benzyl alcohol as a model. The mechanism ‎of the ‎catalytic conversion reaction was ‎suggested, in which the produced ‎(NPNPs) convert alcohols ‎to acids in two steps through the formation of the ‎‎corresponding aldehyde. The produced ‎NiO, because of this conversion, is ‎converted again to (NPNPs) by ‎an excess of K₂S₂O₈ or KBrO₃. This ‎catalytic cycle continues ‎until all the substrate is oxidized.

Keywords: Nickel, oxidation, catalysts, benzyl alcohol

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Authors: M. S. Abd El-Sadek, Mahmoud A. Omar, Gharib M. Taha

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Photodegradation of methylene blue in the presence of tin dioxide (SnO₂) nanoparticles under solar light irradiation are known to be an effective photocatalytic process. In this study, pure and silver (Ag) doped tin dioxide (SnO₂) nanoparticles were prepared at calcination temperature (800ºC) by a modified sol-gel method and studied for their photocatalytic activity with methylene blue as a test contaminant. The characterization of undoped and doped SnO₂ photocatalyst was studied by X-rays diffraction patterns (XRD), transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR) and Energy Dispersive X-ray Microanalysis (EDX). The catalytic degradation of methylene blue in aqueous media was studied using UV-Vis spectrophotometer to monitor the degradation process by measuring its absorption spectra. The main absorption peak of methylene blue is observed at λ= 664 nm. The change in the percent of silver in the catalyst affects the photoactivity of SnO₂ on the degradation of methylene blue. The photoactivity of pure SnO₂ was found to be a maximum at dose 0.2 gm of the catalyst with 100 ml of 5 ppm methylene blue in the water. Within 210 min of photodegradation (under sunlight) after leaving the reaction for 90 minutes in the dark to avoid the effect of adsorption, the pure SnO₂ at calcination temperature 800ºC exhibited the best photocatalytic degradation with removal percentage of 93.66% on methylene blue degradation under solar light.

Keywords: SnO₂ nanoparticles, methylene blue degradation, photocatalysis, silver doped-SnO₂

Procedia PDF Downloads 142

Authors: Saleh Alkarri, Melinda Frame, Dimple Sharma, John Cairney, Lee Maddan, Jin H. Kim, Jonathan O. Rayner, Teresa M. Bergholz, Muhammad Rabnawaz

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Reported herein is an investigation of anti-bacterial and anti-virus properties, mode of action of Mg(OH)₂ and copper-infused Mg(OH)₂ nanoplatelets (NPs) on melt-compounded and thermally embossed polypropylene (PP) surfaces. The anti-viral activity for the NPs was studied in aqueous liquid suspensions against SARS-CoV-2, and the mode of action was investigated on neat NPs and PP samples that were thermally embossed with NPs. Anti-bacterial studies for melt-compounded NPs in PP confirmed approximately 1 log reduction of E. coli populations in 24 h, while for thermally embossed NPs, an 8 log reduction of E. coli populations was observed. In addition, the NPs exhibit anti-viral activity against SARS-CoV-2. Fluorescence microscopy revealed that reactive oxygen species (ROS) is the main mode of action through which Mg(OH)₂ and Cu-Infused Mg(OH)₂act against microbes. Plastics with anti-microbial surfaces from where biocides are non-leachable are highly desirable. This work provides a general fabrication strategy for developing anti-microbial plastic surfaces.

Keywords: anti-microbial activity, E. coli K-12 MG1655, anti-viral activity, SARS-CoV-2, copper-infused magnesium hydroxide, non-leachable, ROS, compounding, surface embossing, dyes

Procedia PDF Downloads 66

Authors: Fatemeh Kourkinejad Gharaei, Tahereh Safari, Zahra Saebinasab

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Metabolic syndrome (MetS) is a set of risk factors associated with cardiovascular diseases, atherosclerosis, and type 2 diabetes. Nonalcoholic fatty liver disease (NAFLD) is the most important liver disorder in metabolic syndrome. High fructose consumption increases the risk of NAFLD. Eugenol shows anti-thrombotic, insulin-sensitive, fat-reducing effects. This study was designed to investigate the protective role of eugenol in NAFLD caused by metabolic syndrome. Methods: Thirty male Wistar rats were randomly divided into five groups; group 1, drinking water intake animals; group 2, fructose, group 3, fructose+eugenol solvent; group 4, fructose+ eugenol 50mg/kg and group 5, fructose+ eugenol 100mg/kg. At the end of the experiment, after 12 hours of fasting and under anesthesia, blood samples were taken for measurement of fast blood glucose (FBS), SGOT, AGPT, LDL, HDL, cholesterol, triglyceride. Results: FBG significantly increased in group 2 compared to group 1 (p < 0.001); however, it significantly decreased in groups 4 and 5 compared to group 2 (p < 0.05). SGOT and SGPT levels significantly increased in group 2 compared to drinking water alone (p < 0.001). However, SGOT and SGPT levels significantly decreased in groups 4 and 5. MDA and LTDS significantly increased in group 2 compared with drinking water alone (p < 0.01), while MDA and LTDS decreased in 4 and 5 groups compared to group 2 (p < 0.05), which confirms the pathology results related to the liver damage. Conclusion: Eugenol has protective effects on the liver and fat accumulation in liver cells.

Keywords: eugenol, fructose, metabolic syndrome, nonalcoholic fatty liver disease

Procedia PDF Downloads 124

Authors: N. P. G. N. Chandrasekara, R. M. Pashley

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Ion exchange (IEX) resins are commonly available as cationic or anionic resins but not as polyampholytic resins. This is probably because sequential acid and base washing cannot produce complete regeneration of polyampholytic resins with chemically attached anionic and cationic groups in close proximity. The ‘Sirotherm’ process, developed by the Commonwealth Scientific and Industrial Research Organization (CSIRO) in Melbourne, Australia was originally based on the use of a physical mixture of weakly basic (WB) and weakly acidic (WA) ion-exchange resin beads. These resins were regenerated thermally and they were capable of removing salts from an aqueous solution at higher temperatures compared to the salt sorbed at ambient temperatures with a significant reduction of the sorption capacity with increasing temperature. A new process for the efficient regeneration of mixed bead resins using ammonium bicarbonate with heat was studied recently and this chemical/thermal regeneration technique has the capability for completely regenerating polyampholytic resins. Even so, the low IEX capacities of polyampholytic resins restrict their commercial applications. Recently, we have established another novel process for increasing the IEX capacity of a typical polyampholytic resin. In this paper we will discuss the chemical/thermal regeneration of a polyampholytic (WA/WB) resin and a novel process for enhancing its ion exchange capacity, by increasing its internal pore area. We also show how effective this method is for completely recycled regeneration, with the potential of substantially reducing chemical waste.

Keywords: capacity, ion exchange, polyampholytic resin, regeneration

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Authors: Ahmed Alkarimi, Kevin Welham

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Organic mixed mode monolithic columns were fabricated from; glycidyl methacrylate-co-ethylene dimethacrylate-co-stearyl methacrylate, using glycidyl methacrylate and stearyl methacrylate as co monomers representing 30% and 70% respectively of the liquid volume with ethylene dimethacrylate crosslinker and 2,2-dimethoxy-2-phenylacetophenone as the free radical initiator. The monomers were mixed with a binary porogenic solvent, comprising propan-1-ol, and methanol (0.825 mL each). The monolith was formed by photo polymerization (365 nm) inside a borosilicate glass tube (1.5 mm ID and 3 mm OD x 50 mm length). The monolith was observed to have formed correctly by optical examination and generated reasonable backpressure, approximately 650 psi at a flow rate of 0.2 mL min⁻¹ 50:50 acetonitrile: water. The morphological properties of the monolithic columns were investigated using scanning electron microscopy images, and Brunauer-Emmett-Teller analysis, the results showed that the monolith was formed properly with 19.98 ± 0.01 mm² surface area, 0.0205 ± 0.01 cm³ g⁻¹ pore volume and 6.93 ± 0.01 nm average pore size. The polymer monolith formed was further investigated using proton nuclear magnetic resonance, and Fourier transform infrared spectroscopy. The monolithic columns were investigated using high-performance liquid chromatography to test their ability to separate different samples with a range of properties. The columns displayed both hydrophobic/hydrophilic and hydrophobic/ion exchange interactions with the compounds tested indicating that true mixed mode separations. The mixed mode monolithic columns exhibited significant separation of proteins.

Keywords: LC separation, proteins separation, monolithic column, mixed mode

Procedia PDF Downloads 162

Authors: Walaa Al-Maghraby

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Endophytes are organisms that colonize internal plant tissues without causing apparent harm to their host. Almost all groups of microorganisms have been found in endophytic association with plants may be fungi. They stimulate the production of secondary metabolites with a diverse range of biological activities. Leptadenia pyrotechnica is a more or less leafless, erect shrub with straight stems which is highly distributed in Saudi Arabia. Four endophytes fungi were isolated from Leptadenia pyrotechnica and identified using 18S ribosomal RNA sequences, which revealed four fungi genuses, namely Aspergillus terreus; Aspergillus welwitschiae; Aspergillus fumigatus and Aspergillus flavus. In this present study, four endophytic fungi from Leptadenia pyrotechnica were used for obtaining crude aqueous and ethyl acetate extracts for antimicrobial screening against 6 human pathogens, the antibacterial tests presented satisfactory results, where the pathogenic bacteria were inhibited by the four extracts tested, except for Escherichia coli that was inhibited by all extracts except ethyl acetate extract of Aspergillus terreus. Analysis of variance showed that the extract produced by endophyte Leptadenia pyrotechnica was the most effective against all bacteria, either gram-negative or positive. However, the extract was not efficient against pathogenic fungi. Therefore, this study indicates that endophytes from medicinal plant Leptadenia pyrotechnica could be potential sources of antibacterial substances.

Keywords: antimicrobial activity, Aspergillus sp, endophytes, Leptadenia pyrotechnica

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Authors: Kazui Sasakii, Seira Mormune-Moriya, Hiroaki Tanahashi, Shigeji Kongaya

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Poly (3.4-ethylenedioxythiophene) doped with poly (4-styrene sulfonate) (PEDOT: PSS) attracted a great deal of attention because of its unique characteristics of flexibility, optical properties, heat resistance and colloidal dispersion in water. It is well known that when high boiling solvents such as ethylene glycol or dimethyl sulfoxide are added as a secondary dopant to the micellar structure, PEDOT microcrystallizes and becomes highly conductive. In previous study bis(4-hydroxyphenyl) sulfone (BPS) was used as a secondary dopant for PEDOT:PSS and the enhancement of the conductivity was revealed. However, ductility is one of the serious issues which limited the application of PEDOT:PSS/BPS. So far, the composition with polymer binders has been conducted, however, polymer binders decrease the conductivity of the materials. In this study, PEDOT: PSS composites with polyester (PEs) were prepared by a simple aqueous process using PEs emulsion. The structural studies revealed that PEDOT:PSS and PEs were homogeneously distributed in the composites. It was found that the properties of PEDOT:PSS were remarkably enhanced by the incorporation of PEs. According to the tensile test, the ductility of PEDOT:PSS was remarkably improved. Interestingly, the conductivity of PEDOT:PSS/PEs composites was higher than that of neat PEDOT:PSS. For example, the conductivity increased by 8% at PEs content of 25 wt%. Since PEDOT:PSS were homogeneously dispersed on the surface of PEs particles, it was assumed that the conductive pathway was constructed by PEs particles in the nanocomposites. Therefore, a significant increase in conductivity was achieved.

Keywords: polymer composites, conductivity, PEDOT:PSS, polyester

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Authors: A. Khan, M. Hussain, S. Afgun

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In the present work, the effect of the surface integration on the piezoelectric properties of zinc oxide (ZnO) nanorods has been investigated. ZnO nanorods were grown by using aqueous chemical growth method on two samples of graphene coated pet plastic substrate. First substrate’s surface was integrated with ZnO nanoparticles while the other substrate was used without ZnO nanoparticles. Various important parameters were analyzed, the growth density and morphological analysis were taken into account through surface scanning electron microscopy; it was observed that the growth density of nanorods on the integrated surface was much higher than the nonintegrated substrate. The crystal quality of growth orientation was analyzed by X-ray diffraction technique. Mechanical stability of ZnO nanorods on an integrated substrate was more appropriate than the nonintegrated substrate. The generated amount of piezoelectric potential from the integrated substrate was two times higher than the nonintegrated substrate. This shows that the layer of nanoparticles plays a crucial role in the enhancement of piezoelectric potential. Besides this, it also improves the performance of fabricated devices like its mechanical stability and piezoelectric properties. Additionally, the obtained results were compared with the other two samples used for the growth of ZnO nanorods on silver coated glass substrates for similar measurement. The consistency of the results verified the importance of surface integration effect. This study will help us to fabricate improved performance devices by using surface integrated substrates.

Keywords: ZnO nanorods, surface integration, mechanical properties, harvesting piezoelectricity

Procedia PDF Downloads 132

Authors: Evgeny E. Tereshatov, C. M. Folden

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Ionic liquids and deep eutectic mixtures represent so-called non-conventional solvents. The former, composed of discrete ions, is a salt with a melting temperature below 100°С. The latter, consisting of hydrogen bond donors and acceptors, is a mixture of at least two compounds, resulting in a melting temperature depression in comparison with that of the individual moiety. These systems also can be water-immiscible, which makes them applicable for metal extraction. This work will cover interactions of In, Tl, Ir, and Rh in hydrochloric acid media with eutectic mixtures and Er, Ir, and At in a gas phase with chemically modified α-detectors. The purpose is to study chemical systems based on non-conventional solvents in terms of their interaction with metals. Once promising systems are found, the next step is to modify the surface of α-detectors used in the online element production at cyclotrons to get the detector chemical selectivity. Initially, the metal interactions are studied by means of the liquid-liquid extraction technique. Then appropriate molecules are chemisorbed on the surrogate surface first to understand the coating quality. Finally, a detector is covered with the same molecule, and the metal sorption on such detectors is studied in the online regime. It was found that chemical treatment of the surface can result in 99% coverage with a monolayer formation. This surface is chemically active and can adsorb metals from hydrochloric acid solutions. Similarly, a detector surface was modified and tested during cyclotron-based experiments. Thus, a procedure of detectors functionalization has been developed, and this opens an interesting opportunity of studying chemisorption of elements which do not have stable isotopes.

Keywords: mechanism, radioisotopes, solvent extraction, gas phase sorption

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Authors: Sarra Boughaba

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The α-aminophosphonates have received considerable attention in organic and medicinal chemistry because of their structural resemblance with α-amino acids. They are used as antitumor agents, anti-inflammatory and antibiotics. As a result, a number of procedures have been developed for their synthesis. However, many of these methods suffer from some disadvantages such as long reaction times, environmental pollution caused by utilization of organic solvents, and expensive catalyst. On the other hand, thiazole components, particularly 2-aminothiazole is an important class of heterocyclic compounds. They appear in the structure of natural products and biologically actives compounds, thiamine (vitamin-B), and some antibiotics drugs (penicillin, micrococcin). In the past few years, heteropolyacids have received great attention as environmentally benign catalysts for organic synthetic processes, they possess unique physicochemical properties, such as super-acidity, high thermal and chemical stability, ability to accept and release electrons and high proton mobility, and the possibility of varying their acidity and oxidizing potential. In this study, an efficient and eco-friendly process has been developed for the synthesis of α-aminophosphonates containing aminothiazole moiety via Kabachnik-Field reaction catalyzed by H₆P₂W₁₈O₆₂.14H₂O as reusable catalyst, by condensation of aromatic aldehydes, 2-aminothiazole and triethylphosphite under free conditions. The X-ray crystallographic data of obtained compounds were provided. The main advantages of our protocol include the absence of solvent in the reaction, easy work-up, short reaction time, atom-economy and reusability of catalyst without significant loss of its activity.

Keywords: aminophosphonates, green synthesis, H₆P₂W₁₈O₆₂.14H₂O catalyst, x-ray study

Procedia PDF Downloads 113

Authors: T. Scattolin, E. Cavarzerani, F. Visentin, F. Rizzolio

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Organopalladium compounds have recently attracted attention for their high stability even under physiological conditions and, above all, for their remarkable in vitro cytotoxicity towards cisplatin-resistant cell lines. Among the organopalladium derivatives, those bearing at least one N-heterocyclic carbene ligand (NHC) and the Pd(II)-η³-allyl fragment have exhibited IC₅₀ values in the micro and sub-micromolar range towards several cancer cell lines in vitro and in some cases selectivity towards cancerous vs. non-tumorigenic cells. Herein, a selection of allyl and indenyl palladates were synthesized using a solvent-free method consisting of grinding the corresponding palladium precursors with different saturated and unsaturated azolium salts. All compounds have been fully characterized by NMR, XRD and elemental analyses. The intramolecular H, Cl interaction has been elucidated and quantified using the Voronoi Deformation Density scheme. Most of the complexes showed excellent cytotoxicity towards ovarian cancer cell lines, with I₅₀ values comparable to or even lower than cisplatin. Interestingly, the potent anticancer activity was also confirmed in a high-serous ovarian cancer (HGSOC) patient-derived tumoroid, with a clear superiority of this class of compounds over classical platinum-based agents. Finally, preliminary enzyme inhibition studies of the synthesized palladate complexes against the model TrxR show that the compounds have high activity comparable to or even higher than auranofin and classical Au(I) NHC complexes. Based on such promising data, further in vitro and in vivo experiments and in-depth mechanistic studies are ongoing in our laboratories.

Keywords: anticancer activity, palladium complexes, organoids, indenyl and allyl ligands

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Authors: Min Yu, Olivier T. Picot, Theo Graves Saunders, Ivo Dlouhy, Amit Mahajan, Michael J. Reece

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Graphene was successfully introduced into a polymer-derived silicon oxycarbide (SiOC) matrix by phase transfer of graphene oxide (GO) from an aqueous (GO dispersed in water) to an organic phase (copolymer as SiOC precursor in diethyl ether). With GO concentrations increasing up to 2 vol%, graphene-containing flakes self-assembled into a lamellar structure in the matrix leading to composite with the anisotropic property. Spark plasma sintering (SPS) was applied to densify the composites with four different GO concentrations (0, 0.5, 1 and 2 vol%) up to ~2.3 g/cm3. The fracture toughness of SiOC-2 vol% GO composites was significantly increased by ~91% (from 0.70 to 1.34 MPa·m¹/²), at the expense of a decrease in the flexural strength (from 85MPa to 55MPa), compared to SiOC-0 vol% GO composites. Moreover, the electrical conductivity in the perpendicular direction (σ┴=3×10⁻¹ S/cm) in SiOC-2 vol% GO composite was two orders of magnitude higher than the parallel direction (σ║=4.7×10⁻³ S/cm) owing to the self-assembled lamellar structure of graphene in the SiOC matrix. The composites exhibited increased electrical conductivity (σ┴) from 8.4×10⁻³ to 3×10⁻¹ S/cm, with the increasing GO content from 0.5 to 2 vol%. The SiOC-2 vol% GO composites further showed the better electrochemical performance of oxygen reduction reaction (ORR) than pure graphene, exhibiting a similar onset potential (~0.75V vs. RHE) and more positive half-wave potential (~0.6V vs. RHE).

Keywords: composite, fracture toughness, flexural strength, electrical conductivity, electrochemical performance

Procedia PDF Downloads 166

Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

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The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe₃O₄/Al₂O₃ NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe₃O₄/Al₂O₃ NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL⁻¹, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL^-1 Fe²⁺ was 2.3%.

Keywords: Alumina-Coated magnetite nanoparticles, Magnetic Mixed Hemimicell Solid-Phase Extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample

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Authors: I. M. B. Omiogbemi, D. S. Yawas, I. M. Dagwa, F. G. Okibe

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This work present the effects of some gas metal arc welding parameters on the corrosion behavior of austenitic stainless steel, exposed to 0.5M sodium hydroxide at ambient temperatures (298K) using conventional weight loss determination, together with surface morphology evaluation by scanning electron microscopy and the application of factorial design of experiment to determine welding conditions which enhance the integrity of the welded stainless steel. The welding variables evaluated include speed, voltage and current. Different samples of the welded stainless steels were immersed in the corrosion environment for 8, 16, 24, 32 and 40 days and weight loss determined. From the results, it was found that increase in welding current and speed at constant voltage gave the optimum performance of the austenitic stainless steel in the environment. At a of speed 40cm/min, 110Amp current and voltage of 230 volt the welded stainless steel showed only a 0.0015mg loss in weight after 40 days. Pit-like openings were observed on the surface of the metals indicating corrosion but were minimal at the optimum conditions. It was concluded from the research that relatively high welding speed and current at a constant voltage gives a good welded austenitic stainless steel with better integrity.

Keywords: welding, current, speed, austenitic stainless steel, sodium hydroxide

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Authors: Zubair Khaliq, M. Bilal Qadir, Amir Shahzad, Zulfiqar Ali, Ahsan Nazir, Ali Afzal, Abdul Jabbar

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Carbon fibers are one of the most demanding materials on earth due to their potential application in energy, high strength materials, and conductive materials. The nanostructure of carbon fibers offers enhanced properties of conductivity due to the larger surface area. The next generation carbon nanofibers demand the porous structure as it offers more surface area. Multiple techniques are used to produce carbon fibers. However, electrospinning followed by carbonization of the polymeric materials is easy to carry process on a laboratory scale. Also, it offers multiple diversity of changing parameters to acquire the desired properties of carbon fibers. Polyacrylonitrile (PAN) is the most used material for the production of carbon fibers due to its promising processing parameters. Also, cellulose is one of the highest yield producers of carbon fibers. However, the electrospinning of cellulosic materials is difficult due to its rigid chain structure. The combination of PAN and cellulose can offer a suitable solution for the production of carbon fibers. Both materials are miscible in the mixed solvent of N, N, Dimethylacetamide and lithium chloride. This study focuses on the production of porous carbon fibers as a function of PAN/Cellulose blend ratio, solution properties, and electrospinning parameters. These single polymer and blend with different ratios were electrospun to give fine fibers. The higher amount of cellulose offered more difficulty in electrospinning of nanofibers. After carbonization, the carbon fibers were studied in terms of their blend ratio, surface area, and texture. Cellulose contents offered the porous structure of carbon fibers. Also, the presence of LiCl contributed to the porous structure of carbon fibers.

Keywords: cellulose, polyacrylonitrile, carbon nanofibers, electrospinning, blend

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Authors: M. Kamil, Rahber Husain Khan

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In the present study, the Interaction of anionic polymer, sodium carboxymethylcellulose (NaCMC), with cationic gemini surfactants 2,2[(oxybis(ethane-1,2-diyl))bis(oxy)]bis(N-hexadecyl1-N,N-[di(E2)/tri(E3)]methyl1-2-oxoethanaminium)chloride (16-E2-16 and 16-E3-16) and conventional surfactant (CTAC) in aqueous solutions have been studied by surface tension measurement of binary mixtures (0.0- 0.5 wt% NaCMC and 1 mM gemini surfactant/10 mM CTAC solution). Surface tension measurements were used to determine critical aggregation concentration (CAC) and critical micelle concentration (CMC). The maximum surface excess concentration (Ґmax) at the air-water interface was evaluated by the Gibbs adsorption equation. The minimum area per surfactant molecule was evaluated, which indicates the surfactant-polymer Interaction in a mixed system. The effect of changing surfactant chain length on CAC and CMC values of mixed polymer-surfactant systems was examined. From the results, it was found that the gemini surfactant interacts strongly with NaCMC as compared to its corresponding monomeric counterpart CTAC. In these systems, electrostatic interactions predominate. The lowering of surface tension with an increase in the concentration of surfactants is higher in the case of gemini surfactants almost 10-15 times. The measurements indicated that the Interaction between NaCMC-CTAC resulted in complex formation. The volume of coacervate increases with an increase in CTAC concentration; however, above 0.1 wt. % concentration coacervate vanishes.

Keywords: anionic polymer, gemni surfactants, tensiometer, CMC, interaction

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Authors: Ricky Saputra, Rashmi Walvekar, Mohammad Khalid, Kaveh Shahbaz, Suganti Ramarad

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This particular study of interest aims to study the effect of coupling ultrasonic treatment with eutectic solvents in devulcanization process of waste rubber tyre. Specifically, three different types of Deep Eutectic Solvents (DES) were utilized, namely ChCl:Urea (1:2), ChCl:ZnCl₂ (1:2) and ZnCl₂:urea (2:7) in which their physicochemical properties were analysed and proven to have permissible water content that is less than 3.0 wt%, degradation temperature below 200ᵒC and freezing point below 60ᵒC. The mass ratio of rubber to DES was varied from 1:20-1:40, sonicated for 1 hour at 37 kHz and heated at variable time of 5-30 min at 180ᵒC. Energy dispersive x-rays (EDX) results revealed that the first two DESs give the highest degree of sulphur removal at 74.44 and 76.69% respectively with optimum heating time at 15 minutes whereby if prolonged, reformation of crosslink network would be experienced. Such is supported by the evidence shown by both FTIR and FESEM results where di-sulfide peak reappears at 30 minutes and morphological structures from 15 to 30 minutes change from smooth with high voidage to rigid with low voidage respectively. Furthermore, TGA curve reveals similar phenomena whereby at 15 minutes thermal decomposition temperature is at the lowest due to the decrease of molecular weight as a result of sulphur removal but increases back at 30 minutes. Type of bond change was also analysed whereby it was found that only di-sulphide bond was cleaved and which indicates partial-devulcanization. Overall, the results show that DES has a great potential to be used as devulcanizing solvent.

Keywords: crosslink network, devulcanization, eutectic solvents, reformation, ultrasonic

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Authors: Nasser A. Al-Shabib

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Food allergens are most common non-native form when exposed to the immune system. Most food proteins undergo various treatments (e.g. thermal or proteolytic processing) during food manufacturing. Such treatments have the potential to impact the chemical structure of food allergens so as to convert them to more denatured or unfolded forms. The conformational changes in the proteins may affect the allergenicity of treated-allergens. However, most allergenic proteins possess high resistance against thermal modification or digestive enzymes. In the present study, ovomucoid (a major allergenic protein of egg white) was heated in phosphate-buffered saline (pH 7.4) at different temperatures, aqueous solutions and on different surfaces for various times. The results indicated that different antibody-based methods had different sensitivities in detecting the heated ovomucoid. When using one particular immunoassay‚ the immunoreactivity of ovomucoid increased rapidly after heating in water whereas immunoreactivity declined after heating in alkaline buffer (pH 10). Ovomucoid appeared more immunoreactive when dissolved in PBS (pH 7.4) and heated on a stainless steel surface. To the best of our knowledge‚ this is the first time that antibody-based methods have been applied for the detection of ovomucoid adsorbed onto different surfaces under various conditions. The results obtained suggest that use of antibodies to detect ovomucoid after food processing may be problematic. False assurance will be given with the use of inappropriate‚ non-validated immunoassays such as those available commercially as ‘Swab’ tests. A greater understanding of antibody-protein interaction after processing of a protein is required.

Keywords: ovomucoid, thermal treatment, solutions, surfaces

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Authors: Mona Marzouk, Nesrine Hegazi, Aliaa Ragheb, Mona El Shabrawy, Salwa Kawashty

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The whole plant of Matthiola longipetala (Brassicaceae) was extracted by 70% methanol to give the total aqueous methanol extract (AME), which was defatted by hexane yielded hexane extract (HE) and defatted AME (DAME). HE was analyzed through GC/MS assay and revealed the detection of 28 non-polar compounds. In addition, the chemical investigation of DAME led to the isolation and purification of twelve flavonoids and three chlorogenic acids. Their structures were interpreted through chemical (complete and partial acid hydrolysis) and spectroscopic analysis (MS, UV, 1D and 2D NMR). Among them, nine compounds have been isolated for the first time from M. longipetala. Moreover, LC-ESI-MS analysis of DAME was achieved to detect additional 46 metabolites, including phospholipids, organic acids, phenolic acids and flavonoids. The biological activity of AME, HE and DAME against alloxan inducing oxidative stress and diabetes in male rats was investigated. Diabetes was induced using a single dose of Alloxan (150 mg/kg b.wt.). HE and DAME significantly increased serum GSH content in rats (37.3±0.7 and 35.9±0.6 mmol/l) compared to diabetic rats (21.8±0.3) and vitamin E (36.2±1.1) at P<0.01. Also, HE, DAME and AME revealed a significant acute anti-hyperglycemic effect potentiated after four weeks of treatment with blood glucose levels of 96.2±5.4, 98.7±6.1 and 98.9±8.6 mg/dl, respectively, compared to diabetic rats (263.4±7.8) and metaformin group (81.9±2.4) at P<0.01.

Keywords: Brassicaceae, Flavonoid, LCMS/MS, Matthiola

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Authors: K. Kamburova, N. Boshkova, N. Boshkov, T. Radeva

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Coatings based on polyaniline (PANI) can improve the resistance of steel against corrosion. Two forms of PANI are generally accepted to have effective protection of steel: the conducting emeraldine salt (ES) and the non-conducting emeraldine base (EB). The ability to intercept electrons at the metal surface and to transport them is typically attributed to ES, while the success of EB as an anticorrosive additive in the coating is attributed to its ability to oxidize and reduce in a reversible way. This electrochemical mechanism is probably combined with barrier effect against corrosion species. In this work, we describe the preparation of stable suspensions of colloidal PANI-SiO₂ particles, suitable for obtaining of composite anticorrosive coating on steel. Electrokinetic data as a function of pH are presented, showing that the zeta potentials of the PANI-SiO₂ particles are governed primarily by the charged groups at the silica oxide surface. Electrosteric stabilization of the PANI-SiO₂ particles’ suspension against aggregation is realized at pH > 5.5 (EB form of PANI) by adsorption of positively charged polyelectrolyte molecules onto negatively charged PANI-SiO₂ particles. We anticipate that incorporation of the small particles will provide a more homogeneous distribution in the coating matrix and will decrease the negative effect on barrier properties of the composite coating.

Keywords: particles, stable dispersion, composite coatings, corrosion protection

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Authors: Babar Ali, Mohammad Rashid, Showkat Rasool Mir, Mohammad Ali, Saiba Shams

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Background: The plant Camellia sinensis (Theaceae) is an evergreen shrub indigenous to Assam (India) and parts of China and Japan. Traditional Chinese medicine has recommended green tea for headaches, body aches and pains, digestion, enhancement of immune defense, detoxification, as an energizer and to prolong life. The leaves have more than 700 chemical constituents, among which flavanoids, amino acids, vitamins (C, E, K), caffeine and polysaccharides. Adulteration and substitution may affect the quality of formulation containing tea leaves. Standardization of medicinal preparation is essential for further therapeutic results and for global acceptance. Hence, chromatographic fingerprint profiles were carried out for establishing the standards. Materials and methods: TLC studies for methanolic extracts of the leaves of Camellia sinensis were carried out in a new developed solvent system, Toluene: Ethyl acetate: Formic acid (7:3:1). TLC plates were dried in air, visualized in UV at wavelengths 254 nm and 366 nm and photographed. Results: Results provide valuable clue regarding their polarity and selection of solvents for separation of phytochemicals. Fingerprinting of methanolic extract of Camellia sinensis leaves revealed the presence of various phytochemicals in UV at 254 nm and 366 nm. Conclusion: Fingerprint profile is quite helpful in setting up of standards and thus to keep a check on intentional/unintentional adulteration. TLC offers major advantages over other conventional chromatographic techniques such as unsurpassed flexibility (esp. stationary and mobile phase), choice of detection wavelength, user friendly, rapid and cost effective.

Keywords: Cammelia sinensis Linn., standardization, methanolic extract, thin layer chromatography

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Authors: Babatunde Oluwole Ogunsile, Omosola Monisola Fasoranti

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High costs and toxicological hazards associated with the physicochemical methods of producing nanoparticles have limited their widespread use in clinical and biomedical applications. An ethically sound alternative is the utilization of plant bioresources as a low cost and eco–friendly biological approach. Silver nanoparticles (AgNPs) were synthesized from aqueous leaf extract of Tithonia diversifolia plant. The UV-Vis Spectrophotometer was used to monitor the formation of the AgNPs at different time intervals and different ratios of plant extract to the AgNO₃ solution. The biosynthesized AgNPs were characterized by FTIR, X-ray Diffraction (XRD) and Scanning Electron Microscope (SEM). Antimicrobial activities of the AgNPs were investigated against ten human pathogens using agar well diffusion method. The AgNPs yields were modeled using a second-order factorial design. The result showed that the rate of formation of the AgNPs increased with respect to time while the optimum ratio of plant extract to the AgNO₃ solution was 1:1. The hydroxyl group was strongly involved in the bioreduction of the silver salt as indicated by the FTIR spectra. The synthesized AgNPs were crystalline in nature, with a uniformly distributed network of the web-like structure. The factorial model predicted the nanoparticles yields with minimal errors. The nanoparticles were active against all the tested pathogens and thus have great potentials as antimicrobial agents.

Keywords: antimicrobial activities, green synthesis, silver nanoparticles, Tithonia diversifolia

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Authors: Komal Kumar, Sreedevi Upadhyayula

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In this study, a two-stage process was established for the synthesis of HMF esters using ionic liquid acid catalyst. Ionic liquid catalyst with different strength of the Bronsted acidity was prepared in the laboratory and characterized using 1H NMR, FT-IR, and 13C NMR spectroscopy. Solid acid catalyst from the ionic liquid catalyst was prepared using the immobilization method. The acidity of the synthesized acid catalyst was measured using Hammett function and titration method. Catalytic performance was evaluated for the biomass conversion to 5-hydroxymethylfurfural (5-HMF) and levulinic acid (LA) in methyl isobutyl ketone (MIBK)-water biphasic system. A good yield of 5-HMF and LA was found at the different composition of MIBK: Water. In the case of MIBK: Water ratio 10:1, good yield of 5-HMF was observed at ambient temperature 150˚C. Upgrading of 5-HMF into monoesters from the reaction of 5-HMF and reactants using biomass-derived monoacid were performed. Ionic liquid catalyst with -SO₃H functional group was found to be best efficient in comparative of a solid acid catalyst for the esterification reaction and biomass conversion. A good yield of 5-HMF esters with high 5-HMF conversion was found to be at 105˚C using the best active catalyst. In this process, process A was the hydrothermal conversion of cellulose and monomer into 5-HMF and LA using acid catalyst. And the process B was the esterification followed by using similar acid catalyst. All monoesters of 5-HMF synthesized here can be used in chemical, cross linker for adhesive or coatings and pharmaceutical industry. A theoretical density functional theory (DFT) study for the optimization of the ionic liquid structure was performed using the Gaussian 09 program to find out the minimum energy configuration of ionic liquid catalyst.

Keywords: biomass conversion, 5-HMF, Ionic liquid, HMF ester

Procedia PDF Downloads 251

Authors: Eman M. Morgan, Hayam M. Lotfy, Yasmin M. Fayez, Mohamed Abdelkawy, Engy Shokry

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Two simple, selective, economic, safe, accurate, precise and environmentally friendly methods were developed and validated for the quantitative determination of valaciclovir (VAL) in the presence of its related substances R1 (acyclovir), R2 (guanine) in bulk powder and in the commercial pharmaceutical product containing the drug. Method A is a colorimetric method where VAL selectively reacts with ferric hydroxamate and the developed color was measured at 490 nm over a concentration range of 0.4-2 mg/mL with percentage recovery 100.05 ± 0.58 and correlation coefficient 0.9999. Method B is a reversed phase ultra performance liquid chromatographic technique (UPLC) which is considered superior in technology to the high-performance liquid chromatography with respect to speed, resolution, solvent consumption, time, and cost of analysis. Efficient separation was achieved on Agilent Zorbax CN column using ammonium acetate (0.1%) and acetonitrile as a mobile phase in a linear gradient program. Elution time for the separation was less than 5 min and ultraviolet detection was carried out at 256 nm over a concentration range of 2-50 μg/mL with mean percentage recovery 100.11±0.55 and correlation coefficient 0.9999. The proposed methods were fully validated as per International Conference on Harmonization specifications and effectively applied for the analysis of valaciclovir in pure form and tablets dosage form. Statistical comparison of the results obtained by the proposed and official or reported methods revealed no significant difference in the performance of these methods regarding the accuracy and precision respectively.

Keywords: hydroxamic acid, related substances, UPLC, valaciclovir

Procedia PDF Downloads 246

Authors: H. Tayefih, F. farajzade ahari, F. Zarghami, V. Zeighamian, N. Zarghami, Y. Pilehvar-soltanahmadi

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Breast cancer is the most frequently occurring cancer among women throughout the world. Natural compounds such as curcumin hold promise to treat a variety of cancers including breast cancer. However, curcumin's therapeutic application is limited, due to its rapid degradation and poor aqueous solubility. On the other hand, previous studies have stated that drug delivery using nanoparticles might improve the therapeutic response to anticancer drugs. Poly (N-isopropylacrylamide-co-methacrylic acid) (PNIPAAm–MAA) is one of the hydrogel copolymers utilized in the drug delivery system for cancer therapy. The aim of this study was to examine the cytotoxic potential of curcumin encapsulated within the NIPAAm-MAA nanoparticle, on the MCF-7 breast cancer cell line. In this work, polymeric nanoparticles were synthesized through the free radical mechanism, and curcumin was encapsulated into NIPAAm-MAA nanoparticles. Then, the cytotoxic effect of curcumin-loaded NIPAAm-MAA on the MCF-7 breast cancer cell line was measured by MTT assays. The evaluation of the results showed that curcumin-loaded NIPAAm-MAA has more cytotoxic effect on the MCF-7 cell line and efficiently inhibited the growth of the breast cancer cell population, compared with free curcumin. In conclusion, this study indicates that curcumin-loaded NIPAAm-MAA suppresses the growth of the MCF-7 cell line. Overall, it is concluded that encapsulating curcumin into the NIPAAm-MAA copolymer could open up new avenues for breast cancer treatment.

Keywords: PNIPAAm-MAA, breast cancer, curcumin, drug delivery

Procedia PDF Downloads 374

Authors: Patcharakamon Nooeaid, Piyachat Chuysrinuan

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Electrospun natural polymers-based nanofibers are one of the most interesting materials used in tissue engineering and drug delivery applications. Bead-on-string nanofibers have gained considerable interest for sustained drug release. Vancomycin was used as the model drug and sodium alginate (SA)/soy protein isolated (SPI) as the polymer blend to fabricate the bead-on-string nanofibers by aqueous-based electrospinning. The bead-on-string SA/SPI nanofibers were successfully fabricated by the addition of poly(ethylene oxide) (PEO) as a co-blending polymer. SA-PEO with mass ratio of 70/30 showed the best spinnability with continuous nanofibers without the occurrence of beads. Bead structure formed with the addition of SPI and bead number increased with increasing SPI content. The electrospinning of 80/20 SA-PEO/SPI was obtained as a great promising bead-on-string nanofibers for drug loading, while the solution of 50/50 was not able to obtain continuous fibers. In vitro release tests showed that a more sustainable release profile up to 14 days with less initial burst release on day 1 could be obtained from the bead-on-string fibers than from smooth fibers with uniform diameter. In addition, vancomycin-loaded beaded fibers inhibited the growth of Staphylococcus aureus (S. aureus) bacteria. Therefore, the SA-PEO/SPI nanofibers showed the potential to be used as biomaterials for tissue engineering and drug delivery.

Keywords: bead-on-string fibers, electrospinning, drug delivery, tissue engineering

Procedia PDF Downloads 334

Authors: Dana A. Thal, Heike Kahlert, Fritz Scholz

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Thiol molecules are known to easily form self-assembled monolayers (SAM) on Au surfaces. Depending on the thiol’s structure, surface modifications via SAM can be used for electrode sensor development. In the presented work, 1-decanethiol coated polycrystalline Au electrodes were applied to indirectly assess the radical scavenging potential of plant compounds and extracts. Different plant compounds with reported antioxidant properties as well as an extract from the plant Gynostemma pentaphyllum were tested for their effectiveness to prevent SAM degradation on the sensor electrodes via photolytically generated radicals in aqueous media. The SAM degradation was monitored over time by differential pulse voltammetry (DPV) measurements. The results were compared to established antioxidant assays. The obtained data showed an exposure time and concentration dependent degradation process of the SAM at the electrode’s surfaces. The tested substances differed in their capacity to prevent SAM degradation. Calculated radical scavenging activities of the tested plant compounds were different for different assays. The presented method poses a simple system for radical scavenging evaluation and, considering the importance of the test system in antioxidant activity evaluation, might be taken as a bridging tool between in-vivo and in-vitro antioxidant assay in order to obtain more biologically relevant results in antioxidant research.

Keywords: alkanethiol SAM, plant antioxidant, polycrystalline Au, radical scavenger

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Authors: Indu Bhushan Sharma, Rashmi Saraswat

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The thermotolerant, solvent stable and alkalophilic lipase producing bacterial strain was isolated from the water sample of the foothills of Trikuta Mountain in Kakryal (Reasi district) in Jammu and Kashmir, India. The lipase-producing microorganisms were screened using tributyrin agar plates. The selected microbe was optimized for maximum lipase production by subjecting to various carbon and nitrogen sources, incubation period and inoculum size. The selected strain was identified as Bacillus subtilis strain kakrayal_1 (BSK_1) using 16S rRNA sequence analysis. Effect of pH, temperature, metal ions, detergents and organic solvents were studied on lipase activity. Lipase was found to be stable over a pH range of 6.0 to 9.0 and exhibited maximum activity at pH 8. Lipolytic activity was highest at 37°C and the enzyme activity remained at 60°C for 24hrs, hence, established as thermo-tolerant. Production of lipase was significantly induced by vegetable oil and the best nitrogen source was found to be peptone. The isolated Bacillus lipase was stimulated by pre-treatment with Mn2+, Ca2+, K+, Zn2+, and Fe2+. Lipase was stable in detergents such as triton X 100, tween 20 and Tween 80. The 100% ethyl acetate enhanced lipase activity whereas, lipase activity were found to be stable in Hexane. The optimization resulted in 4 fold increase in lipase production. Bacillus lipases are ‘generally recognized as safe’ (GRAS) and are industrially interesting. The inducible alkaline, thermo-tolerant lipase exhibited the ability to be stable in detergents and organic solvents. This could be further researched as a potential biocatalyst for industrial applications such as biotransformation, detergent formulation, bioremediation and organic synthesis.

Keywords: bacillus, lipase, thermotolerant, alkalophilic

Procedia PDF Downloads 255

Authors: Yamina Boukari, Nashiru Billa, Andrew Morris, Stephen Doughty, Kevin Shakesheff

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Poly (lactic-co-glycolic) acid (PLGA) is a synthetic polymer that can be used in bone tissue engineering with the aim of creating a scaffold in order to support the growth of cells. The formation of microspheres from this polymer is an attractive strategy that would allow for the development of an injectable system, hence avoiding invasive surgical procedures. The aim of this study was to develop a microsphere delivery system for use as an injectable scaffold in bone tissue engineering and evaluate various formulation parameters on its properties. Porous and lysozyme-containing PLGA microspheres were prepared using the double emulsion solvent evaporation method from various molecular weights (MW). Scaffolds were formed by sintering to contain 1 -3mg of lysozyme per gram of scaffold. The mechanical and physical properties of the scaffolds were assessed along with the release of lysozyme, which was used as a model protein. The MW of PLGA was found to have an influence on microsphere size during fabrication, with increased MW leading to an increased microsphere diameter. An inversely proportional relationship was displayed between PLGA MW and mechanical strength of formed scaffolds across loadings for low, intermediate and high MW respectively. Lysozyme release from both microspheres and formed scaffolds showed an initial burst release phase, with both microspheres and scaffolds fabricated using high MW PLGA showing the lowest protein release. Following the initial burst phase, the profiles for each MW followed a similar slow release over 30 days. Overall, the results of this study demonstrate that lysozyme can be successfully incorporated into porous PLGA scaffolds and released over 30 days in vitro, and that varying the MW of the PLGA can be used as a method of altering the physical properties of the resulting scaffolds.

Keywords: bone, microspheres, PLGA, tissue engineering

Procedia PDF Downloads 425