Search results for: methyl acetate

Authors: Ikechukwu Ejim

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This research project addresses the optimization of biodiesel production from gossypium herbaceum (cottonseed) and moringa oleifera seeds. Soxhlet extractor method using n-hexane for gossypium herbaceum (cottonseed) and ethanol for moringa oleifera were used for solvent extraction. 1250 ml of oil was realized from both gossypium herbaceum (cottonseed) and moringa oleifera seeds before characterization. In transesterification process, a 4-factor-3-level experiment was conducted using an optimal design of Response Surface Methodology. The effects of methanol/oil molar ratio, catalyst concentration (%), temperature (°C) and time (mins), on the yield of methyl ester for both cottonseed and moringa oleifera oils were determined. The design consisted of 25 experimental runs (5 lack of fit points, five replicate points, 0 additional center points and I optimality) and provided sufficient information to fit a second-degree polynomial model. The experimental results suggested that optimum conditions were as follows; cottonseed yield (96.231%), catalyst concentration (0.972%), temperature (55oC), time (60mins) and methanol/oil molar ratios (8/1) respectively while moringa oleifera optimum values were yield (80.811%), catalyst concentration (1.0%), temperature (54.7oC), time (30mins ) and methanol/oil molar ratios (8/1) respectively. This optimized conditions were validated with the actual biodiesel yield in experimental trials and literature.

Keywords: optimization, Gossypium herbaceum, Moringa oleifera, biodiesel

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Authors: Stephen Eyije Abechi, Casimir Emmanuel Gimba, Zaharaddeen Nasiru Garba, Sani Shamsudeen, David Ebuka Authur

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The mechanisms of corrosion inhibition of mild steel in acid medium using Acalypha chamaedrifolia leaves extract as potential green inhibitor were investigated. Gravimetric (weight loss) technique was used for the corrosion studies. Mild steel coupons of 2cm × 1cm × 0.27 cm dimensions were exposed for varying durations of between 24 to 120 hours, in 1M HCl medium containing a varying concentrations of the leaves extract (0.25g/L, - 1.25g/L). The results show that corrosion rates dropped from a value of 0.49 mgcm-2hr-1 for the uninhibited medium to a value of 0.15 mgcm-2hr-1 for the inhibited medium of 1M HCl in 0.25 g/l of the extract. Values of corrosion inhibition efficiencies of 70.38-85.11% were observed as the concentration of the inhibitor were increased from 0.25g/L, - 1.25g/L. Corrosion Inhibition was found to increase with increase in immersion time and temperature. The magnitude of the Ea indicates that the interaction between the metal surface and the inhibitor was chemisorptions. The Adsorption process fit into the Langmuir isotherm model with a correlation coefficient of 0.97. Evidence from molecular dynamics model shows that Methyl stearate (Line 5) and (3Z, 13Z)-2-methyloctadeca-3,13-dien-1-ol (line 11) were found to have the highest binding energy of -197.69 ± 3.12 and-194.56 ± 10.04 in kcal/mol respectively. The binding energy of these compounds indicates that they would be a very good corrosion inhibitor for mild steel and other Fe related materials.

Keywords: binding energy, corrosion, inhibitor, Langmuir isotherm, mild steel.

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Authors: Wilmer Esteban Vallejo Narváez, Serguei Fomine

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The theoretical investigation of Si-doped graphene nanoflakes (NFs) was conducted to understand their catalytic impact on CO₂ reduction using molecular hydrogen at the Density Functional Theory (DFT) level. The introduction of silicon by substituting carbon induces defects in the NF structure, resulting in a polyradical ground state. This silicon defect significantly boosts reactivity towards substrates, making Si-doped graphene NFs more catalytically active in CO₂ reduction to formic acid compared to silicene. Notably, Si-doped graphene demonstrates a preference for formic acid over carbon monoxide, mirroring the behavior of silicene. Furthermore, investigations into formic acid-to-formaldehyde and formaldehyde-to-methanol conversions reveal instances where Si-doped graphene outperforms silicene in terms of efficacy. In the final reduction step, the methanol-to-methane reaction unfolds in four stages, with the rate-determining step involving hydrogen transfer from silicon to methyl. Notably, the activation energy for this step is lower in Si-doped graphene compared to silicene. Consequently, Si-doped graphene NFs emerge as superior catalysts with lower activation energies overall. Remarkably, throughout these catalytic processes, Si-doped graphene maintains environmental stability, further highlighting its enhanced catalytic activity without compromising graphene's inherent stability.

Keywords: silicon-doped graphene, CO₂ reduction, DFT, catalysis

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Authors: Umran Kurtan, Hamide Aydin, Sevim Unugur Celik, Ayhan Bozkurt

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In the present work, novel hBN/polyacrylonitrile composite nanofibers were produced via electrospinning approach and loaded with the electrolyte for rechargeable lithium-ion battery applications. The electrospun nanofibers comprising various hBN contents were characterized by using Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The influence of hBN/PAN ratios onto the properties of the porous composite system, such as fiber diameter, porosity, and the liquid electrolyte uptake capability were systematically studied. Ionic conductivities and electrochemical characterizations were evaluated after loading electrospun hBN/PAN composite nanofiber with liquid electrolyte, i.e., 1 M lithium hexafluorophosphate (LiPF6) in ethylene carbonate (EC)/ethyl methyl carbonate (EMC) (1:1 vol). The electrolyte loaded nanofiber has a highest ionic conductivity of 10−3 S cm⁻¹ at room temperature. According to cyclic voltammetry (CV) results it exhibited a high electrochemical stability window up to 4.7 V versus Li+/Li. Li//10 wt% hBN/PAN//LiCO₂ cell was produced which delivered high discharge capacity of 144 mAhg⁻¹ and capacity retention of 92.4%. Considering high safety and low cost properties of the resulting hBN/PAN fiber electrolytes, these materials can be suggested as potential separator materials for lithium-ion batteries.

Keywords: hexagonal boron nitride, polyacrylonitrile, electrospinning, lithium ion battery

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Authors: Mohamed H. El-Newehy, Badr M. Thamer, Nasser A. M. Barakat, Mohammad A.Abdelkareem, Salem S. Al-Deyab, Hak Y. Kim

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In this study, the influence of nitrogen doping on the electrocatalytic activity of carbon nanofibers with nickel nanoparticles toward methanol oxidation is introduced. The modified carbon nanofibers have been synthesized from calcination of electrospun nanofiber mats composed of nickel acetate tetrahydrate, poly(vinyl alcohol) and urea in argon atmosphere at 750oC. The utilized physicochemical characterizations indicated that the proposed strategy leads to form carbon nanofibers having nickel nanoparticles and doped by nitrogen. Moreover, due to the high-applied voltage during the electrospinning process, the utilized urea chemically bonds with the polymer matrix, which leads to form nitrogen-doped CNFs after the calcination process. Investigation of the electrocatalytic activity indicated that nitrogen doping NiCNFs strongly enhances the oxidation process of methanol as the current density increases from 52.5 to 198.5 mA/cm2 when the urea content in the original electrospun solution was 4 wt% urea. Moreover, the nanofibrous morphology exhibits distinct impact on the electrocatalytic activity. Also, nitrogen-doping enhanced the stability of the introduced Ni-based electrocatalyst. Overall, the present study introduces effective and simple strategy to modify the electrocatalytic activity of the nickel-based materials.

Keywords: electrospinning, methanol electrooxidation, fuel cells, nitrogen-doping, nickel

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Authors: Rafia Asghar, Abdul Hafeez

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The current research was related with natural dyes’ extraction from the powder of Neem (Azadirachta indica) bark and studied characterization of this dye under microwave radiation’s influence. Both cotton fabric and dyeing powder were exposed to microwave rays for different time intervals (2minutes, 4 minutes, 6 minutes, 8 minutes and 10 minutes) using conventional oven. Aqueous, 60% Methanol and Ethyl Acetate solubilized extracts obtained from Neem (Azadirachta indica) bark were also exposed to different time intervals (2minutes, 4 minutes, 6 minutes, 8 minutes and 10 minutes) of microwave rays exposure. Pre, meta and post mordanting with Alum (2%, 4%, 6%, 8%, and 10%) was done to improve color strength of the extracted dye. Exposure of Neem (Azadirachta indica) bark extract and cotton to microwave rays enhanced the extraction process and dyeing process by reducing extraction time, dyeing time and dyeing temperature. Microwave rays treatment had a very strong influence on color fastness and color strength properties of cotton that was dyes using Neem (Azadirachta indica) bark for 30 minutes and dyeing cotton with that Neem bark extract for 75 minutes at 30°C. Among pre, meta and post mordanting, results indicated that 5% concentration of Alum in meta mordanting exhibited maximum color strength.

Keywords: dyes, natural dyeing, ecofriendly dyes, microwave treatment

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Authors: Tengku Muhammad Rafi Nazmi Bin Tengku Razali, Habsah Alwi

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This article based on effect of temperature towards extraction of Aquilaria Subintegra. Aquilaria Subintegra which its main habitat is in Asia-tropical and particularly often found in its native which is Thailand. There is claim which is Aquilaria Subintegra contains antipyretic properties that helps fight fever. Research nowadays also shown that paracetamol consumed bring bad effect towards consumers. This sample will first dry using Vacuum Far Infrared which provides better drying than conventional oven. Soxhlet extractor used to extract oil from sample. Gas Chromatography Mass Spectrometer used to analyze sample to determine its compound. Objective from this research was to determine the active ingredients that exist in the Aquilaria Subintegra leaves and to determine whether compound of Acetaminophen exist or not inside the leaves. Moisture content from 400C was 80%, 500C was 620% and 600C was 36%. The greater temperature resulting lower moisture content inside sample leaves. 7 components were identified in sample T=400C while only 5 components were identified in sample at T=50C and T=60C. Four components were commonly identified in three sample which is 1n-Hexadecanoic acid, 9,12,15-Octadecatrienoic acid, methyl ester (z,z,z), Vitamin E and Squalene. Further studies are needed with new series of temperature to refine the best results.

Keywords: aquilaria subintegra, vacuum far infrared, SOXHLET extractor, gas chromatography mass spectrometer, paracetamol

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Authors: Rowan Moore, Kai Scheffler, Eugen Damoc, Jennifer Sutton, Aaron Bailey, Stephane Houel, Simon Cubbon, Jonathan Josephs

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Purpose: MS analysis of monoclonal antibodies (mAbs) at the protein and peptide levels is critical during development and production of biopharmaceuticals. The compositions of current generation therapeutic proteins are often complex due to various modifications which may affect efficacy. Intact proteins analyzed by MS are detected in higher charge states that also provide more complexity in mass spectra. Protein analysis in native or native-like conditions with zero or minimal organic solvent and neutral or weakly acidic pH decreases charge state value resulting in mAb detection at higher m/z ranges with more spatial resolution. Methods: Three commercially available mAbs were used for all experiments. Intact proteins were desalted online using size exclusion chromatography (SEC) or reversed phase chromatography coupled on-line with a mass spectrometer. For streamlined use of the LC- MS platform we used a single SEC column and alternately selected specific mobile phases to perform separations in either denaturing or native-like conditions: buffer A (20 % ACN, 0.1 % FA) with Buffer B (100 mM ammonium acetate). For peptide analysis mAbs were proteolytically digested with and without prior reduction and alkylation. The mass spectrometer used for all experiments was a commercially available Thermo Scientific™ hybrid Quadrupole-Orbitrap™ mass spectrometer, equipped with the new BioPharma option which includes a new High Mass Range (HMR) mode that allows for improved high mass transmission and mass detection up to 8000 m/z. Results: We have analyzed the profiles of three mAbs under reducing and native conditions by direct infusion with offline desalting and with on-line desalting via size exclusion and reversed phase type columns. The presence of high salt under denaturing conditions was found to influence the observed charge state envelope and impact mass accuracy after spectral deconvolution. The significantly lower charge states observed under native conditions improves the spatial resolution of protein signals and has significant benefits for the analysis of antibody mixtures, e.g. lysine variants, degradants or sequence variants. This type of analysis requires the detection of masses beyond the standard mass range ranging up to 6000 m/z requiring the extended capabilities available in the new HMR mode. We have compared each antibody sample that was analyzed individually with mixtures in various relative concentrations. For this type of analysis, we observed that apparent native structures persist and ESI is benefited by the addition of low amounts of acetonitrile and formic acid in combination with the ammonium acetate-buffered mobile phase. For analyses on the peptide level we analyzed reduced/alkylated, and non-reduced proteolytic digests of the individual antibodies separated via reversed phase chromatography aiming to retrieve as much information as possible regarding sequence coverage, disulfide bridges, post-translational modifications such as various glycans, sequence variants, and their relative quantification. All data acquired were submitted to a single software package for analysis aiming to obtain a complete picture of the molecules analyzed. Here we demonstrate the capabilities of the mass spectrometer to fully characterize homogeneous and heterogeneous therapeutic proteins on one single platform. Conclusion: Full characterization of heterogeneous intact protein mixtures by improved mass separation on a quadrupole-Orbitrap™ mass spectrometer with extended capabilities has been demonstrated.

Keywords: disulfide bond analysis, intact analysis, native analysis, mass spectrometry, monoclonal antibodies, peptide mapping, post-translational modifications, sequence variants, size exclusion chromatography, therapeutic protein analysis, UHPLC

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Authors: Shivankar Agrawal, Indira Sarangthem

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Staphylococcus aureus and Methicillin-resistant Staphylococcus aureus (MRSA) remains one of the major causes of healthcare-associated and community-onset infections worldwide. Hence the search for non-toxic natural compounds having antibacterial activity has intensified for future drug development. The exploration of less studied niches of Earth can highly increase the possibility to discover novel bioactive compounds. Therefore, in this study, the cultivable fraction of fungi from the sediments of natural hot springs has been studied to mine potential fungal candidates with antibacterial activity against the human pathogen Staphylococcus aureus and Methicillin-resistant Staphylococcus aureus. We isolated diverse strains of thermophilic fungi from a collection of samples from sediment. Following a standard method, we isolated a promising thermophilic fungus strain IBSD19, identified as Acrophialophora levis, possessing the potential to produce an anti-Staphylococcus aureus agent. The growth conditions were optimized and scaled to fermentation, and its produced extract was subjected to chemical extraction. The ethyl acetate fraction was found to display significant activity against Staphylococcus aureus and MRSA with a minimum inhibitory concentration (MIC) of 0.5 mg/ml and 4 mg/ml, respectively. The cell membrane integrity assay and SEM suggested that the fungal metabolites cause bacteria clustering and further lysis of the cell.

Keywords: antibacterial activity, antioxidant, fungi, Staphylococcus aureus, MRSA, thermophiles

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Authors: Huafeng Wei

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Dementia in Alzheimer’s Disease (AD) is the number one cause of dementia internationally, without effective treatments. Increasing evidence suggest that disruption of intracellular calcium homeostasis, primarily pathological elevation of cytosol and mitochondria but reduction of endoplasmic reticulum (ER) calcium concentrations, play critical upstream roles on multiple pathologies and associated neurodegeneration, impaired neurogenesis, synapse, and cognitive dysfunction in various AD preclinical studies. The last federal drug agency (FDA) approved drug for AD dementia treatment, memantine, exert its therapeutic effects by ameliorating N-methyl-D-aspartate (NMDA) glutamate receptor overactivation and subsequent calcium dysregulation. More research works are needed to develop other drugs targeting calcium dysregulation at multiple pharmacological acting sites for future effective AD dementia treatment. Particularly, calcium channel blockers for the treatment of hypertension and dantrolene for the treatment of muscle spasm and malignant hyperthermia can be repurposed for this purpose. In our own research work, intranasal administration of dantrolene significantly increased its brain concentrations and durations, rendering it a more effective therapeutic drug with less side effects for chronic AD dementia treatment. This review summarizesthe progress of various studies repurposing drugs targeting calcium dysregulation for future effective AD dementia treatment as potentially disease-modifying drugs.

Keywords: alzheimer, calcium, cognitive dysfunction, dementia, neurodegeneration, neurogenesis

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Authors: S. A. A. Nabeela Nasreen, S. Sundarrajan, S. A. Syed Nizar, Seeram Ramakrishna

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Metal-organic frameworks (MOFs) have attracted considerable interest due to its diverse pore size tunability, fascinating topologies and extensive uses in fields such as catalysis, membrane separation, chemical sensing, etc. Zeolitic imidazolate frameworks (ZIFs) are a class of MOF with porous crystals containing extended three-dimensional structures of tetrahedral metal ions (e.g., Zn) bridged by Imidazolate (Im). Selected ZIFs are used to separate solvent/solvent mixtures. A layer by layer formation of the nanocomposite of Zinc oxide (ZnO) and ZIF on a ceramic support using a solvothermal method was engaged and tested for target solvent/solvent separation. Metal oxide layer was characterized by XRD, SEM, and TEM to confirm the smooth and continuous coating for the separation process. The chemical composition of ZIF films was studied by using X-Ray absorption near-edge structure (XANES) spectroscopy. The obtained ceramic tube with metal oxide and ZIF layer coating were tested for its packing density, thickness, distribution of seed layers and variation of permeation rate of solvent mixture (isopropyl alcohol (IPA)/methyl isobutyl ketone (MIBK). Pervaporation technique was used for the separation to achieve a high permeation rate with separation ratio of > 99.5% of the solvent mixture.

Keywords: metal oxide, membrane, pervaporation, solvothermal, ZIF

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Authors: Tiah Rachmatiah, Subaryanti

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Plants of Lauraceae family are known to contain many chemical compounds which have potential bioactivity such as alkaloids, flavonoids, lactones, terpenes, etc. Actinodaphne macrophylla and Nectandra angustifolia are two species from Lauraceae. A previous study on the crude alkaloidal extract from the bark of Act. macrophylla and n-hexane extract from the bark of N. angustifolia showed antiplasmodial activity against Plasmodium falciparum. The study was continued to find antiplasmodial active compounds from the two extracts. The materials were obtained from Bogor Botanical Garden, West Java, Indonesia. Crude alkaloidal extract of Act. macrophylla was prepared by maceration in dichloromethane after moistened with NH4OH 25% and n-hexane extract of N. angustifolia was prepared by maceration in n-hexane. A major compound was isolated by column chromatography using silica gel and a mixture of CH2Cl2 and methanol as a gradient solvent system for the alkaloidal extract and mixture of n-hexane and ethyl acetate for n-hexane extract. Fine white needle crystals were obtained from the alkaloidal extract and rod crystals from n-hexane extract. Molecular structure of the compounds was determined by analysis of spectra of NMR, IR, MS and compared by references. In vitro bioactivity test of the compound was performed against Plasmodium falciparum. The results showed that the bark of Act. macrophylla contained an aporphine alkaloid, actinodaphnine, that had activity against P. falciparum with IC50 value of 0.095 µg/mL and the bark of N. angustifolia contained a lignan compound, sesamine, with IC50 of 0.122 µg/mL.

Keywords: actinodaphne macrophylla, alkaloid, antiplasmodial, lauraceae, lignan, nectandra angustifolia

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Authors: A. M. T. Jacinto, M.O. Osi

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Tamarind has various medicinal properties among which is its antibacterial property. Its bark contains saponins, alkaloids, sesquiterpenes and tannins. It is rich in phlobapenes which is responsible for antibacterial property. The objective of the study was to determine which bark will produce the highest antibacterial property, develop it into a topical cream and evaluate its quality and characteristics. Powdered barks of Tamarind were extracted by soxhlet method using 70% acetone. Stem bark produced a higher yield than trunk bark (5.85 g vs. 4.73 g). It was found that the trunk bark was more sensitive than stem bark to microorganisms namely Staphylococcus aureus, Corynebacterium minutissimum, and Streptococcus spp. Sensitivity of trunk bark can be attributed to a more developed phytoconstituents. Dermal sensitization test on both sexes of rabbits using the following concentrations: 100%, 40% and 20% of extract showed that Tamarind has no irritating property and therefore safe for formulation into an antibacterial cream. Excipients used for formulation such as methyl paraben, propyl paraben, stearyl alcohol and white petrolatum were compatible with the Tamarind acetone extract through Differential Scanning Calorimetry except sodium lauryl sulfate that exhibited crystallization when subjected at 200˚C. The method of manufacture used in cream is fusion, therefore strict compliance of processing temperature should be observed to prevent polymorphism. Quality control tests of formulated cream based on USP 30 and Philippine Pharmacopeia were satisfactory.

Keywords: antibacterial, differential scanning calorimetry, tannins, dermal sensitization

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Authors: Assia Belfar, Mohamed Hadjadj, Messaouda Dakmouche, Zineb Ghiaba

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Introduction: This study aims to phytochemical screening; Extracting the active compounds and estimate the effectiveness of antioxidant in Medicinal plants desert Limoniastrum guyonianum (Zeïta) from South Algeria. Methods: Total phenolic content and total flavonoid content using Folin-Ciocalteu and aluminum chloride colorimetric methods, respectively. The total antioxidant capacity was estimated by the following methods: DPPH (1.1-diphenyl-2-picrylhydrazyl radical) and reducing power assay. Results: Phytochemical screening of the plant part reveals the presence of phenols, saponins, flavonoids and tannins. While alkaloids and Terpenoids were absent. The acetonic extract of L. guyonianum was extracted successively with ethyl acetate and butanol. Extraction of yield varied widely in the L. guyonianum ranging from (0.9425 %to 11.131%). The total phenolic content ranged from 53.33 mg GAE/g DW to 672.79 mg GAE/g DW. The total flavonoid concentrations varied from 5.45 to 21.71 mg/100g. IC50 values ranged from 0.02 ± 0.0004 to 0.13 ± 0.002 mg/ml. All extracts showed very good activity of ferric reducing power, the higher power was in butanol fraction (23.91 mM) more effective than BHA, BHT and VC. Conclusions: Demonstrated this study that the acetonic extract of L. guyonianum contain a considerable quantity of phenolic compounds and possess a good antioxidant activity. Can be used as an easily accessible source of Natural Antioxidants and as a possible food supplement and in the pharmaceutical industry.

Keywords: limoniastrum guyonianum, phenolics compounds, flavonoid compound, antioxidant activity

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Authors: Diana Serbezeanu, Ionela-Daniela Carja, Tachita Vlad-Bubulac, Sergiu Sova

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New phosphorus-containing monomers having methoxy end functional groups were prepared from methyl 4-hydroxybenzoate and two different dichlorides with phosphorus, namely phenyl phosphonic dichloride and phenyl dichlorophosphate. The structures of the monomers were confirmed by FTIR and NMR spectroscopy. The assignments for the 1H, 13C and 31P chemical shifts are based on 1D and 2D NMR homo- and heteronuclear correlations (H,H-COSY (Correlation Spectroscopy), H,C-HMQC (Heteronuclear Multiple Quantum Correlation and H,C-HMBC (Heteronuclear Multiple Bond Correlation)) and 31P-13C couplings. The monomers exhibited good solubility in common organic solvents. Dimethyl sulfoxide was to be a good solvent to grow crystals of considerable size which were investigated by X-ray analysis. One of these two new monomers presented thermotropic liquid crystalline behaviour, as revealed by differential scanning calorimetry (DSC), polarized light microscopy (PLM) and X-ray diffraction (XRD). The transition temperature from crystal to liquid crystalline state (K→LC) was 143°C and from the LC to isotropic state (LC→I) was 167°C. Upon heating, bis(4-(methoxycarbonyl)phenyl formed fine textures, difficult to be ascribed to smectic or nematic phases. Upon cooling from the isotropic state, bis(4-(methoxycarbonyl)phenyl exhibited a mosaic-type texture. X-ray diffraction measurements at small angles (SAXS) of bis(4-(methoxycarbonyl)phenyl showed two peaks at 1.8 Å and 3.5 Å, respectively suggesting organization at supramolecular level.

Keywords: phosphorus-containing monomers, polarized light microscopy, structure investigation, thermotropic liquid crystalline properties

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Authors: N. Boussoualim, H. Trabsa, I. Krache, S. Aouachria, S. Boumerfeg, L. Arrar, A. Baghiani

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The aim of this study consisted in evaluating the antioxidant in vivo properties, anti-hemolytic and XOR inhibitory effect of Globularia alypum L. (GA) extracts. GA was submitted to extraction and fractionation to give crude (CrE), chloroformique (ChE), ethyle acetate (EAE) and aqueos (AqE) extracts. Total polyphenols contents of GA extracts were determined; EAE is the most rich in polyphenols (157,74±5,27 mg GAE/mg of extract). GA Extracts inhibited XO in a concentration-dependent manner, the EAE showed the highest inhibitory properties on the XOR activity (IC50=0,083±0,001 mg/ml), followed by CrE and ChE. The antioxidant activities of the CrE, EAE, and AqE were tested by an in vivo assay in mice, the plasma ability to inhibit DPPH radical was measured, The CrE was found to exhibit the greatest scavenger activity with 48.41±2.763%, followed by AqE and EAE (40.54±7.51% and 41.79±1.654%, respectively). Total antioxidant capacity of red blood cells was measured, from the kinetics of hemolysis obtained. The calculated HT50 reveal an extension of time for half hemolysis in all treated groups compared with the control group. CrE increase significantly HT50 (112,8±2,427). The hemolysis is lagged, indicating that endogenous antioxidants in the erythrocytes can trap radicals to protect them against free-radical-induced hemolysis. Antimicrobial activities of the extracts were determined by the disc diffusion method. Test microorganisms were; 4 Gram positive, 7 gram negative bacteria, most active extracts were EAE and CrE. We deduce a great relationship between the effect on the extracts antibacterial effect and their contents in flavonoid.

Keywords: Globularia alypum, Xanthine oxidoreductase, in vivo-antioxidant activity, hemolysis, polyphenol

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Authors: Hossein Navid, Maryam Adeli Khadem, Shahin Oustan, Mahmoud Zareie

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Among the nutrients needed by the plants, three elements containing nitrate, phosphorus and potassium are more important. The objective of this research was measuring these nutrient amounts in soil using Fourier transform infrared spectroscopy in range of 400- 4000 cm-1. Soil samples for different soil types (sandy, clay and loam) were collected from different areas of East Azerbaijan. Three types of fertilizers in conventional farming (urea, triple superphosphate, potassium sulphate) were used for soil treatment. Each specimen was divided into two categories: The first group was used in the laboratory (direct measurement) to extract nitrate, phosphorus and potassium uptake by colorimetric method of Olsen and ammonium acetate. The second group was used to measure drug absorption spectrometry. In spectrometry, the small amount of soil samples mixed with KBr and was taken in a small pill form. For the tests, the pills were put in the center of infrared spectrometer and graphs were obtained. Analysis of data was done using MINITAB and PLSR software. The data obtained from spectrometry method were compared with amount of soil nutrients obtained from direct drug absorption using EXCEL software. There were good fitting between these two data series. For nitrate, phosphorus and potassium R2 was 79.5%, 92.0% and 81.9%, respectively. Also, results showed that the range of MIR (mid-infrared) is appropriate for determine the amount of soil nitrate and potassium and can be used in future research to obtain detailed maps of land in agricultural use.

Keywords: nitrate, phosphorus, potassium, soil nutrients, spectroscopy

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Authors: Marijana M. Ačanski, Kristian A. Pastor, Djura N. Vujić

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The identification of lipid and soluble sugar components in flour samples of different cultivars belonging to common oat species (Avena sativa L.) was performed: spring oat, winter oat and hulless oat. Fatty acids were extracted from flour samples with n-hexane, and derivatized into volatile methyl esters, using TMSH (trimethylsulfonium hydroxide in methanol). Soluble sugars were then extracted from defatted and dried samples of oat flour with 96% ethanol, and further derivatized into corresponding TMS-oximes, using hydroxylamine hydrochloride solution and BSTFA (N,O-bis-(trimethylsilyl)-trifluoroacetamide). The hexane and ethanol extracts of each oat cultivar were analyzed using GC-MS system. Lipid and simple sugar compositions are very similar in all samples of investigated cultivars. Chemometric tool was applied to numeric values of automatically integrated surface areas of detected lipid and simple sugar components in their corresponding derivatized forms. Hierarchical cluster analysis shows a very high similarity between the investigated flour samples of oat cultivars, according to the fatty acid content (0.9955). Moderate similarity was observed according to the content of soluble sugars (0.50). These preliminary results support the idea of establishing methods for oat flour authentication, and provide the means for distinguishing oat flour samples, regardless of the variety, from flour samples made of other cereal species, just by lipid and simple sugar profile analysis.

Keywords: oat cultivars, lipid composition, soluble sugar composition, GC-MS, chemometrics, authentication

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Authors: Muhammad Ajmal, Muhammad Siddiq, Nurettin Sahiner

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We prepared poly(methacrylic acid-co-acrylonitrile) (p(MAc-co-AN)) microgels by inverse suspension polymerization, and converted the nitrile groups into amidoxime groups to obtain more hydrophilic amidoximated poly(methacrylic acid-co-acrylonitile) (amid-p(MAc-co-AN)) microgels. Amid-microgels were used as microreactors for in situ synthesis of copper and cobalt nanoparticles. Cu (II) and Co (II) ions were loaded into microgels from their aqueous metal salt solutions and then converted to corresponding metal nanoparticle (MNP) by treating the loaded metal ions with sodium borohydride (NaBH4). The characterization of the prepared microgels and microgel metal nanoparticle composites was carried out by SEM, TEM and TG analysis. The amounts of metal nanoparticles within microgels were estimated by AAS measurements by dissolving the MNP entrapped within microgels by concentrated HCl acid treatment. Catalytic performances of the prepared amid-p(MAc-co-AN)-M (M: Cu, Co) microgel composites were investigated by using them as catalyst for the degradation of cationic and anionic organic dyes such as eosin Y (EY), methylene blue (MB) and methyl Orange (MO), and for the reduction of nitro aromatic pollutants like 2-nitrophenol (2-NP) and 4-nitrophenol (4-NP) to their corresponding amino phenols. Here, we also report for the first time, the simultaneous degradation/reduction of MB, EY, and 4-NP by amid-p(MAc-co-AN)-Cu microgel composites. Different parameters affecting the reduction rates such as metal types, amount of catalysts, temperature and the amount of reducing agent were investigated.

Keywords: microgels, nanoparticles, catalyst, pollutants

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Authors: P. S. Jain, K. D. Bobade, S. J. Surana

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A simple, selective, precise and Stability-indicating High-performance thin-layer chromatographic method for analysis of Naftopidil both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed, HPTLC aluminium plates precoated with silica gel as the stationary phase. The solvent system consisted of hexane: ethyl acetate: glacial acetic acid (4:4:2 v/v). The system was found to give compact spot for Naftopidil (Rf value of 0.43±0.02). Densitometric analysis of Naftopidil was carried out in the absorbance mode at 253 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2=0.999±0.0001 with respect to peak area in the concentration range 200-1200 ng per spot. The method was validated for precision, recovery and robustness. The limits of detection and quantification were 20.35 and 61.68 ng per spot, respectively. Naftopidil was subjected to acid and alkali hydrolysis, oxidation and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and thermal conditions. This indicates that the drug is susceptible to acid, base, oxidation and thermal conditions. The degraded product was well resolved from the pure drug with significantly different Rf value. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Naftopidil in bulk drug and pharmaceutical formulation.

Keywords: naftopidil, HPTLC, validation, stability, degradation

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Authors: Sara Torabi, Sadegh Khazalpour, Mahdi Jamshidi

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Nitro aromatic compounds are valuable materials because of their applications in the preparation of chemical intermediates for the synthesis of dyes, plastics, perfumes, energetic materials, and pharmaceuticals. Chemical and electrochemical procedures are reported for nitration of aromatic compounds. Flavonoid derivatives are present in many vegetables and fruits and are constituent of many common pharmaceuticals and dietary supplements. Electrochemistry provides very versatile means for the electrosynthesis, mechanistic and kinetic studies. To the best of our knowledge, and despite the importance of these compounds in numerous scientific fields, there are no reports on the electrochemical nitration of Quercetin derivatives. Herein, we describe a green electrochemical synthesis of a nitro compound. In this work, electrochemical oxidation of Quercetin has been studied in the presence of nitrite ion as a nucleophile in acetate buffer solution (c = 0.2 M, pH = 6.0), by means of cyclic voltammetry and controlled-potential coulometry. The results indicate the participation of produced o-benzoquinones in Michael reaction with nitrite ion (in the divided cell) to form the corresponding nitro diol (EC mechanism). The purity of product and characterization was done using ¹H NMR, ¹³C NMR, FTIR spectroscopic techniques. The presented strategies use a water/ethanol mixture as solvent. Ethanol as cosolvent was also used in the previous studies because of its low cost, safety, easy availability, recyclability, bioproductability, and biodegradability. These strategies represent a one-pot and facile process for the synthesis of nitro compound in high yield and purity under green conditions.

Keywords: electrochemical synthesis, green chemistry, cyclic voltammetry, molecular docking

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Authors: Saleh N. Maodaa

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Background: Lead (Pb) is an environmental pollutant causing serious health problems, including impairment of reproduction. Visnagin (VIS) is a furanochromone with promising antioxidant and anti-inflammatory effects; however, its protective efficacy against Pb toxicity has not been investigated. Objective: This study evaluated the protective effect of VIS on Pb reproductive toxicity, impaired steroidogenesis and spermatogenesis, oxidative stress and inflammation. Methods: Rats received VIS (30 or 60 mg/kg) and 50 mg/kg lead acetate for 3 weeks, and blood and testes samples were collected. Results: Pb intoxication impaired the pituitary-testicular axis (PTA), manifested by the decreased serum levels of gonadotropins and testosterone. Pb decreased sperm count, motility and viability, increased sperm abnormalities, and downregulated the steroidogenesis markers StAR, CYP17A1, 3β-HSD and 17β-HSD in the testis of rats. VIS significantly increased serum gonadotropins and testosterone, alleviated sperm parameters and upregulated steroidogenesis. In addition, VIS decreased pro-inflammatory cytokines, testicular lipid peroxidation and DNA fragmentation, downregulated Bax, and enhanced antioxidants and Bcl-2 Conclusion: These results demonstrate the protective effect of VIS against Pb reproductive toxicity in rats. VIS improved serum gonadotropins and testosterone, enhanced steroidogenesis and spermatogenesis, and attenuated oxidative injury, inflammation and apoptosis. Therefore, VIS is a promising candidate for the protection against Pb-induced reproduction impairment.

Keywords: pituitary-gonadal axis, cytokines, DNA damage, apoptosis

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Authors: Mohd Adil, Rosina Khan, Danishuddin, Asad U. Khan

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The aim of this study was to evaluate the influence of the crude and active solvent fraction of Trachyspermum ammi on S. mutans cariogenicity, effect on expression of genes involved in biofilm formation and caries development in rats. GC–MS was carried out to identify the major components present in the crude and the active fraction of T. ammi. The crude extract and the solvent fraction exhibiting least MIC were selected for further experiments. Scanning electron microscopy was carried out to observe the effect of the extracts on S. mutans biofilm. Comparative gene expression analysis was carried out for nine selected genes. 2-Isopropyl-5-methyl-phenol was found as major compound in crude and the active fraction. Binding site of this compound within the proteins involved in biofilm formation was mapped with the help of docking studies. Real-time RT-PCR analyses revealed significant suppression of the genes involved in biofilm formation. All the test groups showed reduction in caries (smooth surface as well as sulcal surface caries) in rats. Moreover, it also provides new insight to understand the mechanism influencing biofilm formation in S. mutans. Furthermore, the data suggest the putative cariostatic properties of T. Ammi and hence can be used as an alternative medicine to prevent caries infection.

Keywords: bio-film, Streptococcus mutans, dental caries, bio-informatic

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Authors: Shaya Mahmoudian, Mohammad Reza Sazegar, Nazanin Afshari

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Graphene, a single layer of carbon atoms in a hexagonal lattice, has recently attracted great attention due to its unique mechanical, thermal and electrical properties. The high aspect ratio and unique surface features of graphene resulted in significant improvements of the nano composites properties. In this study, nano composite fibres made of cellulose and graphene nano platelets were wet spun from solution by using ionic liquid, 1-ethyl-3-methylimidazolium acetate (EMIMAc) as solvent. The effect of graphene loading on the thermal and electrical properties of the nanocomposite fibres was investigated. The nano composite fibres characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. XRD analysis revealed a cellulose II crystalline structure for regenerated cellulose and the nano composite fibres. SEM images showed a homogenous morphology and round cross section for the nano composite fibres along with well dispersion of graphene nano platelets in regenerated cellulose matrix. The incorporation of graphene into cellulose matrix generated electrical conductivity. At 6 wt. % of graphene, the electrical conductivity was 4.7 × 10-4 S/cm. The nano composite fibres also showed considerable improvements in thermal stability and char yield compared to pure regenerated cellulose fibres. This work provides a facile and environmentally friendly method of preparing nano composite fibres based on cellulose and graphene nano platelets that can find several applications in cellulose-based carbon fibres, conductive fibres, apparel, etc.

Keywords: nanocomposite, graphene nanoplatelets, regenerated cellulose, electrical properties

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Authors: Y. Kalachyova, O. Lyutakov, V. Svorcik

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One of the most significant obstacles for the application of surface enhanced Raman spectroscopy (SERS) is the poor reproducibility of SERS active substrates: SERS intensity can be varied from one substrate to another and moreover along the one substrate surface. High enhancement of the near-field intensity is the key factor for ultrasensitive SERS realization. SERS substrate can be prepared through introduction of highly ordered metal array, where light focusing is achieved through excitation of surface plasmon-polaritons (SPPs). In this work, we report the preparation of silver nanostructures with plasmon absorption peaks tuned by the metal arrangement. Excimer laser modification of poly(methyl methacrylate) followed by silver evaporation is proposed as an effective way for the creation of reproducible and effective surface plasmon-polaritons (SPP)-based SERS substrate. Theoretical and experimental studies were performed to optimize structure parameter for effective SPP excitation. It was found that the narrow range of grating periodicity and metal thickness exist, where SPPs can be most efficiently excited. In spite of the fact, that SERS response was almost always achieved, the enhancement factor was found to vary more with the effectivity of SPP excitation. When the real structure parameters were set to optimal for SPP excitation, a SERS enhancement factor was achieved up to four times. Theoretical and experimental investigation of SPP excitation on the two-dimensional periodical silver array was performed with the aim to make SERS response as high as possible.

Keywords: grating, nanostructures, plasmon-polaritons, SERS

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Authors: Radovan Cobanovic, Milica Rankov Sicar

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Biodiesel refers to a vegetable oil - or animal fat-based diesel fuel consisting of long-chain alkyl (methyl, ethyl, or propyl) esters. It is derived by alcoholysis of triacylglycerols (triglycerides) from various lipid based materials that can be traditionally categorized into the following main groups: vegetable oils, animal fats, waste and algal oils. The goal of this study was to evaluate microbiological stability of biodiesel samples since it has been made from vegetable oil or animal fat which was stored on room temperature. For the purposes of this study, analyzes were conducted on six samples of biodiesel first at zero sample at the reception day than fifth, thirtieth, sixtieth, ninetieth and one hundred twentieth day from the day of reception. During this period, biodiesel samples were subjected to microbiological analyses (Salmonella spp., Listeria monocytogenes, Enterobacteriaceae and total plate count). All analyses were tested according to ISO methodology: Salmonella spp ISO 6579, Listeria monocytogenes ISO 11290-2, Enterobacteriaceae ISO 21528-1, total plate count ISO 4833-1. The results obtained after the analyses which were done according to the plan during the 120 days indicate that are no changes of products concerning microbiological analyses. Salmonella spp., Listeria monocytogenes, Enterobacteriaceae were not detected and results for total plate count showed values < 10 cfu/g for all six samples. On the basis of this monitoring under defined storage conditions at room temperatures, the results showed that biodiesel is very stable as far as microbiological analysis were concerned.

Keywords: biodiesel, microbiology, room temperature, stability

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Authors: Bilal Bhat, M. Masroor A. Khan, Moin Uddin, M. Naeem

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Aromatic herb, peppermint (Mentha piperita L.), is a natural hybrid (M. aquatica × M. spicata) with immense therapeutic uses, apart from other potential uses. Peppermint oil is one of the most popular and widely used essential oil (EO), because of its main components menthol and menthone. In view of enhancing growth, yield and quality of this medicinally important herb, a pot experiment was conducted in the net-house of the department. The experiment was aimed at studying the effect of graded levels of N, P, and K on growth, biochemical characteristics, and content and composition of EO in Mentha piperita L. Six NPK treatments (viz. N0P0K0, N20P20K20, N40P40K40, N20+20 P20+20 K20+20, N60P60K60, and N30+30 P30+30 K30+30) were tested. The plants were harvested 150 days after transplanting. The crop performance was assessed in terms of growth attributes, physiological activities, herbage yield and content as well as yield of active constituents of Mentha piperita L. Biochemical parameters were analyzed spectrophotometrically. The EO was extracted using Clevenger’s apparatus and the active constituents of the oil were determined using Gas Chromatography. Split-dose application of N, P and K (N30+30 P30+30 K30+30) ameliorated most of the parameters significantly including, fresh and dry weight of plant, NPK content, chlorophyll and carotenoids content, and the activities of carbonic anhydrase and nitrate reductase in the leaves. It also enhanced the EO content (44.0%), EO yield (91.0%), menthol content (14.1%), menthone content (34.0%), menthyl acetate content (16.9%) and 1, 8-cineole content (43.7%) but decreased the pulegone content (36.8%). Conclusively, the fertilization proved useful in enhancing the EO content, yield and other EO components of the plant. Thus, the yield and quality of EO of peppermint may be improved by this agricultural strategy.

Keywords: mentha piperita, menthol, menthone, EO

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Authors: Elene Tatunashvili, Bun Chan, Philippe E. Nashar, Christopher S. P. McErlean

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The reduction of aryl diazonium salts is one of the most efficient ways to generate aryl radicals for use in a wide range of transformations, including Sandmeyer-type reactions, Meerwein arylations of olefins and Gomberg-Bachmann-Hey arylations of heteroaromatic systems. The aryl diazonium species can be reduced electrochemically, by UV irradiation, inner-sphere and outer-sphere single electron transfer processes (SET) from metal salts, SET from photo-excited organic catalysts or fragmentation of adducts with weak bases (acetate, hydroxide, etc.). This paper details an approach for the metal-free reduction of aryl diazonium salts, which facilitates the efficient synthesis of various aromatic compounds under exceedingly mild reaction conditions. By measuring the oxidation potential of a number of organic molecules, a series of nucleophiles were identified that reduce aryl diazonium salts via the addition-fragmentation mechanism. This approach leads to unprecedented operational simplicity: The reactions are very rapid and proceed in the open air; there is no need for external irradiation or heating, and the process is compatible with a large number of radical reactions. We illustrate these advantages by using the addition-fragmentation strategy to regioselectively arylate a series of heterocyclic compounds, to synthesize ketones by arylation of silyl enol ethers, and to synthesize benzothiophene and phenanthrene derivatives by radical annulation reactions.

Keywords: diazonium salts, hantzsch esters, oxygen, radical reactions, synthetic methods

Procedia PDF Downloads 113

Authors: Y. T. Gebreslassie, Abrha Tadesse, R. C. Saini, Rishi Pal

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Caffeine, known chemically as 3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione, is a naturally occurring alkaloid classified as an N-methyl derivative of xanthine. Given its widespread use in coffee and other caffeine-containing products, it is the most commonly consumed psychoactive substance in everyday human life. This research aimed to develop a cost-effective, sensitive, and easily manufacturable sensor for the detection of caffeine. Antraquinone-modified carbon paste electrode (AQMCPE) was fabricated, and the electrochemical behavior of caffeine on this electrode was investigated using cyclic voltammetry (CV) and square wave voltammetry (SWV) in a solution of 0.1M perchloric acid at pH 0.56. The modified electrode displayed enhanced electrocatalytic activity towards caffeine oxidation, exhibiting a two-fold increase in peak current and an 82 mV shift of the peak potential in the negative direction compared to an unmodified carbon paste electrode (UMCPE). Exploiting the electrocatalytic properties of the modified electrode, SWV was employed for the quantitative determination of caffeine. Under optimized experimental conditions, a linear relationship between peak current and concentration was observed within the range of 2.0 x 10⁻⁶ to 1.0× 10⁻⁴ M, with a correlation coefficient of 0.998 and a detection limit of 1.47× 10⁻⁷ M (signal-to-noise ratio = 3). Finally, the proposed method was successfully applied to the quantitative analysis of caffeine in pharmaceutical formulations, yielding recovery percentages ranging from 95.27% to 106.75%.

Keywords: antraquinone-modified carbon paste electrode, caffeine, detection, electrochemical sensor, quantitative analysis

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Authors: Jianfang Wang, Xianzhe Chen, Zhuoliang Liu, Cheng-An Tao, Yujiao Li

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Organophosphorus (OPs) pesticide used as insecticides are widely used in agricultural pest control, household and storage deworming. The detection of pesticides needs more simple and efficient methods. One of the best ways is to make electrochemical biosensors. In this paper, an electrochemical enzyme biosensor based on acetylcholine esterase (AChE) was constructed, and its sensing properties and sensing mechanisms were studied. Reduced graphene oxide-polydopamine complexes (RGO-PDA), gold nanoparticles (AuNPs) and silver nanoparticles (AgNPs) were prepared firstly and composited with AChE and chitosan (CS), then fixed on the glassy carbon electrode (GCE) surface to construct the biosensor GCE/RGO-PDA-AuNPs-AgNPs-AChE-CS by one-pot method. The results show that graphene oxide (GO) can be reduced by dopamine (DA) and dispersed well in RGO-PDA complexes. And the composites have a synergistic catalysis effect and can improve the surface resistance of GCE. The biosensor selectively can detect acetylcholine (ACh) and OPs pesticide with good linear range and high sensitivity. The performance of the biosensor is affected by the ratio and adding ways of AChE and the adding of AuNPs and AChE. And the biosensor can achieve a detection limit of 2.4 ng/L for methyl parathion and a wide linear detection range of 0.02 ng/L ~ 80 ng/L, and has excellent stability, good anti-interference ability, and excellent preservation performance, indicating that the sensor has practical value.

Keywords: acetylcholine esterase, electrochemical biosensor, nanoparticles, organophosphates, reduced graphene oxide

Procedia PDF Downloads 86