Search results for: non aqueous solvent

Authors: Niharul Alam

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The development of energy efficient, economic and eco-friendly synthetic protocols for metal nanoparticles (NPs) with tailor-made structural properties and biocompatibility is a highly cherished goal for researchers working in the field of nanoscience and nanotechnology. In this context, green chemistry is highly relevant and the 12 principles of Green Chemistry can be explored to develop such synthetic protocols which are practically implementable. One of the most promising green chemical synthetic methods which can serve the purpose is biogenic synthetic protocol, which utilizes non-toxic multifunctional reactants derived from natural, biological sources ranging from unicellular organisms to higher plants that are often characterized as “medicinal plants”. Over the past few years, a plethora of medicinal plants have been explored as the source of this kind of multifunctional green chemical agents. In this presentation, we focus on the syntheses of stable monometallic Au and Ag NPs and also bimetallic Au/Ag alloy NPs with highly efficient catalytic property using aqueous extract of leaves of Indian Curry leaf plat (Murraya koenigii Spreng.; Fam. Rutaceae) as green multifunctional agents which is extensively used in Indian traditional medicine and cuisine. We have also studied the interaction between the synthesized metal NPs and surface-adsorbed fluorescent moieties, quercetin and quercetin glycoside which are its chemical constituents. This helped us to understand the surface property of the metal NPs synthesized by this plant based biogenic route and to predict a plausible mechanistic pathway which may help in fine-tuning green chemical methods for the controlled synthesis of various metal NPs in future. We observed that simple experimental parameters e.g. pH and temperature of the reaction medium, concentration of multifunctional agent and precursor metal ions play important role in the biogenic synthesis of Au NPs with finely tuned structures.

Keywords: green multifunctional agent, metal nanoparticles, biogenic synthesis

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Authors: Sonal Gupta, Rakhi Bansal, Javed Ali, Reema Gabrani, Shweta Dang

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Nanoemulsions (NEs) and microemulsions (MEs) have been an attractive tool for encapsulation of both hydrophilic and lipophillic actives. Both these systems are composed of oil phase, surfactant, co-surfactant and aqueous phase. Depending upon the application and intended use, both oil-in-water and water-in-oil emulsions can be designed. NEs are fabricated using high energy methods employing less percentage of surfactant as compared to MEs which are self assembled drug delivery systems. Owing to the nanometric size of the droplets these systems have been widely used to enhance solubility and bioavailability of natural as well as synthetic molecules. The aim of the present study is to assess the effect of % age of surfactants on cell viability of Vero cells (African Green Monkeys’ Kidney epithelial cells) via MTT assay. Green tea catechin (Polyphenon 60) loaded ME employing low energy vortexing and NE employing high energy ultrasonication were prepared using same excipients (labrasol as oil, cremophor EL as surfactant and glycerol as co-surfactant) however, the % age of oil and surfactant needed to prepare the ME was higher as compared to NE. These formulations along with their excipients (oilME=13.3%, SmixME=26.67%; oilNE=10%, SmixNE=13.52%) were added to Vero cells for 24 hrs. The tetrazolium dye, 3-(4,5-dimethylthia/ol-2-yl)-2,5-diphi-iiyltclrazolium bromide (MTT), is reduced by live cells and this reaction is used as the end point to evaluate the cytoxicity level of a test formulation. Results of MTT assay indicated that oil at different percentages exhibited almost equal cell viability (oilME ≅ oilNE) while surfactant mixture had a significant difference in the cell viability values (SmixME < SmixNE). Polyphenon 60 loaded ME and its PlaceboME showed higher toxicity as compared to Polyphenon 60 loaded NE and its PlaceboNE that can be attributed to the higher concentration of surfactants present in MEs. Another probable reason for high % cell viability of Polyphenon 60 loaded NE might be due to the effective release of Polyphenon 60 from NE formulation that helps in the sustenance of Vero cells.

Keywords: cell viability, microemulsion, MTT, nanoemulsion, surfactants, ultrasonication

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Authors: Moshe Mello, Hilary Rutto, Tumisang Seodigeng

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The nature of tires makes them extremely challenging to recycle due to the available chemically cross-linked polymer and, therefore, they are neither fusible nor soluble and, consequently, cannot be remolded into other shapes without serious degradation. Open dumping of tires pollutes the soil, contaminates underground water and provides ideal breeding grounds for disease carrying vermins. The thermal decomposition of tires by pyrolysis produce char, gases and oil. The composition of oils derived from waste tires has common properties to commercial diesel fuel. The problem associated with the light oil derived from pyrolysis of waste tires is that it has a high sulfur content (> 1.0 wt.%) and therefore emits harmful sulfur oxide (SOx) gases to the atmosphere when combusted in diesel engines. Desulphurization of TPO is necessary due to the increasing stringent environmental regulations worldwide. Hydrodesulphurization (HDS) is the commonly practiced technique for the removal of sulfur species in liquid hydrocarbons. However, the HDS technique fails in the presence of complex sulfur species such as Dibenzothiopene (DBT) present in TPO. This study aims to investigate the viability of photodegradation (Photocatalytic oxidative desulphurization) and adsorptive desulphurization technologies for efficient removal of complex and non-complex sulfur species in TPO. This study focuses on optimizing the cleaning (removal of impurities and asphaltenes) process by varying process parameters; temperature, stirring speed, acid/oil ratio and time. The treated TPO will then be sent for vacuum distillation to attain the desired diesel like fuel. The effect of temperature, pressure and time will be determined for vacuum distillation of both raw TPO and the acid treated oil for comparison purposes. Polycyclic sulfides present in the distilled (diesel like) light oil will be oxidized dominantly to the corresponding sulfoxides and sulfone via a photo-catalyzed system using TiO2 as a catalyst and hydrogen peroxide as an oxidizing agent and finally acetonitrile will be used as an extraction solvent. Adsorptive desulphurization will be used to adsorb traces of sulfurous compounds which remained during photocatalytic desulphurization step. This desulphurization convoy is expected to give high desulphurization efficiency with reasonable oil recovery.

Keywords: adsorption, asphaltenes, photocatalytic oxidation, pyrolysis

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Authors: Liana C. Salanță, Maria Tofană, Carmen R. Pop, Vlad Mureșan

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The landscape of functional food is expanding very fast, due to the consumer interest for healthy natural products. Consumers nowadays demand healthy products that impart phytonutrients to encourage good health and well-being, prevent diseases, without sacrificing taste and texture. Candies are foodstuffs appreciated by all category of consumers. They are available in a range variety of forms (jellies, marshmallows, caramels, lollipops, etc.). Jelly is characterized by a gummy and chewy texture typically conferred by a hydrocolloid (gelatin, pectin). The purpose of this research was to obtain hypocaloric jelly (no added sugar) enriched with protein powder from acai, chia seeds and hemp, which are considered superfood. Peach and raspberry juice were used for obtaining functional jelly, due to the specific flavour, natural carbohydrate, natural pigments and vitamins (C, B1, PP, etc). Instead of classic hydrocolloids used in Romania for the industry of jelly, agar-agar was used in this study, due to its properties. Agar-agar is able to form gels in the aqueous medium, stronger than other gel-forming agents. High sugar concentrations or an acid environment (as is necessary with pectins) are not needed. In addition to its gelation properties, Agar-agar is considered to have important nutritional benefits, high content of fibre and has low calories. Six prototypes of jellies were obtained and evaluated by physicochemical, microbiological and sensorial analysis. For the textural profile analysis, the Brookfield CT3 Texture Analyzer, equipped with a 10kg load cell, was used. The results revealed that hypocaloric jelly can serve as a good source of bioactive compounds in the diet. The jelly is a convenient way of delivering potential health benefits of protein powder and agar-agar to a wide range of consumers.

Keywords: agar-agar, functional food, hypocaloric jelly, superfoods

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Authors: Omkar Gaonkar, Indumathi Nambi, Suresh G. Kumar

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The functional and morphological aspects of soil structure determine the soil quality. The dispersion of colloidal soil particles, especially the clay fraction and rupture of soil aggregates, both of which play an important role in soil structure development, lead to degradation of soil quality. The main objective of this work was to determine the effect of the behaviour of soil colloids on the agricultural soil structure and quality. The effect of commercial humic acid and soil natural organic matter on the electrical and structural properties of the soil colloids was also studied. Agricultural soil, belonging to the sandy loam texture class from northern part of India was considered in this study. In order to understand the changes in the soil quality in the presence and absence of humic acids, the soil fabric and structure was analyzed by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) Spectroscopy and Scanning Electron Microscopy (SEM). Electrical properties of natural soil colloids in aqueous suspensions were assessed by zeta potential measurements at varying pH values with and without the presence of humic acids. The influence of natural organic matter was analyzed by oxidizing the natural soil organic matter with hydrogen peroxide. The zeta potential of the soil colloids was found to be negative in the pH range studied. The results indicated that hydrogen peroxide treatment leads to deflocculation of colloidal soil particles. In addition, the humic acids undergoes effective adsorption onto the soil surface imparting more negative zeta potential to the colloidal soil particles. The soil hydrophilicity decreased in the presence of humic acids which was confirmed by surface free energy determination. Thus, it can be concluded that the presence of humic acids altered the soil fabric and structure, thereby affecting the soil quality. This study assumes significance in understanding soil aggregation and the interactions at soil solid-liquid interface.

Keywords: humic acids, natural organic matter, zeta potential, soil quality

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Authors: Jiahui Song

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The use of electric fields with high intensity (~ 100kV/cm or higher) and ultra short pulse durations (nanosecond range) has been a recent development. Most of the studies of electroporation have ignored possible thermal effects because of the small duration of the applied voltage pulses. However, it has been predicted membrane temperature gradients ranging from 0.2×109 to 109 K/m. This research focuses on thermal effects that drive for electroporative enhancements, even though the actual temperature values might not have changed appreciably from their equilibrium levels. The dynamics of pore formation with the application of an externally applied electric field is studied on the basis of molecular dynamics (MD) simulations using the GROMACS package. MD simulations of a lipid layer with constant electric field strength of 0.5 V/nm at 25 °C and 47 °C are implemented to simulate the appropriate thermal effects. The GROMACS provides the force fields for the lipid membranes, which is taken to comprise of dipalmitoyl-phosphatidyl-choline (DPPC) molecules. The water model mimicks the aqueous environment surrounding the membrane. Velocities of water and membrane molecules are generated randomly at each simulation run according to a Maxwellian distribution. The high background electric field is typically used in MD simulations to probe electroporation. It serves as an accelerated test of the pore formation process since low electric fields would take inordinately long simulation time. MD simulation shows no pore is formed in a 1-ns snapshot for a DPPC membrane set at a temperature of 25°C after a 0.5 V/nm electric field is applied. A nano-sized pore is clearly seen in a 0.75-ns snapshot on the same geometry, but with the membrane surfaces kept at temperatures of 47°C. And the pore increases at 1 ns. The MD simulation results suggest the possibility that the increase in temperature can result in different degrees of electrically stimulated bio-effects. The results points to the role of thermal effects in facilitating and accelerating the electroporation process.

Keywords: high-intensity, ultra-short, electroporation, thermal effects, molecular dynamics

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Authors: Abhishek Soti, Aditya Sharma, Akhilendra Bhushan Gupta

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Fouled reverse osmosis membranes are primarily characterized by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectrometer (EDS) for a detailed investigation of foulants; however, this has severe limitations on several accounts. Apart from inaccuracy in spectral properties and inevitable interferences and interactions between sample and instrument, misidentification of elements due to overlapping peaks is a significant drawback of EDS. This paper discusses this limitation by analyzing fouled polyamide RO membranes derived from community RO plants of Rajasthan treating brackish water via a combination of results obtained from EDS and Raman spectroscopy and cross corroborating with ICP-MS analysis of water samples prepared by dissolving the deposited salts. The anomalous behavior of different morphic forms of CaCO₃ in aqueous suspensions tends to introduce false reporting of the presence of certain heavy metals and rare earth metals in the scales of the fouled RO membranes used for treating brackish groundwater when analyzed using the commonly adopted techniques like SEM-EDS or Raman spectrometry. Peaks of CaCO₃ reflected in EDS spectra of the membrane were found to be misinterpreted as Scandium due to the automatic assignment of elements by the software. Similarly, the morphic forms merged with the dominant peak of CaCO₃ might be reflected as a single peak of Molybdenum in the Raman spectrum. A subsequent ICP-MS analysis of the deposited salts showed that both Sc and Mo were below detectable levels. It is always essential to cross-confirm the results through a destructive analysis method to avoid such interferences. It is further recommended to study different morphic forms of CaCO₃ scales, as they exhibit anomalous properties like reverse solubility with temperature and hence altered precipitation tendencies, for an accurate description of the composition of scales, which is vital for the smooth functioning of RO systems.

Keywords: reverse osmosis, foulant analysis, groundwater, EDS, artifacts

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Authors: Zlatina Genisheva, Pedro Ferreira-Santos, Margarida Soares, Cândida Vilarinho, Joana Carvalho

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The wine industry produces significant quantities of waste, much of which remains underutilized as a potential raw material. Typically, this waste is either discarded in the fields or incinerated, leading to environmental concerns. By-products of wine production, like lees and grape pomace, are readily available at relatively low costs and hold promise as raw materials for biochemical conversion into valuable products. Reusing these waste materials is crucial, not only for reducing environmental impact but also for enhancing profitability. The Vinhos Verdes demarcated region, the largest wine-producing area in Portugal, has remained relatively stagnant over time. This project aims to offer an alternative income source for producers in the region while also expanding the limited existing research on this area. The main objective of this project is the study of the sustainable valorization of grape pomace and lees from the production of DOC Vinho Verde. Extraction tests were performed to obtain high-value compounds, targeting phenolic compounds from grape pomace and protein-rich extracts from lees. An environmentally friendly technique, microwave extraction, was used for this process. This method is not only efficient but also aligns with the principles of green chemistry, reducing the use of harmful solvents and minimizing energy consumption. The findings from this study have the potential to open new revenue streams for the region’s wine producers while promoting environmental sustainability. The optimal conditions for extracting proteins from lees involve the use of NaOH at 150ºC. Regardless of the solvent employed, the ideal temperature for obtaining extracts rich in polyphenol compounds and exhibiting strong antioxidant activity is also 150ºC. For grape pomace, extracts with a high concentration of polyphenols and significant antioxidant properties were obtained at 210ºC. However, the highest total tannin concentrations were achieved at 150ºC, while the maximum total flavonoid content was obtained at 170ºC.

Keywords: antioxidants, circular economy, polyphenol compounds, waste valorization

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Authors: Sidra Pervez, Afsheen Aman, Shah Ali Ul Qader

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The importance of attaining an optimum performance of an enzyme is often a question of devising an effective method for its immobilization. Cross-linked enzyme aggregate (CLEAs) is a new approach for immobilization of enzymes using carrier free strategy. This method is exquisitely simple (involving precipitation of the enzyme from aqueous buffer followed by cross-linking of the resulting physical aggregates of enzyme molecules) and amenable to rapid optimization. Among many industrial enzymes, amyloglucosidase is an important amylolytic enzyme that hydrolyzes alpha (1→4) and alpha (1→6) glycosidic bonds in starch molecule and produce glucose as a sole end product. Glucose liberated by amyloglucosidase can be used for the production of ethanol and glucose syrups. Besides this amyloglucosidase can be widely used in various food and pharmaceuticals industries. For production of amyloglucosidase on commercial scale, filamentous fungi of genera Aspergillus are mostly used because they secrete large amount of enzymes extracellularly. The current investigation was based on isolation and identification of filamentous fungi from genus Aspergillus for the production of amyloglucosidase in submerged fermentation and optimization of cultivation parameters for starch saccharification. Natural isolates were identified as Aspergillus niger KIBGE-IB36, Aspergillus fumigatus KIBGE-IB33, Aspergillus flavus KIBGE-IB34 and Aspergillus terreus KIBGE-IB35 on taxonomical basis and 18S rDNA analysis and their sequence were submitted to GenBank. Among them, Aspergillus fumigatus KIBGE-IB33 was selected on the basis of maximum enzyme production. After optimization of fermentation conditions enzyme was immobilized on CLEA. Different parameters were optimized for maximum immobilization of amyloglucosidase. Data of enzyme stability (thermal and Storage) and reusability suggested the applicability of immobilized amyloglucosidase for continuous saccharification of starch in industrial processes.

Keywords: aspergillus, immobilization, industrial processes, starch saccharification

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Authors: Okugbe Ebiotubo Ohore, Jingli Zhang, Binessi Edouard Ifon, Mathieu Nsenga Kumwimba, Xiaoying Mu, Dai Kuang, Zhen Wang, Ji-Dong Gu, Guojing Yang

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Antibiotic pollution and the evolution of antibiotic resistance genes (ARGs) are increasingly viewed as major threats to both ecosystem security and human health, and has drawn attention. This study investigated the fate of antibiotics in aqueous and sedimentary substrates and the impact of ecosystem shifts between water and sedimentary phases on resistome profiles. The findings indicated notable variations in the concentration and distribution patterns of antibiotics across various environmental phases. Based on the partition coefficient (Kd), the total antibiotic concentration was significantly greater in the surface water (1405.45 ng/L; 49.5%) compared to the suspended particulate matter (Kd =0.64; 892.59 ng/g; 31.4%) and sediment (Kd=0.4; 542.64 ng/g; 19.1%). However, the relative abundance of ARGs in surface water and sediment was disproportionate to the abundance of antibiotics concentration, and sediments were the predominant ARGs reservoirs. Phylogenetic divergence of the microbial communities between the surface water and the sedimentary ecosystems potentially played important roles in driving the ARGs profiles between the two distinctive ecosystems. ARGs of Clinical importance; including blaGES, MCR-7.1, ermB, tet(34), tet36, tetG-01, and sul2 were significantly increased in the surface water, while blaCTX-M-01, blaTEM, blaOXA10-01, blaVIM, tet(W/N/W), tetM02, and ermX were amplified in the sediments. cfxA was an endemic ARG in surface-water ecosystems while the endemic ARGs of the sedimentary ecosystems included aacC4, aadA9-02, blaCTX-M-04, blaIMP-01, blaIMP-02, bla-L1, penA, erm(36), ermC, ermT-01, msrA-01, pikR2, vgb-01, mexA, oprD, ttgB, and aac. These findings offer a valuable information for the identification of ARGs-specific high-risk reservoirs.

Keywords: antibiotic resistance genes, microbial diversity, suspended particulate matter, sediment, surface water

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Authors: Sara Mosallanejad, Bogdan Z. Dlugogorski, Jeff Gore, Mohammednoor Altarawneh

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Ammonium nitrate (NH­₄NO₃, AN) is commonly used as the main component of AN emulsion and fuel oil (ANFO) explosives, that use extensively in civilian and mining operations for underground development and tunneling applications. The emulsion formulation and wettability of AN prills, which affect the physical stability and detonation of ANFO, highly depend on the surface tension, density, viscosity of the used liquid. Therefore, for engineering applications of this material, the determination of density and surface tension of concentrated aqueous solutions of AN is essential. The molecular dynamics (MD) simulation method have been used to investigate the density and the surface tension of high concentrated ammonium nitrate solutions; up to its solubility limit in water. Non-polarisable models for water and ions have carried out the simulations, and the electronic continuum correction model (ECC) uses a scaling of the charges of the ions to apply the polarisation implicitly into the non-polarisable model. The results of calculated density and the surface tension of the solutions have been compared to available experimental values. Our MD simulations show that the non-polarisable model with full-charge ions overestimates the experimental results while the reduce-charge model for the ions fits very well with the experimental data. Ions in the solutions show repulsion from the interface using the non-polarisable force fields. However, when charges of the ions in the original model are scaled in line with the scaling factor of the ECC model, the ions create a double ionic layer near the interface by the migration of anions toward the interface while cations stay in the bulk of the solutions. Similar ions orientations near the interface were observed when polarisable models were used in simulations. In conclusion, applying the ECC model to the non-polarisable force field yields the density and surface tension of the AN solutions with high accuracy in comparison to the experimental measurements.

Keywords: ammonium nitrate, electronic continuum correction, non-polarisable force field, surface tension

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Authors: Bharti Jain, Rajeev Jain, Abuzar Kabir, Torki Zughaibi, Shweta Sharma

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Drug-facilitated crimes (DFCs) entail the use of a single drug or a mixture of drugs to render a victim unable. Traditionally, biological samples have been gathered from victims and conducted analysis to establish evidence of drug administration. Nevertheless, the rapid metabolism of various drugs and delays in analysis can impede the identification of such substances. For this, the present article describes a rapid, sustainable, highly efficient and miniaturized protocol for the identification and quantification of three sedative-hypnotic drugs, namely diazepam, chlordiazepoxide and ketamine in alcoholic beverages and complex food samples (cream of biscuit, flavored milk, juice, cake, tea, sweets and chocolate). The methodology involves utilizing fabric phase sorptive extraction (FPSE) to extract diazepam (DZ), chlordiazepoxide (CDP), and ketamine (KET). Subsequently, the extracted samples are subjected to analysis using gas chromatography-mass spectrometry (GC-MS). Several parameters, including the type of membrane, pH, agitation time and speed, ionic strength, sample volume, elution volume and time, and type of elution solvent, were screened and thoroughly optimized. Sol-gel Carbowax 20M (CW-20M) has demonstrated the most effective extraction efficiency for the target analytes among all evaluated membranes. Under optimal conditions, the method displayed linearity within the range of 0.3–10 µg mL–¹ (or µg g–¹), exhibiting a coefficient of determination (R2) ranging from 0.996–0.999. The limits of detection (LODs) and limits of quantification (LOQs) for liquid samples range between 0.020-0.069 µg mL-¹ and 0.066-0.22 µg mL-¹, respectively. Correspondingly, the LODs for solid samples ranged from 0.056-0.090 µg g-¹, while the LOQs ranged from 0.18-0.29 µg g-¹. Notably, the method showcased better precision, with repeatability and reproducibility both below 5% and 10%, respectively. Furthermore, the FPSE-GC-MS method proved effective in determining diazepam (DZ) in forensic food samples connected to drug-facilitated crimes (DFCs). Additionally, the proposed method underwent evaluation for its whiteness using the RGB12 algorithm.

Keywords: drug facilitated crime, fabric phase sorptive extraction, food forensics, white analytical chemistry

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Authors: Md. Maksudur Rahman Khan, M. Rahim Uddin, Hamidah Abdullah, Kaykobad Md. Rezaul Karim, Abu Yousuf, Chin Kui Cheng, Huei Ruey Ong

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A systematic study was conducted to explore the photocatalytic reduction of carbon dioxide (CO₂) into methanol on TiO₂ loaded copper ferrite (CuFe₂O₄) photocatalyst under visible light irradiation. The phases and crystallite size of the photocatalysts were characterized by X-ray diffraction (XRD) and it indicates CuFe₂O₄ as tetragonal phase incorporation with anatase TiO₂ in CuFe₂O₄/TiO₂ hetero-structure. The XRD results confirmed the formation of spinel type tetragonal CuFe₂O₄ phases along with predominantly anatase phase of TiO₂ in the CuFe₂O₄/TiO₂ hetero-structure. UV-Vis absorption spectrum suggested the formation of the hetero-junction with relatively lower band gap than that of TiO₂. Photoluminescence (PL) technique was used to study the electron–hole (e⁻/h⁺) recombination process. PL spectra analysis confirmed the slow-down of the recombination of electron–hole (e⁻/h⁺) pairs in the CuFe₂O₄/TiO₂ hetero-structure. The photocatalytic performance of CuFe₂O₄/TiO₂ was evaluated based on the methanol yield with varying amount of TiO₂ over CuFe₂O₄ (0.5:1, 1:1, and 2:1) and changing light intensity. The mechanism of the photocatalysis was proposed based on the fact that the predominant species of CO₂ in aqueous phase were dissolved CO₂ and HCO₃^- at pH ~5.9. It was evident that the CuFe₂O₄ could harvest the electrons under visible light irradiation, which could further be injected to the conduction band of TiO₂ to increase the life time of the electron and facilitating the reactions of CO₂ to methanol. The developed catalyst showed good recycle ability up to four cycles where the loss of activity was ~25%. Methanol was observed as the main product over CuFe₂O₄, but loading with TiO₂ remarkably increased the methanol yield. Methanol yield over CuFe₂O₄/TiO₂ was found to be about three times higher (651 μmol/g_cat L) than that of CuFe₂O₄ photocatalyst. This occurs because the energy of the band excited electrons lies above the redox potentials of the reaction products CO₂/CH₃OH.

Keywords: photocatalysis, CuFe2O4/TiO2, band-gap energy, methanol

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Authors: Seyedeh Bahar Hashemi, Alireza Rahimi, Mehdi Arjmand

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Food is the source of energy and growth through the breakdown of its vital components and plays a vital role in human health and nutrition. Many natural compounds found in plant and animal materials play a special role in biological systems and the origin of many such compounds directly or indirectly is algae. Algae is an enormous source of polysaccharides and have gained much interest in human flourishing. In this study, algae biomass extraction is conducted using deep eutectic-based solvents (NADES) and Ultrasound-assisted extraction (UAE). The aim of this research is to extract bioactive compounds including total carotenoid, antioxidant activity, and polyphenolic contents. For this purpose, the influence of three important extraction parameters namely, biomass-to-solvent ratio, temperature, and time are studied with respect to their impact on the recovery of carotenoids, and phenolics, and on the extracts’ antioxidant activity. Here we employ the Response Surface Methodology for the process optimization. The influence of the independent parameters on each dependent is determined through Analysis of Variance. Our results show that Ultrasound-assisted extraction (UAE) for 50 min is the best extraction condition, and proline:lactic acid (1:1) and choline chloride:urea (1:2) extracts show the highest total phenolic contents (50.00 ± 0.70 mgGAE/gdw) and antioxidant activity [60.00 ± 1.70 mgTE/gdw, 70.00 ± 0.90 mgTE/gdw in 2.2-diphenyl-1-picrylhydrazyl (DPPH), and 2.2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS)]. Our results confirm that the combination of UAE and NADES provides an excellent alternative to organic solvents for sustainable and green extraction and has huge potential for use in industrial applications involving the extraction of bioactive compounds from algae. This study is among the first attempts to optimize the effects of ultrasonic-assisted extraction, ultrasonic devices, and deep natural eutectic point and investigate their application in bioactive compounds extraction from algae. We also study the future perspective of ultrasound technology which helps to understand the complex mechanism of ultrasonic-assisted extraction and further guide its application in algae.

Keywords: natural deep eutectic solvents, ultrasound-assisted extraction, algae, antioxidant activity, phenolic compounds, carotenoids

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Authors: Snezana Rajkovic, Miroslava Markovic, Ljubinko Rakonjac, Aleksandar Lucic, Radoslav Rajkovic

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Woolly apple aphid, Eriosoma lanigerum (Hausmann) is a widely distributed pest of apple trees, especially where its parasites have been killed by insecticides. It can also be found on pear, hawthorn, mountain ash, and elm trees. Relatively small to medium-sized aphids, characterized by a reddish-brown body, a blood-red stain when crushed and a fluffy, flocculent wax covering. Specialized dermal glands produce the characteristic fluffy or powdery wax, which gives E. lanigerum its characteristic 'woolly' appearance. Also, woolly apple aphid is a problemm in nursery production of spure.The experiments were carried out in the nursery “Nevade” in Gornji Milanovac, "Srbijasume" on the spruce seedlings, aged 2 years. In this study, organic insecticide King Bo, aqueous solution (a. i. oxymatrine 0.2% + psoralen 0.4%), manufacturer Beijing Kingbo Biotech Co. Ltd., Beijing, China. extracted from plants and used as pesticides in nursery production were investigated. King Bo, bioinsecticide is manufactured from refined natural herbal extract several wild medicinal plants, such as Sophora flavescens Ait, Veratrum nigrum L, A. Carmichael, etc. Oxymatrine 2.4 SL is a stomach poison that has antifeeding and repellent action. This substance stimulates development and growth in a host plant and also controls the appearance of downy mildew.The trials were set according to instructions of methods-monitoring of changes in the number of larvae and adults compared to before treatment. The treatment plan was made according to fully randomized block design. The experiment was conducted in four repetitions. The basic plot had the area of 25 m2. Phytotoxicity was estimated by PP methods 1/135 (2), the intensity of infection according to Towsend-Heuberger, the efficiency by Abbott, the analysis of variance with Ducan test and PP/181 (2).

Keywords: bioinsecticide, efficacy, nurssery production, woolly apple aphid

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Authors: Aniela Pop, Ianina Birsan, Corina Orha, Rodica Pode, Florica Manea

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Carbon nanofiber-epoxy composite electrode has been investigated through voltammetric and amperometric techniques in order to detect parabens from aqueous solutions. The occurrence into environment as emerging pollutants of these preservative compounds has been extensively studied in the last decades, and consequently, a rapid and reliable method for their quantitative quantification is required. In this study, methylparaben (MP) and propylparaben (PP) were chosen as representatives for paraben class. The individual electrochemical detection of each paraben has been successfully performed. Their electrochemical oxidation occurred at the same potential value. Their simultaneous quantification should be assessed electrochemically only as general index of paraben class as a cumulative signal corresponding to both MP and PP from solution. The influence of pH on the electrochemical signal was studied. pH ranged between 1.3 and 9.0 allowed shifting the detection potential value to smaller value, which is very desired for the electroanalysis. Also, the signal is better-defined and higher sensitivity is achieved. Differential-pulsed voltammetry and square-wave voltammetry were exploited under the optimum pH conditions to improve the electroanalytical performance for the paraben detection. Also, the operation conditions were selected, i.e., the step potential, modulation amplitude and the frequency. Chronomaprometry application as the easiest electrochemical detection method led to worse sensitivity, probably due to a possible fouling effect of the electrode surface. The best electroanalytical performance was achieved by pulsed voltammetric technique but the selection of the electrochemical technique is related to the concrete practical application. A good reproducibility of the voltammetric-based method using carbon nanofiber-epoxy composite electrode was determined and no interference effect was found for the cation and anion species that are common in the water matrix. Besides these characteristics, the long life-time of the electrode give to carbon nanofiber-epoxy composite electrode a great potential for practical applications.

Keywords: carbon nanofiber-epoxy composite electrode, electroanalysis, methylparaben, propylparaben

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Authors: Mannar R. Maurya, Bithika Sarkar, Fernando Avecilla

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Peroxidase activity is possibly successfully used for different industrial processes in medicine, chemical industry, food processing and agriculture. However, they bear some intrinsic drawback associated with denaturation by proteases, their special storage requisite and cost factor also. Now a day’s artificial enzyme mimics are becoming a research interest because of their significant applications over conventional organic enzymes for ease of their preparation, low price and good stability in activity and overcome the drawbacks of natural enzymes e.g serine proteases. At present, a large number of artificial enzymes have been synthesized by assimilating a catalytic center into a variety of schiff base complexes, ligand-anchoring, supramolecular complexes, hematin, porphyrin, nanoparticles to mimic natural enzymes. Although in recent years a several number of vanadium complexes have been reported by a continuing increase in interest in bioinorganic chemistry. To our best of knowledge, the investigation of artificial enzyme mimics of vanadium complexes is very less explored. Recently, our group has reported synthetic vanadium schiff base complexes capable of mimicking peroxidases. Herein, we have synthesized monoidovanadium(IV) and dioxidovanadium(V) complexes of pyrazoleone derivateis ( extensively studied on account of their broad range of pharmacological appication). All these complexes are characterized by various spectroscopic techniques like FT-IR, UV-Visible, NMR (1H, 13C and 51V), Elemental analysis, thermal studies and single crystal analysis. The peroxidase mimic activity has been studied towards oxidation of pyrogallol to purpurogallin with hydrogen peroxide at pH 7 followed by measuring kinetic parameters. The Michaelis-Menten behavior shows an excellent catalytic activity over its natural counterparts, e.g. V-HPO and HRP. The obtained kinetic parameters (Vmax, Kcat) were also compared with peroxidase and haloperoxidase enzymes making it a promising mimic of peroxidase catalyst. Also, the catalytic activity has been studied towards the oxidation of 1-phenylethanol in presence of H2O2 as an oxidant. Various parameters such as amount of catalyst and oxidant, reaction time, reaction temperature and solvent have been taken into consideration to get maximum oxidative products of 1-phenylethanol.

Keywords: oxovanadium(IV)/dioxidovanadium(V) complexes, NMR spectroscopy, Crystal structure, peroxidase mimic activity towards oxidation of pyrogallol, Oxidation of 1-phenylethanol

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Authors: Ji Un Shin, Wei Mao, Hyuk Sang Yoo

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Electrospinning is a versatile tool for fabricating nano-structured polymeric materials. Gelatin hydrogels are considered to be a good material for cell cultivation because of high water swellability as well as good biocompatibility. Three-dimensional (3-D) cell cultivation is a desirable method of cell cultivation for preparing tissues and organs because cell-to-cell interactions or cell-to-matrix interactions can be much enhanced through this approach. For this reason, hydrogels were widely employed as tissue scaffolds because they can support cultivating cells and tissue in multi-dimensions. Major disadvantages of hydrogel-based cell cultivation include low mechanical properties, lack of topography, which should be enhanced for successful tissue engineering. Herein we surface-immobilized gelatin on the surface of nanofibrous matrix for 3-D cell cultivation in topographical cues added environments. Electrospun nanofibers were electrospun with injection of poly(caprolactone) through a single nozzle syringe. Electrospun meshes were then chopped up with a high speed grinder to fine powders. This was hydrolyzed in optimized concentration of sodium hydroxide solution from 1 to 6 hours and harvested by centrifugation. The freeze-dried powders were examined by scanning electron microscopy (SEM) for revealing the morphology and fibrilar shaped with a length of ca. 20um was observed. This was subsequently immersed in gelatin solution for surface-coating of gelatin, where the process repeated up to 10 times for obtaining desirable coating of gelatin on the surface. Gelatin-coated nanofibrils showed high waterswellability in comparison to the unmodified nanofibrils, and this enabled good dispersion properties of the modified nanofibrils in aqueous phase. The degree of water-swellability was increased as the coating numbers of gelatin increased, however, it did not any meaning result after 10 times of gelatin coating process. Thus, by adjusting the gelatin coating times, we could successfully control the degree of hydrophilicity and water-swellability of nanofibrils.

Keywords: nano, fiber, cell, tissue

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Authors: Debanjan Dey, Tamal Banerjee, Kaustubha Mohanty

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Global scalar properties are calculated based on higher occupied molecular orbital (HOMO) and lower unoccupied molecular orbital (LUMO) energy to study the interaction between ionic liquids with Bituminous and Anthracite coal using density function theory (DFT) method. B3LYP/6-31G* calculation predicts HOMO-LUMO energy gap, electronegativity, global hardness, global softness, chemical potential and global softness for individual compounds with their clusters. HOMO-LUMO interaction, electron delocalization, electron donating and accepting is the main source of attraction between individual compounds with their complexes. Cation used in this study: 1-butyl-1-methylpyrrolidinium [BMPYR], 1-methyl -3-propylimmidazolium [MPIM], Tributylmethylammonium [TMA] and Tributylmethylphosphonium [MTBP] with the combination of anion: bis(trifluromethylsulfonyl)imide [Tf2N], methyl carbonate [CH3CO3], dicyanamide [N(CN)2] and methylsulfate [MESO4]. Basically three-tier approach comprising HOMO/LUMO energy, Scalar quantity and infinite dilution activity coefficient (IDAC) by sigma profile generation with COSMO-RS (Conductor like screening model for real solvent) model was chosen for simultaneous interaction. [BMPYR]CH3CO3] (1-butyl-1-methylpyrrolidinium methyl carbonate) and [MPIM][CH3CO3] (1-methyl -3-propylimmidazolium methyl carbonate ) are the best effective ILs on the basis of HOMO-LUMO band gap for Anthracite and Bituminous coal respectively and the corresponding band gap is 0.10137 hartree for Anthracite coal and 0.12485 hartree for Bituminous coal. Further ionic liquids are screened quantitatively with all the scalar parameters and got the same result based on CH-π interaction which is found for HOMO-LUMO gap. To check our findings IDAC were predicted using quantum chemical based COSMO-RS methodology which gave the same trend as observed our scalar quantity calculation. Thereafter a qualitative measurement is doing by sigma profile analysis which gives complementary behavior between IL and coal that means highly miscible with each other.

Keywords: coal-ionic liquids cluster, COSMO-RS, DFT method, HOMO-LUMO interaction

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Authors: Meriem Abid, Erika Oliveria-Jardim, Andres Fullana, Joaquin Silvestre-Albero

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The rapid industrial development associated with the increase of volatile organic compounds (VOCs) has seriously impacted the environment. Among VOCs, hydrogen sulfide (H₂S) is known as a highly toxic, malodorous, flammable, and corrosive gas, which is emitted from diverse chemical processes, including industrial waste-gas streams, natural gas processing, and biogas purification. The high toxicity, corrosively, and very characteristic odor threshold of H2S call for urgent development of efficient desulfurization processes from the viewpoint of environmental protection and resource regeneration. In order to reduce H₂S emissions, effective technologies for have been performed. The general method of H₂S removal included amine aqueous solution, adsorption process, biological methods, and fixed-bed solid catalytic oxidation processes. Ecologically and economically, low-temperature direct oxidation of H₂S to elemental sulfur using catalytic oxidation is the preferred approach for removing H₂S-containing gas streams. A large number of catalysts made from carbon, metal oxides, clay, and others, have been studied extensively for this application. In this sense, activated carbon (AC) is an attractive catalyst for H₂S removal because it features a high specific surface area, diverse functional groups, low cost, durability, and high efficiency. It is interesting to stand out that AC is modified using metal oxides to promote the efficiency of H₂S removal and to enhance the catalytic performance. Based on these premises, the main goal of the present study is the evaluation of the H₂S adsorption performance in carbon-encapsulated iron nanoparticles obtained from an olive mill, thermally treated at 600, 800 and 1000 ºC temperatures under anaerobic conditions. These results anticipate that carbon-encapsulated iron nanoparticles exhibit a promising performance for the H₂S removal up to 360 mg/g.

Keywords: H₂S removal, catalytic oxidation, carbon encapsulated iron, olive mill wastewater

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Authors: Ai Serizawa, Kotaro Mori, Takahiro Ishizaki

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Al alloys have been used as advanced structural materials in automobile and railway industries because of excellent physical and mechanical properties such as low density, good heat conductivity, and high specific strength. Their low corrosion resistance, however, limits their use in the corrosive environment. To improve the corrosion resistance of the Al alloys, the development of a novel coating technology has been highly desirable. Chemical conversion methods using layered double hydroxide (LDH) have attracted much attention because the LDH can suppress corrosion reaction due to their trapping ability of corrosive anions such as Cl- between layers. In this presentation, we report on a novel preparation method of AlOOH film containing Mg-Al layered double hydroxide (LDH) on Al alloy by steam coating. The corrosion resistance of the composite film including LDH was especially focused. Al-Mg-Si alloy was used as the substrate. The substrates were ultrasonically cleaned in ethanol for 10 min. The cleaned substrates were set in the autoclave with a 100 mL capacity. 20 ml of ultrapure water was located at the bottom of the autoclave to produce steam. The autoclave was heated up to a temperature of 100 to 200 °C, and then held at this temperature for up to 48 h, and was subsequently cooled naturally to room temperature, resulting in the formation of anticorrosive films on Al alloys. The resultant films were characterized by XRD, FT-IR, FE-SEM and electrochemical measurements. FE-SEM image of film surface treated at 180 °C for 48 h demonstrated that needle-like nanostructure was densely formed on the surface. XRD patterns revealed that the film formed on the Al alloys by steam coating was composed of crystal AlOOH and Mg-Al LDH. The corrosion resistance of the film was evaluated using electrochemical measurements. The potentiodynamic polarization curves of the film coated and uncoated substrates of Al-Mg-Si alloy after immersion in the 5 wt% NaCl aqueous solution for 30 min revealed that the corrosion current density, jcorr, of the film coated sample decreased by more than two orders of magnitude as compared to the uncoated sample, indicating that the corrosion resistance of the substrates of Al-Mg-Si alloy were improved by the formation of the anticorrosive film via steam coating.

Keywords: aluminum alloy, boehmite, corrosion resistance, steam process

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Authors: Gargi Prasad, Ashiho A. Mao, Deepu Vijayan, S. Mandal

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The main objective of the present study was to optimize and develop an efficient protocol for in vitro propagation of a medicinally important orchid Cephalantheropsis obcordata (Lindl.) Ormerod along with genetic stability analysis of regenerated plants. This plant has been traditionally used in Chinese folk medicine and the decoction of whole plant is known to possess anticancer activity. Nodal segments used as explants were inoculated on Murashige and Skoog (MS) medium supplemented with various concentrations of isopentenyl adenine (2iP). The rooted plants were successfully acclimatized in the greenhouse with 100% survival rate. Inter-simple sequence repeats (ISSR) markers were used to assess the genetic fidelity of in vitro raised plants and the mother plant. It was revealed that monomorphic bands showing the absence of polymorphism in all in vitro raised plantlets analyzed, confirming the genetic uniformity among the regenerants. Phytochemical analysis was done to compare the antioxidant activities and HPLC fingerprinting assay of 80% aqueous ethanol extract of the leaves and stem of in vitro and in vivo grown C. obcordata. The extracts of the plants were examined for their antioxidant activities by using free radical 1, 1-diphenyl-2-picryl hydrazyl (DPPH) scavenging method, 2,2’-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical scavenging ability, reducing power capacity, estimation of total phenolic content, flavonoid content and flavonol content. A simplified method for the detection of ascorbic acid, phenolic acids and flavonoids content was also developed by using reversed phase high-performance liquid chromatography (HPLC). This is the first report on the micropropagation, genetic integrity study and quantitative phytochemical analysis of in vitro regenerated plants of C. obcordata.

Keywords: Cephalantheropsis obcordata, genetic fidelity, ISSR markers, HPLC

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

Abstract:

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

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

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Authors: Afifa Hafidh, Fathi Touati, Ahmed Hichem Hamzaoui, Sayda Somrani

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The objective of the present study has been to synthesize and to characterize silica hybrid materials using sol-gel technic and to investigate their properties. Silica materials were successfully fabricated using various bi-functional 1,3,4-thiadiazoles and tetraethoxysilane (TEOS) as co-precursors via a facile one-pot sol-gel pathway. TEOS was introduced at room temperature with 1,3,4-thiadiazole 2,5-difunctiunal adducts, in ethanol as solvent and using HCl acid as catalyst. The sol-gel process lead to the formation of monolithic, coloured and transparent gels. TEOS was used as a principal network forming agent. The incorporation of 1,3,4-thiadiazole molecules was realized by attachment of these later onto a silica matrix. This allowed covalent linkage between organic and inorganic phases and lead to the formation of Si-N and Si-S bonds. The prepared hybrid materials were characterized by Fourier transform infrared, NMR ²⁹Si and ¹³C, scanning electron microscopy and nitrogen absorption-desorption measurements. The optic and magnetic properties of hybrids are studied respectively by ultra violet-visible spectroscopy and electron paramagnetic resonance. It was shown in this work, that heterocyclic moieties were successfully attached in the hybrid skeleton. The formation of the Si-network composed of cyclic units (Q3 structures) connected by oxygen bridges (Q4 structures) was proved by ²⁹Si NMR spectroscopy. The Brunauer-Elmet-Teller nitrogen adsorption-desorption method shows that all the prepared xerogels have isotherms type IV and are mesoporous solids. The specific surface area and pore volume of these materials are important. The obtained results show that all materials are paramagnetic semiconductors. The data obtained by Nuclear magnetic resonance ²⁹Si and Fourier transform infrared spectroscopy, show that Si-OH and Si-NH groups existing in silica hybrids can participate in adsorption interactions. The obtained materials containing reactive centers could exhibit adsorption properties of metal ions due to the presence of OH and NH functionality in the mesoporous frame work. Our design of a simple method to prepare hybrid materials may give interest of the development of mesoporous hybrid systems and their use within the domain of environment in the future.

Keywords: hybrid materials, sol-gel process, 1, 3, 4-thiadaizole, TEOS

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Authors: Lucky Malise, Hilary Rutto, Tumisang Seodigeng

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Heavy metal contamination in waste water is a very serious issue affecting a lot of industrialized countries due to the health and environmental impact of these heavy metals on human life and the ecosystem. Adsorption using activated carbon is the most promising method for the removal of heavy metals from waste water but commercial activated carbon is expensive which gives rise to the need for alternatively activated carbon derived from cheap precursors, agricultural wastes, or byproducts from other processes. In this study activated bio-carbon derived from the carbonaceous material obtained from the pyrolysis of Marula nut shells was chemically activated and used as an adsorbent for the removal of lead (II) and copper (II) ions from aqueous solution. The surface morphology and chemistry of the adsorbent before and after chemical activation with zinc chloride impregnation were studied using SEM and FTIR analysis respectively and the results obtained indicate that chemical activation with zinc chloride improves the surface morphology of the adsorbent and enhances the intensity of the surface oxygen complexes on the surface of the adsorbent. The effect of process parameters such as adsorbent dosage, pH value of the solution, initial metal concentration, contact time, and temperature on the adsorption of lead (II) and copper (II) ions onto Marula nut activated carbon were investigated, and their optimum operating conditions were also determined. The experimental data was fitted to both the Langmuir and Freundlich isotherm models, and the data fitted best on the Freundlich isotherm model for both metal ions. The adsorption kinetics were also evaluated, and the experimental data fitted the pseudo-first order kinetic model better than the pseudo second-order kinetic model. The adsorption thermodynamics were also studied and the results indicate that the adsorption of lead and copper ions is spontaneous and exothermic in nature, feasible, and also involves a dissociative mechanism in the temperature range of 25-45 °C.

Keywords: adsorption, isotherms, kinetics, marula nut shells activated carbon, thermodynamics

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Authors: Yu-Wen Cheng, Jau-Der Ho, Liang-Huan Wu, Fan-Li Lin, Li-Huei Chen, Hung-Ming Chang, Yueh-Hsiung Kuo, George Hsiao

Abstract:

Retina glial activation and neuroinflammation have been confirmed to cause devastating responses in retinodegenerative diseases. The expression and activation of matrix metalloproteinase (MMP)-9 and inducible nitric oxide synthase (iNOS) could be exerted as the crucial pathological factors in glaucoma- and blue light-induced retinal injuries. The present study aimed to investigate the retinoprotective effects and mechanisms of fungal ingredient 3,4-dihydroxybenzalacetone (DBL) isolated from Phellinus linteus in the retinal glial activation and retinodegenerative animal models. According to the cellular studies, DBL significantly and concentration-dependently abrogated MMP-9 activation and expression in TNFα-stimulated retinal Müller (rMC-1) cells. We found the inhibitory activities of DBL were strongly through the STAT- and ERK-dependent pathways. Furthermore, DBL dramatically attenuated MMP-9 activation in the stimulated Müller cells exposed to conditioned media from LPS-stimulated microglia BV-2 cells. On the other hand, DBL strongly suppressed LPS-induced production of NO and ROS and expression of iNOS in microglia BV-2 cells. Consistently, the phosphorylation of STAT was substantially blocked by DBL in LPS-stimulated microglia BV-2 cells. In the evaluation of retinoprotective functions, the high IOP-induced scotopic electroretinographic (ERG) deficit and blue light-induced abnormal pupillary light response (PLR) were assessed. The deficit scotopic ERG responses markedly recovered by DBL in a rat model of glaucoma-like ischemia/reperfusion (I/R)-injury. DBL also reduced the aqueous gelatinolytic activity and retinal MMP-9 expression in high IOP-injured conditions. Additionally, DBL could restore the abnormal PLR and reduce retinal MMP-9 activation. In summary, DBL could ameliorate retinal neuroinflammation and MMP-9 activation by predominantly inhibiting STAT3 activation in the retinal Müller cells and microglia, which exhibits therapeutic potential for glaucoma and other retinal degenerative diseases.

Keywords: glaucoma, blue light, DBL, retinal Müller cell, MMP-9, STAT, Microglia, iNOS, ERG, PLR

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Authors: Alaa Hamed Salama, Rehab Nabil Shamma

Abstract:

Introduction: Polymeric micelles that can deliver drug to intended sites of the eye have attracted much scientific attention recently. The aim of this study was to review the aqueous-based formulation of drug-loaded polymeric micelles that hold significant promise for ophthalmic drug delivery. This study investigated the synergistic performance of mixed polymeric micelles made of linear and branched poly (ethylene oxide)-poly (propylene oxide) for the more effective encapsulation of Lornoxicam (LX) as a hydrophobic model drug. Methods: The co-micellization process of 10% binary systems combining different weight ratios of the highly hydrophilic poloxamers; Synperonic® PE/P84, and Synperonic® PE/F127 and the hydrophobic poloxamine counterpart (Tetronic® T701) was investigated by means of photon correlation spectroscopy and cloud point. The drug-loaded micelles were tested for their solubilizing capacity towards LX. Results: Results showed a sharp solubility increase from 0.46 mg/ml up to more than 4.34 mg/ml, representing about 136-fold increase. Optimized formulation was selected to achieve maximum drug solubilizing power and clarity with lowest possible particle size. The optimized formulation was characterized by 1HNMR analysis which revealed complete encapsulation of the drug within the micelles. Further investigations by histopathological and confocal laser studies revealed the non-irritant nature and good corneal penetrating power of the proposed nano-formulation. Conclusion: LX-loaded polymeric nanomicellar formulation was fabricated allowing easy application of the drug in the form of clear eye drops that do not cause blurred vision or discomfort, thus achieving high patient compliance.

Keywords: confocal laser scanning microscopy, Histopathological studies, Lornoxicam, micellar solubilization

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Authors: Mehrosadat Mirmohammadi, Sara Taghdisi, Ali Padash, Mohammad Hossein Pazandeh

Abstract:

Gossypol, a yellowish anti-nutritional compound found in cotton plants, exists in various plant parts, including seeds, husks, leaves, and stems. Chemically, gossypol is a potent polyphenolic aldehyde with antioxidant and therapeutic properties. However, its free form can be toxic, posing risks to both humans and animals. Initially, we extracted gossypol from cotton seeds using n-hexane as a solvent (yield: 84.0 ± 4.0%). We also obtained cotton seed and cotton boll extracts via Soxhlet extraction (25:75 hydroalcoholic ratio). These extracts, combined with cornstarch, formed four herbal medicinal formulations. Ethical approval allowed us to investigate their effects on Leishmania-caused skin wounds, comparing them to glucantime (local ampoule). Herbal formulas outperformed the control group (ethanol only) in wound treatment (p-value 0.05). The average wound diameter after two months did not significantly differ between plant extract ointments and topical glucantime. Notably, cotton boll extract with 1% extra gossypol crystal showed the best therapeutic effect. We extracted gossypol from cotton seeds using n-hexane via Soxhlet extraction. Saponification, acidification, and recrystallization steps followed. FTIR, UV-Vis, and HPLC analyses confirmed the product’s identity. Herbal medicines from cotton seeds effectively treated chronic wounds compared to the ethanol-only control group. Wound diameter differed significantly between extract ointments and glucantime injections. It seems that due to the presence of large amounts of fat in the oil, the extraction of gossypol from it faces many obstacles. The extraction of this compound with our technique showed that extraction from oil has a higher efficiency, perhaps because of the preparation of oil by cold pressing method, the possibility of losing this compound is much less than when extraction is done with Soxhlet. On the other hand, the gossypol in the oil is mostly bound to the protein, which somehow protects the gossypol until the last stage of the extraction process. Since this compound is very sensitive to light and heat, it was extracted as a derivative with acetic acid. Also, in the treatment section, it was found that the ointment prepared with the extract is more effective and Gossypol is one of the effective ingredients in the treatment. Therefore, gossypol can be extracted from the oil and added to the extract from which gossypol has been extracted to make an effective medicine with a certain dose.

Keywords: cottonseed, glucantime, gossypol, leishmaniasis

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Authors: Geevika J. Ganegama Arachchi, Steve H. Flint, Lynn McIntyre, Cristina D. Cruz, Beatrice M. Dias-Wanigasekera, Craig Billington, J. Andrew Hudson, Anthony N. Mutukumira

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In seafood processing plants, Listeriamonocytogenes(L. monocytogenes)likely exists in a metabolically stressed state due to the nutrient-deficient environment, processing treatments such as heating, curing, drying, and freezing, and exposure to detergents and disinfectants. Stressed L. monocytogenes cells have been shown to be as pathogenic as unstressed cells. This study investigated lytic efficacy of (LiMN4L, LiMN4p, and LiMN17) which were previouslycharacterized as virulent against physiologically stressed cells of three seafood borne L. monocytogenesstrains (19CO9, 19DO3, and 19EO3).Physiologically compromised cells ofL. monocytogenesstrains were prepared by aging cultures in TrypticaseSoy Broth at 15±1°C for 72 h; heat injuringcultures at 54±1 - 55±1°C for 40 - 60 min;salt-stressing cultures in Milli-Q water were incubated at 25±1°C in darkness for three weeks; and incubating cultures in 9% (w/v) NaCl at 15±1°C for 72 h. Low concentrations of physiologically compromised cells of three L. monocytogenesstrainswere challenged in vitrowith high titre of three phages in separate experiments using Fish Broth medium (aqueous fish extract) at 15 °C in order to mimic the environment of seafood processing plant. Each phage, when present at ≈9 log10 PFU/ml, reduced late exponential phase cells of L. monocytogenes suspended in fish protein broth at ≈2-3 log10 CFU/ml to a non-detectable level (< 10 CFU/ml). Each phage, when present at ≈8.5 log10 PFU/ml, reduced both heat-injured cells present at 2.5-3.6 log10 CFU/ml and starved cells that were showed coccoid shape, present at ≈2-3 log10 CFU/ml to < 10 CFU/ml after 30 min. Phages also reduced salt-stressed cellspresent at ≈3 log10 CFU/ml by > 2 log10. L. monocytogenes (≈8 log10 CFU/ml) were reduced to below the detection limit (1 CFU/ml) by the three successive phage infections over 16 h, indicating that emergence of spontaneous phage resistance was infrequent. The three virulent phages showed high decontamination potential for physiologically stressed L. monocytogenes strains from seafood processing environments.

Keywords: physiologically stressed L. monocytogenes, heat injured, seafood processing environment, virulent phage

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

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

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

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