Search results for: Solvent

Authors: F. Portet-Koltalo, Y. Tian, I. Berger, C. Boulanger-Lecomte, A. Benamar, N. Machour

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Sediments are complex environments which can accumulate a great variety of persistent toxic contaminants such as polychlorobiphenyles (PCBs), polycyclic aromatic hydrocarbons (PAHs) and some of their more toxic degradation metabolites such as hydroxylated PAHs (OH-PAHs). Owing to their composition, fine clayey sediments can be more difficult to extract than soils using conventional solvent extraction processes. So this study aimed to compare the potential of MSPD (matrix solid phase dispersive extraction) to extract PCBs, PAHs and OH-PAHs, in comparison with microwave assisted extraction (MAE). Methodologies: MAE extraction with various solvent mixtures was used to extract PCBs, PAHs and OH-PAHs from sediments in two runs, followed by two GC-MS analyses. MSPD consisted in crushing the dried sediment with dispersive agents, introducing the mixture in cartridges and eluting the target compounds with an appropriate volume of selected solvents. So MSPD combined with cartridges containing MIPs (molecularly imprinted polymers) designed for OH-PAHs was used to extract the three families of target compounds in only one run, followed by parallel analyses in GC-MS for PAHs/PCBs and HPLC-FLD for OH-PAHs. Results: MAE extraction was optimized to extract from clayey sediments, in two runs, PAHs/PCBs in one hand and OH-PAHs in the other hand. Indeed, the best conditions of extractions (mixtures of extracting solvents, temperature) were different if we consider the polarity and the thermodegradability of the different families of target contaminants: PAHs/PCBs were better extracted using an acetone/toluene 50/50 mixture at 130°C whereas OH-PAHs were better extracted using an acetonitrile/toluene 90/10 mixture at 100°C. Moreover, the two consecutive GC-MS analyses contributed to double the total analysis time. A matrix solid phase dispersive (MSPD) extraction procedure was also optimized, with the first objective of increasing the extraction recovery yields of PAHs and PCBs from fine-grained sediment. The crushing time (2-10 min), the nature of the dispersing agents added for purifying and increasing the extraction yields (Florisil, octadecylsilane, 3-chloropropyle, 4-benzylchloride), the nature and the volume of eluting solvents (methylene chloride, hexane, hexane/acetone…) were studied. It appeared that in the best conditions, MSPD was a better extraction method than MAE for PAHs and PCBs, with respectively, mean increases of 8.2% and 71%. This method was also faster, easier and less expensive. But the other advantage of MSPD was that it allowed to introduce easily, just after the first elution process of PAHs/PCBs, a step permitting the selective recovery of OH-PAHs. A cartridge containing MIPs designed for phenols was coupled to the cartridge containing the dispersed sediment, and various eluting solvents, different from those used for PAHs and PCBs, were tested to selectively concentrate and extract OH-PAHs. Thereafter OH-PAHs could be analyzed at the same time than PAHs and PCBs: the OH-PAH extract could be analyzed with HPLC-FLD, whereas the PAHs/PCBs extract was analyzed with GC-MS, adding only few minutes more to the total duration of the analytical process. Conclusion: MSPD associated to MIPs appeared to be an easy, fast and low expensive method, able to extract in one run a complex mixture of toxic apolar and more polar contaminants present in clayey fine-grained sediments, an environmental matrix which is generally difficult to analyze.

Keywords: contaminated fine-grained sediments, matrix solid phase dispersive extraction, microwave assisted extraction, molecularly imprinted polymers, multi-pollutant analysis

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Authors: Arash Esmaeili, Zhibang Liu, Yang Xiang, Jimmy Yun, Lei Shao

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A high pressure carbon dioxide (CO₂) absorption from a specific gas in a conventional column has been evaluated by the Aspen HYSYS simulator using a wide range of single absorbents and blended solutions to estimate the outlet CO₂ concentration, absorption efficiency and CO₂ loading to choose the most proper solution in terms of CO₂ capture for environmental concerns. The property package (Acid Gas-Chemical Solvent) which is compatible with all applied solutions for the simulation in this study, estimates the properties based on an electrolyte non-random two-liquid (E-NRTL) model for electrolyte thermodynamics and Peng-Robinson equation of state for the vapor and liquid hydrocarbon phases. Among all the investigated single amines as well as blended solutions, piperazine (PZ) and the mixture of piperazine and monoethanolamine (MEA) have been found as the most effective absorbents respectively for CO₂ absorption with high reactivity based on the simulated operational conditions.

Keywords: absorption, amine solutions, Aspen HYSYS, carbon dioxide, simulation

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Authors: Oscar Corredor, Alexander Guzman, Adan Leon

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Density is a bulk physical property that indicates the quality of a petroleum fraction. It is also a useful property to estimate various physicochemical properties of fraction and petroleum fluids; however, the determination of density of extra heavy residual (EHR) fractions by standard methodologies, (ASTM D70) shows limitations for samples with higher densities than 1.0879 g/cm3. For this reason, a dilution methodology was developed in order to determinate density for those particular fractions, 87 (EHR) fractions were obtained as products of the fractionation of Colombian typical Vacuum Distillation Residual Fractions using molecular distillation (MD) and extraction with Solvent N-hexane in Supercritical Conditions (SFEF) pilot plants. The proposed methodology showed reliable results that can be demonstrated with the standard deviation of repeatability and reproducibility values of 0.0031 and 0.0061 g/ml respectively. In the same way, it was possible to determine densities in fractions EHR up to 1.1647g/cm3 and °API values obtained were ten times less than the water reference value.

Keywords: API, density, vacuum residual, molecular distillation, supercritical fluid extraction

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Authors: Duchel Jeanedvi Kinouani Kinavouidi, Christian Aimé Kayath, Etienne Nguimbi

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Biosurfactants are amphipathic molecules produced by many microorganisms, usually bacteria, fungi, and yeasts. +ey possesses the property of reducing the tension of the membrane interfaces. No studies have been conducted on Shigella species showing the role of biosurfactant-like molecules (BLM) in pathogenicity. +e aim of this study is to assess the ability of Shigella environmental and clinical strains to produce BLM and investigate the involvement of biosurfactants in pathogenicity. Our study has shown that BLM is secreted in the extracellular medium with EI24 ranging from 80% to 100%. +e secretion depends on the type III secretion system (T3SS). Moreover, our results have shown that S. flexneri, S. boydii, and S. sonnei are able to interact with hydrophobic areas with 17.64%, 21.42%, and 22.22% hydrophobicity, respectively. BLM secretion is totally prevented due to the inhibition of T3SS by 100 mM benzoic and 1.5 mg/ml salicylic acids. P. aeruginosa harboring T3SS is able to produce 100% of BLM in the presence or in the absence of both T3SS inhibitors. +e secreted BLM are extractable with an organic solvent such as chloroform, and this could entirely be considered a lipopeptide or polypeptide compound. Secretion of BLM allows some Shigella strains to induce multicellular phenomena like ‘swarming.’

Keywords: shigella flexneri, biosurfactant, T3SS, Lipopeptide

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Authors: M. Michael Gromiha, A. Mary Thangakani, Sandeep Kumar, D. Velmurugan

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The main cause of several neurodegenerative diseases such as Alzhemier, Parkinson, and spongiform encephalopathies is formation of amyloid fibrils and plaques in proteins. We have analyzed different sets of proteins and peptides to understand the influence of sequence-based features on protein aggregation process. The comparison of 373 pairs of homologous mesophilic and thermophilic proteins showed that aggregation-prone regions (APRs) are present in both. But, the thermophilic protein monomers show greater ability to ‘stow away’ the APRs in their hydrophobic cores and protect them from solvent exposure. The comparison of amyloid forming and amorphous b-aggregating hexapeptides suggested distinct preferences for specific residues at the six positions as well as all possible combinations of nine residue pairs. The compositions of residues at different positions and residue pairs have been converted into energy potentials and utilized for distinguishing between amyloid forming and amorphous b-aggregating peptides. Our method could correctly identify the amyloid forming peptides at an accuracy of 95-100% in different datasets of peptides.

Keywords: aggregation, amyloids, thermophilic proteins, amino acid residues, machine learning techniques

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Authors: Kumalo F. I., Malimabe M. A., Gumede T. P., Mosoabisane M. F. T.

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This study investigates the fabrication and characterization of bio-nanocomposites consisting of poly (butylene succinate) (PBS) and poly (ԑ-caprolactone) (PCL), reinforced with cellulose extracted from Eucomis autumnalis, a medicinal plant. Bio-nanocomposite films were prepared using the solvent casting method, with cellulose content ranging from 1 to 3 wt%. During the solution casting method, 15 ml of chloroform was used to dissolve an overall mass of 0.5g of each polymer as well as the combination of their bio-nanocomposites. Comprehensive analysis was conducted using FTIR, SEM, TEM, DSC, TGA, and XRD to assess morphological, thermal, and structural properties. Mechanical properties were not investigated due to the thin nature of the films. The results indicated significant improvements in the thermal stability and morphological properties with increasing cellulose content, showcasing the potential of these materials for tissue engineering applications. The use of cellulose extracted from a medicinal plant highlights the potential for sustainable and biocompatible materials in biomedical applications.

Keywords: bio-nanocomposites, poly (butylene succinate), poly(ԑ-caprolactone), Eucomis autumnalis, medicinal plant

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Authors: Amira Shakila Razali, Faridah Lisa Supian, Muhammad Mat Salleh, Suriani Abu Bakar

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Water contamination by toxic compound is one of the serious environmental problems today. These toxic compounds mostly originated from industrial effluents, agriculture, natural sources and human waste. These study are focused on modification of multiwalled carbon nanotube (MWCNTs) with nanoparticle of calixarene and explore the possibility of using this nanocomposites for the remediation of cadmium in water. The nanocomposites were prepared by dissolving calixarene in chloroform solution as solvent, followed by additional multiwalled carbon nanotube (MWCNTs) then sonication process for 3 hour and fabricated the nanocomposites on substrate by spin coating method. Finally, the nanocomposites were tested on cadmium ion (10 mg/ml). The morphology of nanocomposites was investigated by FESEM showing the formation of calixarene on the outer walls of carbon nanotube and cadmium ion also clearly seen from the micrograph. This formation was supported by using energy dispersive x-ray (EDX). The presence of cadmium ions in the films, leads to some changes in the surface potential and Fourier Transform Infrared spectroscopy (FTIR).This nanocomposites have potential for development of sensor for pollutant monitoring and nanoelectronics devices applications

Keywords: calixarene, multiwalled carbon nanotubes, cadmium, surface potential

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Authors: Gloria M. Ntuba-Jua, Afui M. Mih, Eneke E. T. Bechem

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Prunus africana (Hook. F.) Kalkman, commonly known as Pygeum or African cherry belongs to the Rosaceae family. It is a medium to large, evergreen tree with a spreading crown of 10 to 20 m. It is used by the traditional medical practitioners for the treatment of over 45ailments in Cameroon and sub-Sahara Africa. In modern medicine, it is used in the treatment of benign prostrate hyperplasia (BPH), prostate gland hypertrophy (enlarged prostate glands). This is possible because of its ability to produce some secondary metabolites which are believed to have bioactivity against these ailments. The ready international market for the sale of Prunus bark, uncontrolled exploitation, illegal harvesting using inappropriate techniques and poor timing of harvesting have contributed enormously to making the plant endangered. It is known to harbor a large number of endophytic fungi with the potential to produce similar secondary metabolites as the parent plant. Alternative sourcing of medicinal principles through endophytic fungi requires succinct knowledge of the endophytic fungi. This will serve as a conservation measure for Prunus africana by reducing dependence on Prunus bark for such metabolites. This work thus sought to compare the production of some major secondary metabolites produced by P. africana and some of its associated endophytic fungi. The leaves and stem bark of the plant from different provenances were soaked in methanol for 72 hrs to yield the methanolic crude extract. The phytochemical screening of the methanolic crude extracts using different standard procedures revealed the presence of tannins, flavonoids, terpenoids, saponins, phenolics and steroids. Pure cultures of some predominantly isolated endophyte species from the difference Prunus provenances such as Curvularia sp, and Morphospecies P001 were also grown in Potato Dextrose Broth (PDB) for 21 days and later extracted with Methylene dichloride (MDC) solvent after 24hrs to produce crude culture extracts. Qualitative assessment of crude culture extracts showed the presence of tannins, terpenoids, phenolics and steroids particularly β-Sitosterol, (a major bioactive metabolite) as did the plant tissues. Qualitative analysis by thin layer chromatography (TLC) was done to confirm and compare the production of β-Sitosterol (as marker compounds) in the crude extracts of the plant and endophyte. Samples were loaded on TLC silica gel aluminium barked plate (Kieselgel 60 F254, 0.2 mm, Merck) using acetone/hexane, (3.0:7.0) solvent system. They were visualized under an ultra violet lamp (UV254 and UV360). TLC revealed that leaves had a higher concentration of β-sitosterol in terms of band intensity than stem barks from the different provenances. The intensity of β-sitosterol bands in the culture extracts of endophytes was comparable to the plant extracts except for Curvularia sp (very minute) whose band was very faint. The ability of these fungi to make β-sitosterol was confirmed by TLC analysis with the compound having chromatographic properties (retention factor) similar to those of β-sitosterol standard. The ability of these major endophytes to produce secondary metabolites similar to the host has therefore been demonstrated. There is, therefore, the potential of developing the in vitro production system of Prunus secondary metabolites thereby enhancing its conservation.

Keywords: Caneroon, endophytic fungi, Prunus africana, secondary metabolite

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Authors: Mahsa Kangazian Kangazi, Ali Akbar Ghareh Aghaji, Majid Montazer

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Nowadays, silica nanofibers are highly regarded among the inorganic nanofibers due to the high reactivity and availability of silicon compounds in nature. Sol-gel process is required for electrospinning of silica nanofibers in which a metal alkoxide is hydrolyzed, and the viscosity is increased. In this study, silica nanofibers containing silver nanoparticles were synthesized and electrospun from a mixture of silica sol with an easy spinnable polymer (PVA) as an additive. The silica sol contains tetraethyl orthosilicate (TEOS), silver nitrate, distilled water, nitric acid, and ethanol. Nanofibers were formed through electrospinning setup. The nanofibers were calcinated to remove the solvent and additive polymer. Consequently, pure silica nanofibers were produced. FTIR analysis indicated entire removal of polyvinyl alcohol from the structure and formation of silan groups. The presence of silver, silica and oxygen was confirmed by EDX. Also, XRD patterns revealed the presence of silver nanoparticles with a mean crystal size of 18 nm. FESEM images showed that adding silver nitrate into the sol-gel, resulted in lower nanofibers diameter from 286 to 136 nm. Furthermore, the electrospun nanofibers were more resistance in acidic media than alkaline media.

Keywords: in situ synthesis of silver nanoparticles, silica nanofibers, sol-gel, tetraethyl orthosilicate

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Authors: Rashad Al-Gaashani, Muataz A. Atieh

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In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

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Authors: H. Özkan Gülsoy, Antonyraj Arockiasamy

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The application of powder injection molding technology for the fabrication of metallic and non-metallic components is of growing interest as the process considerably saves time and cost. Utilizing this fabrication method, full dense components are being prepared in various sizes. In this work, our effort is focused to study the densification behavior of the parts made using different size 316L stainless steel powders. The metal powders were admixed with an adequate amount of polymeric compounds and molded as standard tensile bars. Solvent and thermal debinding was carried out followed by sintering in ultra pure hydrogen atmosphere based on the differential scanning calorimetry (DSC) cycle. Mechanical property evaluation and microstructural characterization of the sintered specimens was performed using universal Instron tensile testing machine, Vicker’s microhardness tester, optical (OM) and scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction were used. The results are compared and analyzed to predict the strength and weakness of the test conditions.

Keywords: powder injection molding, sintering, particle size, stainless steels

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Authors: Neda Sinaei, Davood Zare, Mehrdad Azin

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Polyhydroxyalkanoates (PHAs) are biocompatible and biodegradable polymers produced by a wide range of bacterial strains. These biopolymers are significantly studied for drug delivery and tissue engineering applications because of their fascinating physicochemical properties. Polyhydroxybutyrate (PHB) scaffold that has been extracted from a novel bacteria using oil wastewater was selected to study. Some physical parameters affecting scaffold properties such as PHB concentration, solvent evaporation speed, and ultrasonic time were investigated. Scanning electron microscopy was used to evaluate the porosity. Afterward, the biocompatibility of PHB scaffold was assessed. Initial results showed the highly porous PHB scaffold structure with a variety of pore sizes. Subsequent results indicated that more unique pore sizes can be obtained by optimizing physical factors. It would be noticed that the morphology of the pore structure was accordingly affected by ultrasonic time. Hence, In vitro cell viability tests on the PHB scaffold using human foreskin fibroblasts revealed strong cell attachment and proliferation supports. Therefore, it can be concluded that the cost-effective PHB scaffold has the potential using as a biomaterial cell adhesion substrate in therapeutic applications.

Keywords: Polyhydroxybutyrate, biocompatible, scaffold, porous, tissue engineering

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Authors: Samir Hmaimou, Marouane Ait Lahcen, Mohamed Adardour, Mohamed Maatallah, Abdesselam Baouid

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The stereoisomers (E)-2,2-dimethyl-4-(4-subsitutedstyryl)-2,3-dihydro-1H-[1,5]-benzodiazepine 3(a-d) were synthesized via the condensation reaction of 2,2,3 4-trimethyl-2,3-dihydro-1H-1,5-benzodiazepine (BZD) 1 with the benzaldehyde derivatives 2(a-d) in polar protic solvent as ethanol. The chemical structure of the prepared products was confirmed by NMR (¹H and ¹³C), HRMS, and X-ray analysis of the crystal structure 3d. The condensation reaction was examined using DFT calculations at the theoretical level of B3LYP/6-311G(d,p). Frontier molecular orbital analysis shows that the most favorable interaction is between the HOMO of BZD 1 and the LUMO of 2(a-d). On the other hand, the calculation of the global reactivity indices (softness, hardness, and chemical potential) confirmed that benzodiazepine BDZ 1 act as a nucleophile, whereas the aldehyde derivatives 2(a-d) play the role of electrophile. Furthermore, we identified each reagent's reactive sites by the measurement of the reactivity indices to explain the experimentally observed regioselectivity, using Fukui local reactivity descriptors. A one-step mechanism reaction and order 2 water elimination were investigated. We also looked at how the electron-withdrawing groups (EWG) of various aldehydes affected the reaction's mechanism and the stability of products 3(a-d).

Keywords: benzodiazepine, DFT calculations, crystal structure, regioselective, condensation Reaction

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Authors: Mostafa Rezaee Saraji, Ali Keshavarz Panahi

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In this work, the processing steps for producing alumina parts using powder injection molding (PIM) technique and nano-powder were investigated and the thermal conductivity and flexural strength of samples were determined as a function of sintering temperature and holding time. In the first step, the feedstock with 58 vol. % of alumina nano-powder with average particle size of 100nm was prepared using Extrumixing method to obtain appropriate homogeneity. This feedstock was injection molded into the two cavity mold with rectangular shape. After injection molding step, thermal and solvent debinding methods were used for debinding of molded samples and then these debinded samples were sintered in different sintering temperatures and holding times. From the results, it was found that the flexural strength and thermal conductivity of samples increased by increasing sintering temperature and holding time; in sintering temperature of 1600ºC and holding time of 5h, the flexural strength and thermal conductivity of sintered samples reached to maximum values of 488MPa and 40.8 W/mK, respectively.

Keywords: alumina nano-powder, thermal conductivity, flexural strength, powder injection molding

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Authors: Niharika Kaushal, Minni Singh

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Citrus fruits fall into the category of those commercially grown fruits that constitute an excellent repository of phytochemicals with health-promoting properties. Fruits belonging to the citrus family, when processed by industries, produce tons of agriculture by-products in the form of peels, pulp, and seeds, which normally have no further usage and are commonly discarded. In spite of this, such residues are of paramount importance due to their richness in valuable compounds; therefore, agro-waste is considered a valuable bioresource for various purposes in the food sector. A range of biological properties, including anti-oxidative, anti-cancerous, anti-inflammatory, anti-allergenicity, and anti-aging activity, have been reported for these bioactive compounds. Taking advantage of these inexpensive residual sources requires special attention to extract bioactive compounds. Mandarin (Citrus nobilis X Citrus deliciosa) is a potential source of bioflavonoids with antioxidant properties, and it is increasingly regarded as a functional food. Despite these benefits, flavonoids suffer from a barrier of pre-systemic metabolism in gastric fluid, which impedes their effectiveness. Therefore, colloidal delivery systems can completely overcome the barrier in question. This study involved the extraction and identification of key flavonoids from mandarin biomass. Using a green chemistry approach, supercritical fluid extraction at 330 bar, temperature 40C, and co-solvent 10% ethanol was employed for extraction, and the identification of flavonoids was made by mass spectrometry. As flavonoids are concerned with a limitation, the obtained extract was encapsulated in polylactic-co-glycolic acid (PLGA) matrix using a solvent evaporation method. Additionally, the antioxidant potential was evaluated by the 2,2-diphenylpicrylhydrazyl (DPPH) assay. A release pattern of flavonoids was observed over time using simulated gastrointestinal fluids. From the results, it was observed that the total flavonoids extracted from the mandarin biomass were estimated to be 47.3 ±1.06 mg/ml rutin equivalents as total flavonoids. In the extract, significantly, polymethoxyflavones (PMFs), tangeretin and nobiletin were identified, followed by hesperetin and naringin. The designed flavonoid-PLGA nanoparticles exhibited a particle size between 200-250nm. In addition, the bioengineered nanoparticles had a high entrapment efficiency of nearly 80.0% and maintained stability for more than a year. Flavonoid nanoparticles showed excellent antioxidant activity with an IC50 of 0.55μg/ml. Morphological studies revealed the smooth and spherical shape of nanoparticles as visualized by Field emission scanning electron microscopy (FE-SEM). Simulated gastrointestinal studies of free extract and nanoencapsulation revealed the degradation of nearly half of the flavonoids under harsh acidic conditions in the case of free extract. After encapsulation, flavonoids exhibited sustained release properties, suggesting that polymeric encapsulates are efficient carriers of flavonoids. Thus, such technology-driven and biomass-derived products form the basis for their use in the development of functional foods with improved therapeutic potential and antioxidant properties. As a result, citrus processing waste can be considered a new resource that has high value and can be used for promoting its utilization.

Keywords: citrus, agrowaste, flavonoids, nanoparticles

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Authors: Mochamad Chalid, Imam Prabowo

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The pollution due to non-degradable material such as plastics, has led to studies about the development of environmental-friendly material. Because of biodegradability obtained from natural sources, polylactid acid (PLA) and ijuk fiber are interesting to modify into a composite. This material is also expected to reduce the impact of environmental pollution. Surface modification of ijuk fiber through alkalinization with 0.25 M NaOH solution for 30 minutes, was aimed to enhance it’s compatibility to PLA, in order to improve properties of the composite such as the mechanical properties. Alkalinization of the ijuk fibers annihilates some surface components such as lignin, wax and hemicelloluse, so the pore on the surface clearly appeared, decreasing of the density and diameter of the ijuk fibers. The change of the ijuk fiber properties leads to increase the mechanical properties of PLA composites reinforced the ijuk fibers through strengthening of the mechanical interlocking with the PLA matrix. An addition to enhance the distribution of the fibers in the PLA matrix, the stirring during DCM solvent evaporation from the mixture of the ijuk fibers and the dissolved-PLA can reduce amount of the trapped-voids and fibers pull-out phenomena, which can decrease the mechanical properties of the composite.

Keywords: polylactic acid, Arenga pinnata, alkalinization, compatibility, adhesion, morphology, mechanical properties, volume fraction, distributiom

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Authors: Yousef Bakhbakhi

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Crystallization with supercritical fluids (SCFs), as a developed technology to produce particles of micron and sub-micron size with narrow size distribution, has found appreciable importance as an environmentally friendly technology. Particle synthesis using SCFs can be achieved employing a number of special processes involving solvent and antisolvent mechanisms. In this study, the compressed antisolvent (PCA) process is utilized as a model to analyze the theoretical complexity of crystallization with supercritical fluids. The population balance approach has proven to be an effectual technique to simulate and predict the particle size and size distribution. The nucleation and growth mechanisms of the particles formation in the PCA process is investigated using the population balance equation, which describes the evolution of the particle through coalescence and breakup levels with time. The employed mathematical population balance model contains a set of the partial differential equation with algebraic constraints, which demands a rigorous numerical approach. The combined Collocation and Galerkin finite element method are proposed as a high-resolution technique to solve the dynamics of the PCA process.

Keywords: particle formation, particle size and size distribution, PCA, supercritical carbon dioxide

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Authors: Ihsan Burak Cam, Ferhan Balci-Torun, Ayhan Topuz, Esin Ari, Ismail Gokhan Deniz, Ilker Genc

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The seeds of Vaccaria hispanica have been used in food and pharmaceutical industry. It is an important product due to its superior starch granules, triterpenic saponins, and cyclopeptides suitable for drug delivery. V. hispanica naturally grows in different climatic regions and has genotypes that differ in terms of seed content and composition. Sixty-six V. hispanica seed specimens were collected based on the representation of the distribution in all regions of Turkey and the determination of possible genotypic differences between regions. The seeds, collected from each of the 66 locations, were grown in greenhouse conditions in Akdeniz University, Antalya. Saponin and cyclopeptide contents of the V. hispanica seeds were determined after harvest. Accelerated solvent extraction (ASE) was applied for the extraction of saponins and cyclopeptides. Cyclopeptide (segetalin A) and saponin content of V. hispanica seeds were found in the range of 0.165-0.654 g/100 g and 0.15-1.14 g/100 g, respectively. The results were found to be promising for the seeds from Turkey in terms of saponin content and quality. Acknowledgment: This study was supported by the Scientific and Research Council of Turkey (TUBITAK) (project no 112 O 136).

Keywords: Vaccaria hispanica, saponin, cyclopeptid, cow cockle seeds

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Authors: Chandrashekar, R. T. Radhika, B. M. Venkatesha, S. Ananda, Shivalingegowda, T. S. Shashikumar, H. Ramachandra

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The kinetics of the oxidation of amitriptyline (AT) by sodium N-bromotoluene sulphonamide (C₆H₅SO₂NBrNa) has been studied in an acidic buffer medium of pH 1.2 at 303 K. The oxidation reaction of AT was followed spectrophotometrically at maximum wavelength, 410 nm. The reaction rate shows a first order dependence each on concentration of AT and concentration of sodium N-bromotoluene sulphonamide. The reaction also shows an inverse fractional order dependence at low or high concentration of HCl. The dielectric constant of the solvent shows negative effect on the rate of reaction. The addition of halide ions and the reduction product of BAT have no significant effect on the rate. The rate is unchanged with the variation in the ionic strength (NaClO₄) of the medium. Addition of reaction mixtures to be aqueous acrylamide solution did not initiate polymerization, indicating the absence of free radical species. The stoichiometry of the reaction was found to be 1:1 and oxidation product of AT is identified. The Michaelis-Menton type of kinetics has been proposed. The CH₃C₆H₅SO₂NHBr has been assumed to be the reactive oxidizing species. Thermodynamical parameters were computed by studying the reactions at different temperatures. A mechanism consistent with observed kinetics is presented.

Keywords: amitriptyline, bromamine-T, kinetics, oxidation

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Authors: Hassiba Bougueria, Nesrine Benarous, Souheyla Chetioui

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Azo dyes are one of the most widely used compounds in organic chemistry, primarily due to their relatively simple preparation methods. They have therefore been widely used, in particular as colorants for textiles, printing inks, cosmetics, and food additives. In addition to their use as dyes, azo compounds have attracted much attention from chemists as their potential applications are important in coordination chemistry, metal-organic frameworks (MOF) structures, COF (covalent-organic frameworks), and catalysis. Moreover, they have found many applications in different fields, such as nonlinear optics, optical storage, photoluminescence, and magnetism. The compound bis{(E)-1-[(2,4,6-tribromophenyl)diazenyl]naphthalen-2-olato}copper(II) dimethyl sulfoxide monosolvate, the CuII atom is tetracoordinate with a square-planar geometry, surrounded by two bidentate (E)-1-[(2,4,6-tribromophenyl)diazenyl]naphthalene-2-olate ligands via two N atoms and two O atoms. The O-Cu-O angles and N-Cu-N are of the order of 177.90(16)° and 177.8(2)°, respectively. The distances Cu-O and Cu- N are 1.892(4) Å and 1.976(4) Å, respectively. The cohesion of the crystal is ensured by hydrogen bonds of the C—H…O type and by π=π staking interactions [centroid–centroid distance = 3.679(4)Å]. The DMSO solvent molecule is disordered at two positions with occupancy rates of 0.70 and 0.30.

Keywords: azo dyes, DRX, structural characterization, biological activity

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Authors: Norsyamimi Hassim, Masturah Markom

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Supercritical fluid extraction (SFE) has been known as a sustainable and safe extraction technique for plant extraction due to the minimal usage of organic solvent. In this study, a scale-up process for the selected herbal plant (Phyllanthus niruri) was investigated by using supercritical carbon dioxide (SC-CO2) with food-grade (ethanol-water) cosolvent. The quantification of excess ethanol content in the final dry extracts was conducted to determine the safety of enriched extracts. The extraction yields obtained by scale-up SFE unit were not much different compared to the predicted extraction yields with an error of 2.92%. For component contents, the scale-up extracts showed comparable quality with laboratory-scale experiments. The final dry extract showed that the excess ethanol content was 1.56% g/g extract. The fish embryo toxicity test (FETT) on the zebrafish embryos showed no toxicity effects by the extract, where the LD50 value was found to be 505.71 µg/mL. Thus, it has been proven that SFE with food-grade cosolvent is a safe extraction technique for the production of bioactive compounds from P. niruri.

Keywords: scale-up, supercritical fluid extraction, enriched extract, toxicity, ethanol content

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Authors: Edgar Aguilar-Ortíz, Nicolas Lévaray, Mireille Vonlanthen, Eric G. Morales-Espinoza, Ernesto Rivera, Xiao Xia Zhu

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Four new star compounds bearing a porphyrin core and cholic acid units, (TPPh(Zn) tetra-CA, TPPh(2H) tetra-CA, TPPh(Zn) octa-CA and TPPh(2H) octa-CA), have been synthesized using the Click Chemistry approach, which consist on azide-alkyne couplings. These novel functionalized porphyrins were characterized by 1H and 13C NMR spectroscopy and their structure was confirmed by MALDI-TOF. The optical properties of these compounds were studied by absorption and fluorescence spectroscopy. On the other hand, order to evaluate the amphiphilic properties of the cholic acid units combined with the optical response of the porphyrin core, we performed absorption and fluorescence studies in function of the polarity of the environment. It was found that as soon as we increase the polarity of the solvent, the Zn-metallated porphyrins, (TPPh(Zn) tetra-CA and TPPh(Zn) octa-CA), are able to form J aggregates, whereas the free-base porphyrins, TPPh(2H) tetra-CA and TPPh(2H) octa-CA, behaved differently.

Keywords: aggregates, amphiphilic, cholic acid, click-chemistry, porphyrin

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Authors: Rasike De Silva, Xungai Wang, Nolene Byrne

Abstract:

We report on the blending of cotton and duck feather towards developing a new textile fibre. The cotton and duck feather were blended together by dissolving both components in an ionic liquid. Ionic liquids are designer solvents consisting entirely of ions with a melting point below 100˚C. Ionic liquids can be designed to have numerous and varied properties which include the ability to dissolve bio polymers. The dissolution of bio polymers such as cotton or wool generally requires very harsh acid or alkaline conditions and high temperatures. The ionic liquids which can dissolve bio polymers can be considered environmentally benign since they have negligible vapor pressure and can be recycled and reused. We have selected the cellulose dissolving and recyclable ionic liquid 1-allyl-3-methylimidazolium chloride (AMIMCl) as the dissolving and blending solvent for the cotton and duck feather materials. We have casted films and wet spun fibres at varying cotton and duck feather compositions and characterized the material properties of these. We find that the addition of duck feather enhances the elasticity of regenerated cotton. The strain% at breakage of the regenerated film was increased from 4.2% to 11.63% with a 10% duck feather loading, while the corresponding stress at breakage reduced from 54.89 MPa to 47.16 MPa.

Keywords: textile materials, bio polymers, ionic liquids, duck feather

Procedia PDF Downloads 479

Authors: N. R. Putra, A. H. Abdul Aziz, A. S. Zaini, Z. Idham, F. Idrus, M. Z. Bin Zullyadini, M. A. Che Yunus

Abstract:

The content of omega-3 in soybean oil is important in the development of infants and is an alternative for the omega-3 in fish oils. The investigation of extraction of soybean oil is needed to obtain the bioactive compound in the extract. Supercritical carbon dioxide extraction is modern and green technology to extract herbs and plants to obtain high quality extract due to high diffusivity and solubility of the solvent. The aim of this study was to obtain the optimum condition of soybean oil extraction by modified supercritical carbon dioxide. The soybean oil was extracted by using modified supercritical carbon dioxide (SC-CO₂) under the temperatures of 40, 60, 80 °C, pressures of 150, 250, 350 Bar, and constant flow-rate of 10 g/min as the parameters of extraction processes. An experimental design was performed in order to optimize three important parameters of SC-CO₂ extraction which are pressure (X₁), temperature (X₂) to achieve optimum yields of soybean oil. Box Behnken Design was applied for experimental design. From the optimization process, the optimum condition of extraction of soybean oil was obtained at pressure 338 Bar and temperature 80 °C with oil yield of 2.713 g. Effect of pressure is significant on the extraction of soybean oil by modified supercritical carbon dioxide. Increasing of pressure will increase the oil yield of soybean oil.

Keywords: soybean oil, SC-CO₂ extraction, yield, optimization

Procedia PDF Downloads 255

Authors: Boris M. Popović, Tatjana Jurić, Bojana Blagojević, Denis Uka, Ružica Ždero Pavlović

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Green solvents are environmentally friendly and greatly improve the sustainability of chemical processes. There is a growing interest in the green extraction of polyphenols from fruits. In this study, we consider three Natural Deep Eutectic Solvents (NADES) systems based on choline chloride as a hydrogen bond acceptor and malic acid, urea, and fructose as hydrogen bond donors. NADES systems were prepared by heating and stirring, ultrasound, and microwave (MW) methods. Sour cherry pomace was used as a natural source of polyphenols. Polyphenol extraction from cherry pomace was performed by ultrasound-assisted extraction and microwave-assisted extraction and compared with conventional heat and stirring method extraction. It was found that MW-assisted preparation of NADES was the fastest, requiring less than 30 s. Also, MW extraction of polyphenols was the most rapid, with less than 5 min necessary for the extract preparation. All three NADES systems were highly efficient for anthocyanin extraction, but the most efficient was the system with malic acid as a hydrogen bond donor (yield of anthocyanin content was enhanced by 62.33% after MW extraction with NADES compared with the conventional solvent).

Keywords: anthocyanins, green extraction, NADES, polyphenols

Procedia PDF Downloads 92

Authors: Naruphorn Dararatana, Farzad Seidi, Daniel Crespy

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Protection of metals is a critical issue in industry. The annual cost of corrosion in the world is estimated to be about 2.5 trillion dollars and continuously increases. Therefore, there is a need for developing novel protection approaches to improve corrosion protection. We designed and synthesized smart polymer/corrosion inhibitor conjugates as new generations of corrosion protecting materials. Firstly, a polymerizable acrylate derivative of 8-hydroxyquinoline (8HQ), an effective corrosion inhibitor, containing acid-labile β-thiopropionate linkage was prepared in three steps. Then, it was copolymerized with ethyl acrylate in the presence of 1,1′-azobis(cyclohexanecarbonitrile) (ABCN) by radical polymerization. Nanoparticles with an average diameter of 140 nm were prepared from the polymer conjugate by the miniemulsion-solvent evaporation process. The release behavior of 8HQ from the the nanoparticles was studied in acidic (pH 3.5) and neutral media (pH 7.0). The release profile showed a faster release of 8HQ in acidic medium in comparison with neutral medium. Indeed 100% of 8HQ was released after 14 days in acidic medium whereas only around 15% of 8HQ was released during the same period at neutral pH. Therefore, the polymer conjugate nanoparticles are suitable materials as additives or to form coatings on metal substrates for corrosion protection.

Keywords: Corrosion inhibitor, 8-Hydroxyquinoline, Polymer conjugated, β-Thiopropionate

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Authors: Rupan Das Chakraborty, Surendra K. Martha

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Hard carbons (HCs) are extensively used as anode materials for sodium-ion batteries due to their availability, low cost, and ease of synthesis. It possesses the ability to store Na ion between stacked sp2 carbon layers and micropores. In this work, hard carbons are synthesized from different concentrations (0.5M to 5M) of dextrose solutions by hydrothermal synthesis followed by high-temperature calcination at 1100 ⁰C in an inert atmosphere. Dextrose has been chosen as a precursor material as it is a eco-friendly and renewable source. Among all hard carbon derived from different concentrations of dextrose solutions, hard carbon derived from 3M dextrose solution delivers superior electrochemical performance compared to other hard carbons. Hard carbon derived from 3M dextrose solution (Dextrose derived Hard Carbon-3M) provides an initial reversible capacity of 257 mAh g-1 with a capacity retention of 83 % at the end of 100 cycles at 30 mA g-1). The carbons obtained from different dextrose concentration show very similar Cyclic Voltammetry and chargedischarging behavior at a scan rate of 0.05 mV s-1 the Cyclic Voltammetry curve indicate that solvent reduction and the solid electrolyte interface (SEI) formation start at E < 1.2 V (vs Na/Na+). Among all 3M dextrose derived electrode indicate as a promising anode material for Sodium-ion batteries (SIBs).

Keywords: dextrose derived hard carbon, anode, sodium-ion battery, electrochemical performance

Procedia PDF Downloads 118

Authors: A.Cifarelli, L. Boggioni, F. Bertini, L. Magon, M. Pitalieri, S. Losio

Abstract:

Nowadays, the growing environmental awareness and the dwindling of fossil resources stimulate the polyurethane (PU) industry towards renewable polymers with low carbon footprint to replace the feed stocks from petroleum sources. The main challenge in this field consists in replacing high-performance products from fossil-fuel with novel synthetic polymers derived from 'green monomers'. The bio-polyols from plant oils have attracted significant industrial interest and major attention in scientific research due to their availability and biodegradability. Triglycerides rich in unsaturated fatty acids, such as soybean oil (SBO) and linseed oil (ELO), are particularly interesting because their structures and functionalities are tunable by chemical modification in order to obtain polymeric materials with expected final properties. Unfortunately, their use is still limited for processing or performance problems because a high functionality, as well as OH number of the polyols will result in an increase in cross-linking densities of the resulting PUs. The main aim of this study is to evaluate soy and linseed-based polyols as precursors to prepare prepolymers for the production of polyurethane foams (PUFs) or waterborne-polyurethanes (WPU) used as coatings. An effective reaction route is employed for its simplicity and economic impact. Indeed, bio-polyols were synthesized by a two-step method: epoxidation of the double bonds in vegetable oils and solvent-free ring-opening reaction of the oxirane with organic acids. No organic solvents have been used. Acids with different moieties (aliphatic or aromatics) and different length of hydrocarbon backbones can be used to customize polyols with different functionalities. The ring-opening reaction requires a fine tuning of the experimental conditions (time, temperature, molar ratio of carboxylic acid and epoxy group) to control the acidity value of end-product as well as the amount of residual starting materials. Besides, a Lewis base catalyst is used to favor the ring opening reaction of internal epoxy groups of the epoxidized oil and minimize the formation of cross-linked structures in order to achieve less viscous and more processable polyols with narrower polydispersity indices (molecular weight lower than 2000 g/mol⁻¹). The functionality of optimized polyols is tuned from 2 to 4 per molecule. The obtained polyols are characterized by means of GPC, NMR (¹H, ¹³C) and FT-IR spectroscopy to evaluate molecular masses, molecular mass distributions, microstructures and linkage pathways. Several polyurethane foams have been prepared by prepolymer method blending conventional synthetic polyols with new bio-polyols from soybean and linseed oils without using organic solvents. The compatibility of such bio-polyols with commercial polyols and diisocyanates is demonstrated. The influence of the bio-polyols on the foam morphology (cellular structure, interconnectivity), density, mechanical and thermal properties has been studied. Moreover, bio-based WPUs have been synthesized by well-established processing technology. In this synthesis, a portion of commercial polyols is substituted by the new bio-polyols and the properties of the coatings on leather substrates have been evaluated to determine coating hardness, abrasion resistance, impact resistance, gloss, chemical resistance, flammability, durability, and adhesive strength.

Keywords: bio-polyols, polyurethane foams, solvent free synthesis, waterborne-polyurethanes

Procedia PDF Downloads 129

Authors: Sivakumar Singaravelu, Giriprasath Ramanathan, M. D. Raja, Uma Tirichurapalli Sivagnanam

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The goal of the present study was to develop and evaluate composite film for tissue engineering application. The keratin was extracted from bovine horn and used for preparation of keratin (HK), physiologically clotted fibrin (PCF) and gelatin (G) blend films in different stoichiometric ratios (1:1:1, 1:1:2 and 1:1:3) by using solvent casting method. The composite films (HK-PCF-G) were characterized physiochemically using Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM). The mechanical properties of the composite films were analyzed. The results of tensile strength show that ultimate strength and elongation were 10.72 Mpa and 4.83 MPA respectively for 1:1:3 ratio combination. The SEM image showed a slight smooth surface for 1:1:3 ratio combination compared to other films. In order to impart antibacterial activities, the composite films were loaded with Mupirocin (MP) to act against infection. The composite films acted as a suitable carrier to protect and release the drug in a controlled manner. This developed composite film would be a suitable alternative material for tissue engineering application.

Keywords: bovine horn, keratin, fibrin, gelatin, tensile strength

Procedia PDF Downloads 449

Authors: M. E. Abalaka, S. Y. Daniyan, S. O. Adeyemo, D. Damisa

Abstract:

Gold nanoparticles (AuNPs) have gained increasing interest in recent times. This is greatly due to their special features, which include unusual optical and electronic properties, high stability and biological compatibility, controllable morphology and size dispersion, and easy surface functionalization. In typical synthesis, AuNPs were produced by reduction of gold salt AuCl4 in an appropriate solvent. A stabilizing agent was added to prevent the particles from aggregating. The antibacterial activity of different sizes of gold nanoparticles was investigated against Staphylococcus aureus, Salmonella typhi and Pseudomonas pneumonia using the disk diffusion method in a Müeller–Hinton Agar. The Au-NPs were effective against all bacteria tested. That the Au-NPs were successfully synthesized in suspension and were used to study the antibacterial activity of the two medicinal plants against some bacterial pathogens suggests that Au-NPs can be employed as an effective bacteria inhibitor and may be an effective tool in medical field. The study clearly showed that the Au-NPs exhibiting inhibition towards the tested pathogenic bacteria in vitro could have the same effects in vivo and thus may be useful in the medical field if well researched into.

Keywords: gold nanoparticles, Gomphrena celesioides, Prunus amygdalus, pathogens

Procedia PDF Downloads 311