Search results for: emulsion solvent evaporation

Authors: Lucia Steenkamp, Chris V. D. Westhuyzen, Kgama Mathiba

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Ambergris, and more specifically its oxidation product (–)-ambrafuran, is a scarce, valuable, and sought-after perfumery ingredient. The material is used as a fixative agent to stabilise perfumes in formulations by reducing the evaporation rate of volatile substances. Ambergris is a metabolic product of the sperm whale (Physeter macrocephatus L.), resulting from intestinal irritation. Chemically, (–)-ambrafuran is produced from the natural product sclareol in eight synthetic steps – in the process using harsh and often toxic chemicals to do so. An overall yield of no more than 76% can be achieved in some routes, but generally, this is lower. A new 'green' route has been developed in our laboratory in which sclareol, extracted from the Clary sage plant, is converted to (–)-ambrafuran in two steps with an overall yield in excess of 80%. The first step uses a microorganism, Hyphozyma roseoniger, to bioconvert sclareol to an intermediate diol using substrate concentrations up to 50g/L. The yield varies between 90 and 67% depending on the substrate concentration used. The purity of the diol product is 95%, and the diol is used without further purification in the next step. The intermediate diol is then cyclodehydrated to the final product (–)-ambrafuran using a zeolite, which is not harmful to the environment and is readily recycled. The yield of the product is 96%, and following a single recrystallization, the purity of the product is > 99.5%. A preliminary LC-MS study of the bioconversion identified several intermediates produced in the fermentation broth under oxygen-restricted conditions. Initially, a short-lived ketone is produced in equilibrium with a more stable pyranol, a key intermediate in the process. The latter is oxidised under Norrish type I cleavage conditions to yield an acetate, which is hydrolysed either chemically or under lipase action to afford the primary fermentation product, an intermediate diol. All the intermediates identified point to the likely CYP450 action as the key enzyme(s) in the mechanism. This invention is an exceptional example of how the power of biocatalysis, combined with a mild, benign chemical step, can be deployed to replace a total chemical synthesis of a specific chiral antipode of a commercially relevant material.

Keywords: ambrafuran, biocatalysis, fragrance, microorganism

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Authors: Wai Keng Teng, Gek Cheng Ngoh, Rozita Yusoff, Mohamed Kheireddine Aroua

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As a by-product of the biodiesel industries, glycerol has been vastly generated which surpasses the market demand. It is imperative to develop an efficient glycerol valorization processes in minimizing the net energy requirement and intensifying the biodiesel production. In this study, base-catalyzed transesterification of glycerol with dimethyl carbonate using microwave irradiation as heating method to produce glycerol carbonate was conducted by varing grades of glycerol i.e. 70%, 86% and 99% purity that obtained from biodiesel plant. Metal oxide catalysts were used with varying operating parameters including reaction time, DMC/glycerol molar ratio, catalyst weight %, temperature and stirring speed. From the study on the effect of different operating parameters; it was found that the type of catalyst used has the most significant effect on the transesterification reaction. Admist the metal oxide catalysts examined, CaO gave the best performance. This study indicates the feasibility of producing glycerol carbonate using different grade of glycerol in both conventional thermal activation and microwave irradiation with CaO as catalyst. Microwave assisted transesterification (MAT) of glycerol into glycerol carbonate has demostrated itself as an energy efficient route by achieving 94.3% yield of GC at 65°C, 5 minutes reaction time, 1 wt% CaO and DMC/glycerol molar ratio of 2. The advantages of MAT transesterification route has made the direct utilization of bioglycerol from biodiesel production without the need of purification. This has marked a more economical and less-energy intensive glycerol carbonate synthesis route.

Keywords: base-catalyzed transesterification, glycerol, glycerol carbonate, microwave irradiation

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Authors: Anjana Jain, S. Jayanth Kumar

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Polyvinylidene fluoride (PVDF) is a well-known material for remarkable mechanical properties, resistance to chemicals and superior ferroelectric performances. This endows PVDF the potential for application in supercapacitor devices. The dielectric properties of PVDF, however, are not very high. To improve the dielectric properties of Polyvinylidene fluoride (PVDF), Piezoelectric polymer nanocomposites are prepared without affecting the other useful properties of PVDF. Polyaniline (PANI) was chosen as a filler material to prepare the nanocomposites. PVDF-PANI nanocomposite films were prepared using solvent cast method with different volume fractions of PANI varying from 0.04% to 0.048% of PANI content. The films are characterized for structural, mechanical, and surface morphological properties using X-ray diffraction, differential scanning calorimeter, Raman spectra, Infrared spectra, tensile testing, and scanning electron microscopy. The X-ray diffraction analysis shows that, prepared films were in β-phase. The DSC scans indicated that the degree of crystallinity in PVDF-PANI is improved. Raman and Infrared spectrum further confirm the presence of β-phase of PVDF-PANI film. Tensile properties of PVDF-PANI films were in good agreement with those reported in literature. The surface feature shows that PANI is uniformly distributed in PVDF and also results in disappearance of spherulites. The influence of volume fraction of PANI in PVDF on dielectric properties was analyzed. The results showed that the dielectric permittivity of PVDF-PANI (120) was much higher than that of PVDF (12). The sensitivity of these films was studied on application of a pressure and a constant output voltage was obtained.

Keywords: dielectric Properties, PANI, PVDF, smart materials

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Authors: Eriko Ochiai, Fumiko Satoh, Keiko Miyashita, Yu Kakimoto, Motoki Osawa

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Sudden and unexpected deaths from unknown causes occur in infants and youths. Recently, molecular links between a part of these deaths and several genetic diseases are examined in the postmortem. For instance, hereditary long QT syndrome and Burgada syndrome are occasionally fatal through critical ventricular tachyarrhythmia. There are a large number of target genes responsible for such diseases, the conventional analysis using the Sanger’s method has been laborious. In this report, we attempted to analyze sudden deaths comprehensively using the next generation sequencing (NGS) technique. Multiplex PCR to subject’s DNA was performed using Ion AmpliSeq Library Kits 2.0 and Ion AmpliSeq Inherited Disease Panel (Life Technologies). After the library was constructed by emulsion PCR, the amplicons were sequenced 500 flows on Ion Personal Genome Machine System (Life Technologies) according to the manufacture instruction. SNPs and indels were analyzed to the sequence reads that were mapped on hg19 of reference sequences. This project has been approved by the ethical committee of Tokai University School of Medicine. As a representative case, the molecular analysis to a 40 years old male who received a diagnosis of Brugada syndrome demonstrated a total of 584 SNPs or indels. Non-synonymous and frameshift nucleotide substitutions were selected in the coding region of heart disease related genes of ANK2, AKAP9, CACNA1C, DSC2, KCNQ1, MYLK, SCN1B, and STARD3. In particular, c.629T-C transition in exon 3 of the SCN1B gene, resulting in a leu210-to-pro (L210P) substitution is predicted “damaging” by the SIFT program. Because the mutation has not been reported, it was unclear if the substitution was pathogenic. Sudden death that failed in determining the cause of death constitutes one of the most important unsolved subjects in forensic pathology. The Ion AmpliSeq Inherited Disease Panel can amplify the exons of 328 genes at one time. We realized the difficulty in selection of the true source from a number of candidates, but postmortem genetic testing using NGS analysis deserves of a diagnostic to date. We now extend this analysis to SIDS suspected subjects and young sudden death victims.

Keywords: postmortem genetic testing, sudden death, SIDS, next generation sequencing

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Authors: Singh Baljinder, Sharma Navneet

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Foeniculum vulgare Miller is a biennial medicinal and aromatic plant belonging to the family Apiaceae (Umbelliferaceae). It is a hardy, perennial–umbelliferous herb with yellow flowers and feathery leaves. The aim is to study the control of blood glucose in alloxan induced diabetic mice.Method used for extraction was continuous hot percolation method in which Soxhlet apparatus was used.95%ethanol was used as solvent. Male albino mice weighing about 20-25 g obtained from Guru Angad Dev University of Veterinary Science, Ludhiana were used for the study. Diabetes was induced by a single i.p. injection of 125 mg/kg of alloxan monohydrate in sterile saline (11). After 48 h, animals with serum glucose level above 200 mg/dl (diabetic) were selected for the study. Blood samples from mice were collected by retro-orbital puncture (ROP) technique. Serum glucose levels were determined by glucose oxidase and peroxidase method. Single administration (single dose) of aqueous extract of fennel (25, 50, and 100 mg/kg, p.o.) in diabetic Swiss albino mice, showed reduction in serum glucose level after 45 min. Maximum reduction in serum glucose level was seen at doses of 100 mg/kg. Aqueous extract of fennel in all doses except 25 mg/kg did not cause any significant decrease in blood glucose. It may be said that the aqueous extract of fennel decreased the serum glucose level and improved glucose tolerance owing to the presence of aldehyde moiety. The aqueous extract of fennel has antihyperglycemic activity as it lowers serum glucose level in diabetic mice.

Keywords: Foeniculum vulgare Miller, antihyperglycemic, diabetic mice, Umbelliferaceae

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Authors: Cristian Soitu, Alexander Feuerborn, Cyril Deroy, Alfonso Castrejon-Pita, Peter R. Cook, Edmond J. Walsh

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Microfluidics now stands as an academically mature technology after a quarter of a century research activities have delivered a vast array of proof of concepts for many biological workflows. However, translation to industry remains poor, with only a handful of notable exceptions – e.g. digital PCR, DNA sequencing – mainly because of biocompatibility issues, limited range of readouts supported or complex operation required. This technology exploits the domination of interfacial forces over gravitational ones at the microscale, replacing solid walls with fluid ones as building blocks for cell micro-environments. By employing only materials used by biologists for decades, the system is shown to be biocompatible, and easy to manufacture and operate. The method consists in displacing a continuous fluid layer into a pattern of isolated chambers overlaid with an immiscible liquid to prevent evaporation. The resulting fluid arrangements can be arrays of micro-chambers with rectangular footprint, which use the maximum surface area available, or structures with irregular patterns. Pliant, self-healing fluid walls confine volumes as small as 1 nl. Such fluidic structures can be reconfigured during the assays, giving the platform an unprecedented level of flexibility. Common workflows in cell biology are demonstrated – e.g. cell growth and retrieval, cloning, cryopreservation, fixation and immunolabeling, CRISPR-Cas9 gene editing, and proof-of-concept drug tests. This fluid-shaping technology is shown to have potential for high-throughput cell- and organism-based assays. The ability to make and reconfigure on-demand microfluidic circuits on standard Petri dishes should find many applications in biology, and yield more relevant phenotypic and genotypic responses when compared to standard microfluidic assays.

Keywords: fluid walls, micro-chambers, reconfigurable, freestyle

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Authors: Sachin Latiyan, T. S. Sampath Kumar, Mukesh Doble

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Natural polymer based nanofibrous wound dressings have gained increased attention because of their high surface area, bioactivity, biodegradability and resemblance to extracellular matrix. Agarose (a natural polymer) have been used largely for angiogenesis, cartilage formation and wound healing applications. However, electrospinning of agarose is tedious thereby rendering limited studies on fabrication and evaluation of agarose based nanofibrous wound dressings. Thus, present study focuses on the fabrication of agarose (10% w/v)/ polyvinyl alcohol (12% w/v) based multifunctional nanofibrous scaffolds. Zinc citrate (1, 3 and 5% w/w of the polymer) was added as a potential antibacterial agent to combat wound infections. The fabricated scaffolds exhibit ~500% swelling (in phosphate buffer saline) with enhanced mechanical strength which is suitable for most of the wound healing applications. In vitro studies were found to reveal an increased migration and proliferation of L929 mouse fibroblasts with agarose blends w.r.t to the control. The fabricated dressings were found to be effective against both Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive) bacterial strains. Hence, a multifunctional (as provides effective swelling and mechanical support along with antibacterial property), natural product based, eco-friendly scaffold was successfully fabricated to serve as a potential wound dressing material.

Keywords: antibacterial dressings, benign solvent, nanofibrous agarose, biocompatibility, enhanced swelling and mechanical strength, biopolymeric dressings

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Authors: Tanveer Iqbal, Saima Yasin, Muhammad Zafar, Ahmad Shakeel, Fahad Nazir, Paul F. Luckham

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The contact performance of polymeric composites is dependent on the localized mechanical properties of materials. This is particularly important for fiber oriented polymeric materials where self-lubrication from top layers has been the basic requirement. The nanoindentation response of fiber reinforced poly(etheretherketone), PEEK, composites have been evaluated to determine the near-surface mechanical characteristics. Load-displacement compliance, hardness and elastic modulus data based on contact compliance mode (CSM) indentation of carbon fiber oriented and glass fiber oriented PEEK composites are reported as a function of indentation contact displacement. The composite surfaces were indented to a maximum penetration depth of 5µm using Berkovich tip indenter. A typical multiphase response of the composite surface is depicted from analysis of the indentation data for the composites, showing presence of polymer matrix, fibers, and interphase regions. The observed experimental results show that although the surface mechanical properties of carbon fiber based PEEK composite were comparatively higher, the properties of matrix material were seen to be increased in the presence of glass fibers. The experimental methodology may provide a convenient means to understand morphological description of the multimodal polymeric composites.

Keywords: nanoindentation, PEEK, modulus, hardness, plasticization

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

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

Keywords: naftopidil, HPTLC, validation, stability, degradation

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Authors: Sara Torabi, Sadegh Khazalpour, Mahdi Jamshidi

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

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

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Authors: Shaya Mahmoudian, Mohammad Reza Sazegar, Nazanin Afshari

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

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

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Authors: Qasar Saleem

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The aim of this project was to synthesize and analyze Polylactic acid-grafted TiO2 nanocomposite. When dispersed at the nanoscale TiO2 can behave as see through transparent UV filters and thermomechanical materials. The synthesis plan involved three stages. First, dispersion of TiO2 white powder in water/ethanol solvent system. Second grafting TiO2 surface by oligomers of lactic acid aimed at changing its surface features. Third polymerization of lactic acid monomer with grafted TiO2 in the presence of anhydrous stannous chloride as a catalyst. Polylactic acid grafted-TiO2 nanocomposite was synthesized by melt polycondensation in situ of lactic acid onto titanium oxide (TiO2) nanoparticles surface. The product was characterized by TGA, DSC, FTIR, and UV analysis and degradation observation. An idea regarding bonds between the grafting polymer and surface modified titanium oxide nanoparticles. Characteristics peaks of Ti–carbonyl bond, the related intensities of the Fourier transmission absorption peaks of graft composite, the melt and decomposition behavior stages of Polylactic acid-grafted TiO2 nanocomposite convinced that oligomers of polylactic acid were chemically bonded on the surface of TiO2 nanoparticles. Through grafting polylactic acid, the Polylactic acid grafted -TiO2 sample shown good absorption in UV region and degradation behavior under normal atmospheric conditions. Regaining transparency of degraded white opaque Polylactic acid-grafted TiO2 nanocomposite on heating was another character. Polylactic acid-grafted TiO2 nanocomposite will be a potential candidate in future for biomedical, UV shielding and environment friendly material.

Keywords: condensation, nanocomposites, oligomers, polylactic

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Authors: J. K. D. M. P. Madara, R. B. L. Dharmawickreme, Linu John, Ivee Boiss

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Flemingia vestita, commonly known as ‘Sohphlang’ is an important medicinal plant found in the North-Eastern region of India, which is traditionally recognized for its anthelmintic properties. This study was aimed to evaluate the phytochemical constituents and antibacterial activity of the tuber skin extracts of the plant species. Methanol, acetone, and water were used to obtain the solvent extractions of the skin peel extracts. Concentrated extracts of skin peel were tested using previously established qualitative phytochemical assays. The antibacterial efficacy of methanol tuber skin extract was tested against Gram-negative and positive microorganisms, namely, Klebsiella pneumonia, Escherichia coli, Pseudomonas aeruginosa, Bacillus subtilis, and Mycobacterium tuberculosis strains. Agar well diffusion method was employed to determine the zone of inhibition of the plant extracts. Obtained data were statistically analyzed. Methanol extracts of Flemingia vestita were found to be effective against Bacillus subtilis and Mycobacterium tuberculosis at concentrations of 0.5 mg/ml. The reported zone of inhibition for the two strains was 13.3mm ± 0.57 and 16.3mm ± 4.9, respectively. However Klebsiella pneumoniae, Pseudomonas aeruginosa and Escherichia coli were resistant to the plant extracts with no zone of inhibition. Alkaloids, glycosides, and phenols were found to be present in aqueous, methanol, and acetone extracts of the plant in qualitative phytochemical analysis.

Keywords: flemingia vestita, antibacterial activity, phytochemical screening, well diffusion method

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Authors: Tamseela Habib, Muhammad Amjad, Muhammad Edokali, Masome Moeni, Olivia Pickup, Ali Hassanpour

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Nanofluid-assisted steam generation is rapidly attracting attention amongst the scientific community since it can be applied in a wide range of industrial processes. Because of its high absorption rate of solar energy, nanoparticle-based solar steam generation could be a major contributor to many applications, including water desalination, sterilization and power generation. Lithium bromide-based iron oxide nanofluids have been previously studied in steam generation, which showed promising results. However, the efficiency of the system could be improved if a more heat-conductive nanofluid system could be utilised. In the current paper, we report on an experimental investigation of the photothermal conversion properties of functionalised Copper oxide (CuO) nanoparticles used in Lithium Bromide salt solutions. CuO binary nanofluid was prepared by chemical functionalization with polyethyleneimine (PEI). Long-term stability evaluation of prepared binary nanofluid was done by a high-speed centrifuge analyser which showed a 0.06 Instability index suggesting low agglomeration and sedimentation tendencies. This stability is also supported by the measurements from dynamic light scattering (DLS), transmission electron microscope (TEM), and ultraviolet-visible (UV-Vis) spectrophotometer. The fluid rheology is also characterised, which suggests the system exhibits a Newtonian fluid behavior. The photothermal conversion efficiency of different concentrations of CuO was experimentally investigated under a solar simulator. Experimental results reveal that the binary nanofluid in this study can remarkably increase the solar energy trapping efficiency and evaporation rate as compared to conventional fluids due to localized solar energy harvesting by the surface of the nanofluid. It was found that 0.1wt% CuO NP is the optimum nanofluid concentration for enhanced sensible and latent heat efficiencies.

Keywords: nanofluids, vapor absorption refrigeration system, steam generation, high salinity

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Authors: Amina Merghad, Cherif Abdennour

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Solvents are widely used in paint industry, where humans are highly exposed, especially from inhalation. A case report describes how paint affects reproductive markers and the health of workers. Sixty four subjects were chosen and divided into two groups; a control and an exposed group. A questionnaire was given to male workers from similar socio-economic status in order to know their ages, working conditions, clinical symptoms, working period, smoking history, shift, medical history and nutrition. Blood was withdrawn in the morning from volunteers. The measurement of blood testosterone and prolactin concentrations was then carried out. Results showed that the ages of the two groups were almost similar and were up to 47 and 43 years. The period of employment was 17 years and 14 years for the control and the exposed workers, respectively. Concerning clinical symptoms, the frequency of neuropsychological symptoms of the two groups are presented. It is clear that the symptom of memory loss, headaches are the highest among exposed workers followed by poor coordination, poor concentration and insomnia. On the other hand, the symptoms’ frequency in the control was less than that of the exposed group. Testosterone concentration has significantly decreased in group 2 (4.61±2,005 ng/ml) and group 3 (4.25±1.67 ng/ml) of exposed workers. On the other hand, prolactin concentration was higher in group 3 compared to other groups. To conclude, paint industry has disturbed reproductive markers and created high frequency of neuropsychological symptoms.

Keywords: blood, paint, prolactin, occupational exposure, organic solvent, reproductive toxicity, testosterone

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Authors: Sanjay Kumar, Dinesh Pathak, Sudhir Saralch

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Copper oxide is a semiconductor that has been studied for several reasons such as the natural abundance of starting material copper (Cu); the easiness of production by Cu oxidation; their non-toxic nature and the reasonably good electrical and optical properties. Copper oxide is well-known as cuprite oxide. The cuprite is p-type semiconductors having band gap energy of 1.21 to 1.51 eV. As a p-type semiconductor, conduction arises from the presence of holes in the valence band (VB) due to doping/annealing. CuO is attractive as a selective solar absorber since it has high solar absorbency and a low thermal emittance. CuO is very promising candidate for solar cell applications as it is a suitable material for photovoltaic energy conversion. It has been demonstrated that the dip technique can be used to deposit CuO films in a simple manner using metallic chlorides (CuCl₂.2H₂O) as a starting material. Copper oxide films are prepared using a methanolic solution of cupric chloride (CuCl₂.2H₂O) at three baking temperatures. We made three samples, after heating which converts to black colour. XRD data confirm that the films are of CuO phases at a particular temperature. The optical band gap of the CuO films calculated from optical absorption measurements is 1.90 eV which is quite comparable to the reported value. Dip technique is a very simple and low-cost method, which requires no sophisticated specialized setup. Coating of the substrate with a large surface area can be easily obtained by this technique compared to that in physical evaporation techniques and spray pyrolysis. Another advantage of the dip technique is that it is very easy to coat both sides of the substrate instead of only one and to deposit otherwise inaccessible surfaces. This method is well suited for applying coating on the inner and outer surfaces of tubes of various diameters and shapes. The main advantage of the dip coating method lies in the fact that it is possible to deposit a variety of layers having good homogeneity and mechanical and chemical stability with a very simple setup. In this paper, the CuO thin films preparation by dip coating method and their characterization will be presented.

Keywords: absorber material, cupric oxide, dip coating, thin film

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Authors: Maninderjeet K. Grewal, Sakshi Bhatnor, Renu Chadha

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The composition of pharmaceutical entities and the molecular interactions can be altered to optimize drug properties such as solubility and bioavailability by the crystal engineering technique. The present work has emphasized on the preparation, characterization, and biopharmaceutical evaluation of co-crystal of BCS Class II anti-osteoarthritis drug, Oxaprozin (OXA) with aspartic acid (ASPA) as co-former. The co-crystals were prepared through the mechanochemical solvent drop grinding method. Characterization of the prepared co-crystal (OXA-ASPA) was done by using analytical tools such as differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD). DSC thermogram of OXA-ASPA cocrystal showed a single sharp melting endotherm at 235 ºC, which was between the melting peaks of the drug and the counter molecules suggesting the formation of a new phase which is a co-crystal that was further confirmed by using other analytical techniques. FT-IR analysis of OXA-ASPA cocrystal showed a shift in a hydroxyl, carbonyl, and amine peaks as compared to pure drugs indicating all these functional groups are participating in cocrystal formation. The appearance of new peaks in the PXRD pattern of cocrystals in comparison to individual components showed that a new crystalline entity has been formed. The Crystal structure of cocrystal was determined using material studio software (Biovia) from PXRD. The equilibrium solubility study of OXA-ASPA showed improvement in solubility as compared to pure drug. Therefore, it was envisioned to prepare the co-crystal of oxaprozin with a suitable conformer to modulate its physiochemical properties and consequently, the biopharmaceutical parameters.

Keywords: cocrystals, coformer, oxaprozin, solubility

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Authors: Fatemeh Saadat Ghareh Bagh, Srimanta Ray, Jerald Lalman

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Lignin, the largest inventory of organic carbon with a high caloric energy value is a major component in woody and non-woody biomass. In pulping mills, a large amount of the lignin is burned for energy. At the same time, the phenolic structure of lignin enables it to be converted to value-added compounds.This study has focused on extracting lignin from black liquor using deep eutectic solvents (DESs). Therefore, three choline chloride (ChCl)-DESs paired with lactic acid (LA) (1:11), oxalic acid.2H₂O (OX) (1:4), and malic acid (MA) (1:3) were synthesized at 90oC and atmospheric pressure. The kinetics of lignin recovery from black liquor using DES was investigated at three moderate temperatures (338, 353, and 368 K) at time intervals from 30 to 210 min. The extracted lignin (acid soluble lignin plus Klason lignin) was characterized by Fourier transform infrared spectroscopy (FTIR). The FTIR studies included comparing the extracted lignin with a model Kraft lignin. The extracted lignin was characterized spectrophotometrically to determine the acid soluble lignin (ASL) [TAPPI UM 250] fraction and Klason lignin was determined gravimetrically using TAPPI T 222 om02. The lignin extraction reaction using DESs was modeled by first-order reaction kinetics and the activation energy of the process was determined. The ChCl:LA-DES recovered lignin was 79.7±2.1% at 368K and a DES:BL ratio of 4:1 (v/v). The quantity of lignin extracted for the control solvent, [emim][OAc], was 77.5+2.2%. The activation energy measured for the LA-DES system was 22.7 KJ mol⁻¹, while the activation energy for the OX-DES and MA-DES systems were 7.16 KJ·mol⁻¹ and 8.66 KJ·mol⁻¹ when the total lignin recovery was 75.4 ±0.9% and 62.4 ±1.4, % respectively.

Keywords: black liquor, deep eutectic solvents, kinetics, lignin

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Authors: Mohamed dammak

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Great attention has been paid to the design and synthesis of novel organic-inorganic compounds in recent decades because of their structural variety and the large diversity of atomic arrangements. In this work, the structure for the novel dimethyl aminopyridine tetrachlorocobaltate (C₇H₁₁N₂)₂CoCl₄ prepared by the slow evaporation method at room temperature has been successfully discussed. The X-ray diffraction results indicate that the hybrid material has a triclinic structure with a P space group and features a 0D structure containing isolated distorted [CoCl₄]2- tetrahedra interposed between [C7H11N²⁻]+ cations forming planes perpendicular to the c axis at z = 0 and z = ½. The effect of the synthesis conditions and the reactants used, the interactions between the cationic planes, and the isolated [CoCl4]2- tetrahedra are employing N-H...Cl and C-H…Cl hydrogen bonding contacts. The inspection of the Hirshfeld surface analysis helps to discuss the strength of hydrogen bonds and to quantify the inter-contacts. A phase transition was discovered by thermal analysis at 390 K, and comprehensive dielectric research was reported, showing a good agreement with thermal data. Impedance spectroscopy measurements were used to study the electrical and dielectric characteristics over a wide range of frequencies and temperatures, 40 Hz–10 MHz and 313–483 K, respectively. The Nyquist plot (Z" versus Z') from the complex impedance spectrum revealed semicircular arcs described by a Cole-Cole model. An electrical circuit consisting of a link of grain and grain boundary elements is employed. The real and imaginary parts of dielectric permittivity, as well as tg(δ) of (C₇H₁₁N₂)₂CoCl₄ at different frequencies, reveal a distribution of relaxation times. The presence of grain and grain boundaries is confirmed by the modulus investigations. Electric and dielectric analyses highlight the good protonic conduction of this material.

Keywords: organic-inorganic, phase transitions, complex impedance, protonic conduction, dielectric analysis

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Authors: Shubham Sharma, Swarna Jaiswal, Brendan Duffy, Amit Jaiswal

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The key features of any active packaging film are its biodegradability and antimicrobial properties. Biological macromolecules such as polyphenols (ferulic acid (FA) and tannic acids (TA)) are naturally found in plants such as grapes, berries, and tea. In this study, antimicrobial activity screening of several polyphenols was carried out by using minimal inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) against two strains of gram-negative bacteria - Salmonella typhimurium, Escherichia coli, and two-gram positive strains - Staphylococcus aureus and Listeria monocytogenes. FA and TA had shown strong antibacterial activity at the low concentration against both gram-positive and gram-negative bacteria. The selected polyphenols FA and TA were incorporated at various concentrations (1%, 5%, and 10% w/w) in the poly(lactide) – poly (butylene adipate-co-terephthalate) (PLA-PBAT) composite film by using the solvent casting method. The effect of TA and FA incorporation in the packaging was characterized based on morphological, optical, color, mechanical, thermal, and antimicrobial properties. The thickness of the FA composite film was increased by 1.5 – 7.2%, while for TA composite film, it increased by 0.018 – 1.6%. FA and TA (10 wt%) composite film had shown approximately 65% - 66% increase in the UV barrier property. As the FA and TA concentration increases from 1% - 10% (w/w), the TS value increases by 1.98 and 1.80 times, respectively. The water contact angle of the film was observed to decrease significantly with the increase in the FA and TA content in the composite film. FA has shown more significant increase in antimicrobial activity than TA in the composite film against Listeria monocytogenes and E. coli. The FA and TA composite film has the potential for its application as an active food packaging.

Keywords: active packaging, biodegradable film, polyphenols, UV barrier, tensile strength

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Authors: Hanifa Taher, Sulaiman Al-Zuhair, Ali H. Al-Marzouqi, Yousef Haik, Mohammed Farid

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Biodiesel, as an alternative renewable fuel, has been receiving increasing attention due to the limited supply of fossil fuels and the increasing need for energy. Microalgae is a promising source for lipids, which can be converted to biodiesel. The biodiesel production from microalgae lipids using lipase catalyzed reaction in supercritical CO2 medium has several advantages over conventional production processes. However, identifying the optimum microalgae lipid extraction and transesterification conditions is still a challenge. In this study, the lipids extracted from Scenedesmus sp. and their enzymatic transesterification using supercritical carbon dioxide have been investigated. The effect of extraction variables (temperature, pressure and solvent flow rate) and reaction variables (enzyme loading, incubation time, methanol to lipids molar ratio and temperature) were considered. Process parameters and their effects were studied using a full factorial analysis of both. Response Surface Methodology (RSM) and was used to determine the optimum conditions for the extraction and reaction steps. For extraction, the optimum conditions were 53 °C and 500 bar, whereas for the reaction the optimum conditions were 35% enzyme loading, 4 h reaction, 9:1 molar ratio and 50 oC. At these optimum conditions, the highest biodiesel production yield was found to be 82 %. The fuel properties of the produced biodiesel, at optimum reaction condition, were determined and compared to ASTM standards. The properties were found to comply with the limits, and showed a low glycerol content, without any separation step.

Keywords: biodiesel, lipase, supercritical CO2, standards

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Authors: Elin Julianti, Marlia Singgih, Masayoshi Arai, Jianyu Lin, Masteria Yunovilsa Putra, Muhammad Azhari, Agnia S. Muharam

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The search for a source of new medicinal compounds with anticancer activity from natural products has become important to resolve the ineffectiveness problem of pancreatic cancer therapy. Fungal marine microorganisms are prolific sources of bioactive natural products. In this present study, the ethyl acetate extract of cultured broth of Trichoderma longibrachiatum marine sponge-derived fungi exhibited selective cytotoxicity against human pancreatic carcinoma PANC-1 cells cultured under glucose-deficient conditions (IC50 = 98,4 µg/mL). The T. longibrachiatum was fermented by the static method at room temperature for 60 days. The culture broth was extracted using ethyl acetate by liquid-liquid extraction method. The liquid-liquid extraction was conducted toward the ethyl extract by using 90% MeOH-H₂O and n-|Hexane as a solvent. The extract of 90% MeOH-H₂O was fractionated by liquid extraction using by C₁₈ reversed-phase vacuum flash chromatography using mixtures of MeOH-H₂O, from 50:50 to 100:0, and 1% TFA MeOH as the eluents to yield six fractions. The fraction 2 (MeOH-H2O, 70:30) and fraction 3 (MeOH-H2O, 80:20) showed moderate cytotoxicity with IC50 value of 119.3 and 274.7 µg/mL, respectively. Fraction 4 (MeOH-H₂O, 90:10) showed the highest cytotoxicity activity with IC₅₀value of < 10 µg/mL. The chemical compounds of the fractions that are responsible for cytotoxic activity are potent for further investigation.

Keywords: cytotoxic activity, trichoderma longibrachiatum, marine-derived fungi, PANC-1 cell line

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Authors: T. C. Machaba, S. M. Mahlo

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The current study investigates the antifungal properties of crude plant extracts from selected medicinal plant species. Eight plant species used by the traditional healers and local people to treat fungal infections were selected for further phytochemical analysis and biological assay. The selected plant species were extracted with solvent of various polarities such as acetone, methanol, ethanol, hexane, dichloromethane, ethyl acetate and water. Leaf, roots and bark extracts of Maerua juncea Pax, Albuca seineri (Engl & K. Krause) J.C Manning & Goldblatt, Senna italica Mill., Elephantorrhiza elephantina (Burch.) Skeels, Indigofera circinata Benth., Schinus molle L., Asparagus buchananii Bak., were screened for antifungal activity against three animal fungal pathogens (Candida albicans, Aspergillus fumigatus and Cryptococcus neoformans). All plant extracts were active against the tested microorganisms. Acetone, dichloromethane, hexane and ethanol extracts of Senna italica and Elephantorrhiza elephantine had excellent activity against Candida albicans and A. fumigatus with the lowest MIC value of 0.02 mg/ml. Bioautography assay was used to determine the number of antifungal compounds presence in the plant extracts. No active compounds were observed in plant extracts of Indigofera circinnata, Schinus molle and Pentarrhinum insipidum with good antifungal activity against C. albicans and A. fumigatus indicating possible synergism between separated metabolites.

Keywords: antifungal activity, bioautography, ethnobotanical survey, minimum inhibitory concentration

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Authors: Mahmoud A. Abdulhamid

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Poly(ether-ether-ketone) (PEEK) has received increased attention due to its outstanding performance in different membrane applications including gas and liquid separation. However, it suffers from a semi-crystalline morphology, bad solubility and low porosity. To fabricate membranes from PEEK, the usage of harsh acid such as sulfuric acid is essential, regardless its hazardous properties. In this work, we report the molecular design of poly(ether-ether-ketones) (iPEEKs) with intrinsic porosity character, by incorporating kinked units into PEEK backbone such as spirobisindane, Tröger's base, and triptycene. The porous polymers were used to fabricate stable membranes for organic solvent nanofiltration application. To better understand the mechanism, we conducted molecular dynamics simulations to evaluate the possible interactions between the polymers and the solvents. Notable enhancement in separation performance was observed confirming the importance of molecular engineering of high-performance polymers. The iPEEKs demonstrated good solubility in polar aprotic solvents, a high surface area of 205–250 m² g⁻¹, and excellent thermal stability. Mechanically flexible nanofiltration membranes were prepared from N-methyl-2-pyrrolidone dope solution at iPEEK concentrations of 19–35 wt%. The molecular weight cutoff of the membranes was fine-tuned in the range of 450–845 g mol⁻¹ displaying 2–6 fold higher permeance (3.57–11.09 L m⁻² h⁻¹ bar⁻¹) than previous reports. The long-term stabilities were demonstrated by a 7 day continuous cross-flow filtration.

Keywords: molecular engineering, polymer synthesis, membrane fabrication, liquid separation

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Authors: F. Bellali, M. Kharroubi, M. Loutfi, N.Bourhim

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In Morocco, fish processing industry is an important source income for a large amount of byproducts including skins, bones, heads, guts and scales. Those underutilized resources particularly scales contain a large amount of proteins and calcium. Scales from Sardina plichardus resulting from the transformation operation have the potential to be used as raw material for the collagen production. Taking into account this strong expectation of the regional fish industry, scales sardine upgrading is well justified. In addition, political and societal demands for sustainability and environment-friendly industrial production systems, coupled with the depletion of fish resources, drive this trend forward. Therefore, fish scale used as a potential source to isolate collagen has a wide large of applications in food, cosmetic and bio medical industry. The main aim of this study is to isolate and characterize the acid solubilize collagen from sardine fish scale, Sardina pilchardus. Experimental design methodology was adopted in collagen processing for extracting optimization. The first stage of this work is to investigate the optimization conditions of the sardine scale deproteinization on using response surface methodology (RSM). The second part focus on the demineralization with HCl solution or EDTA. Moreover, the last one is to establish the optimum condition for the isolation of collagen from fish scale by solvent extraction. The basic principle of RSM is to determinate model equations that describe interrelations between the independent variables and the dependent variables.

Keywords: Sardina pilchardus, scales, valorization, collagen extraction, response surface methodology

Procedia PDF Downloads 389

Authors: Maria Magdy Danial Riad

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The objective of this study was to investigate the effect of different protein sources with different degradability ratios during late gestation of ewes on colostrum composition and its IgG concentration, body weight change of dams, and birth weight of their lambs. Objectives: 35 multiparous native crossbred ewes (BW= 59±2.5kg) were randomly allocated to five dietary treatments (7 ewes / treatment) for 2 months prior to lambing. Methods: Experimental diets were isonitrogenous (12.27% CP) and isocaloric (2.22 Mcal ME/kg DM). In diet I (the control), solvent extract soybeans (SESM 33% RUP of CP), II feed grade urea (FGU 31% RUP), III slow release urea (SRU 31% RUP). As sources of undegradable protein, extruded expeller SBM-EESM 40 (37% RUP) and extruded expeller SBM-EESM 60 (41% RUP) were used in groups IV and V, respectively. Results showed no significant effect on feed intake, crude protein (CP), metabolizable energy (ME), and body condition score (BCS). Ewes fed the 37% RUP diet gained more (p<0.05) weight compared with ewes fed the 31% RUP diet (5.62 vs. 2.5kg). Ewes in EESM 60 had the highest levels of fat, protein, total solid, solid not fat, and immunoglobulin and the lowest in urea N content (P< 0.05) in colostrum during the first 24hrs after lambing. Conclusions: Protein source and RUP levels in ewes’ diets had no significant effect (P< 0.05) on lambs’ birth weight and ewes' blood biochemical parameters. Increasing the RUP content of diet during late gestation resulted in an increase in colostrum constituents and its IgG level but had no effect on ewes’ performance and their lambs’ outcome.

Keywords: colostrum, ewes, lambs output, pregnancy, undegradable protein

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Authors: Fatemeh Kourkinejad Gharaei, Tahereh Safari, Zahra Saebinasab

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

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

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Authors: Ahmed Alkarimi, Kevin Welham

Abstract:

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

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

Procedia PDF Downloads 138

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

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

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

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Authors: Sarra Boughaba

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

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

Procedia PDF Downloads 85