Search results for: planar chromatography

Authors: Igor Jerkovic

Abstract:

Biodiversity of flora provides many different nectar sources for the bees. Unifloral honeys possess distinctive flavours, mainly derived from their nectar sources (characteristic volatile organic components (VOCs)). Specific or nonspecific VOCs (chemical markers) could be used for unifloral honey characterisation as addition to the melissopalynologycal analysis. The main honey volatiles belong, in general, to three principal categories: terpenes, norisoprenoids, and benzene derivatives. Some of these substances have been described as characteristics of the floral source, and other compounds, like several alcohols, branched aldehydes, and furan derivatives, may be related to the microbial purity of honey processing and storage conditions. Selection of the extraction method for the honey volatiles profiling should consider that heating of the honey produce different artefacts and therefore conventional methods of VOCs isolation (such as hydrodistillation) cannot be applied for the honey. Two-way approach for the isolation of the honey VOCs was applied using headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE). The extracts were analysed by gas chromatography and mass spectrometry (GC-MS). HS-SPME (with the fibers of different polarity such as polydimethylsiloxane/ divinylbenzene (PDMS/DVB) or divinylbenzene/carboxene/ polydimethylsiloxane (DVB/CAR/PDMS)) enabled isolation of high volatile headspace VOCs of the honey samples. Among them, some characteristic or specific compounds can be found such as 3,4-dihydro-3-oxoedulan (in Centaurea cyanus L. honey) or 1H-indole, methyl anthranilate, and cis-jasmone (in Citrus unshiu Marc. honey). USE with different solvents (mainly dichloromethane or the mixture pentane : diethyl ether 1 : 2 v/v) enabled isolation of less volatile and semi-volatile VOCs of the honey samples. Characteristic compounds from C. unshiu honey extracts were caffeine, 1H-indole, 1,3-dihydro-2H-indol-2-one, methyl anthranilate, and phenylacetonitrile. Sometimes, the selection of solvent sequence was useful for more complete profiling such as sequence I: pentane → diethyl ether or sequence II: pentane → pentane/diethyl ether (1:2, v/v) → dichloromethane). The extracts with diethyl ether contained hydroquinone and 4-hydroxybenzoic acid as the major compounds, while (E)-4-(r-1’,t-2’,c-4’-trihydroxy-2’,6’,6’-trimethylcyclo-hexyl)but-3-en-2-one predominated in dichloromethane extracts of Allium ursinum L. honey. With this two-way approach, it was possible to obtain a more detailed insight into the honey volatile and semi-volatile compounds and to minimize the risks of compound discrimination due to their partial extraction that is of significant importance for the complete honey profiling and identification of the chemical biomarkers that can complement the pollen analysis.

Keywords: honey chemical biomarkers, honey volatile compounds profiling, headspace solid-phase microextraction (HS-SPME), ultrasonic solvent extraction (USE)

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Authors: Peter Joseph Basil Morris, Chhabi Nigam, S. Ramakrishnan, P. Radhakrishna

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This paper brings out the analysis of the airborne Synthetic Aperture Radar (SAR) data using the Range Migration Algorithm (RMA) for the spotlight mode of operation. Unlike in polar format algorithm (PFA), space-variant defocusing and geometric distortion effects are mitigated in RMA since it does not assume that the illuminating wave-fronts are planar. This facilitates the use of RMA for imaging scenarios involving severe differential range curvatures enabling the imaging of larger scenes at fine resolution and at shorter ranges with low center frequencies. The RMA algorithm for the spotlight mode of SAR is analyzed in this paper using the airborne data. Pre-processing operations viz: - range de-skew and motion compensation to a line are performed on the raw data before being fed to the RMA component. Various stages of the RMA viz:- 2D Matched Filtering, Along Track Fourier Transform and Slot Interpolation are analyzed to find the performance limits and the dependence of the imaging geometry on the resolution of the final image. The ability of RMA to compensate for severe differential range curvatures in the two-dimensional spatial frequency domain are also illustrated in this paper.

Keywords: range migration algorithm, spotlight SAR, synthetic aperture radar, matched filtering, slot interpolation

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Authors: H. Yousefnia, A. Golabi Dezfuli, S. Zolghadri, M. Hosntalab

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Peptide receptor radionuclide therapy is nowadays used for the treatment of various abnormalities with somatostatin receptors. In this study, 166Ho-DOTATOC was prepared and the best conditions for its radiolabeling was obtained. For this purpose, a certain of DOTATOC was added to a vial containing 166Ho. various experiments by varying ligand concentration, pH, temperature and time were performed to determine the best conditions. Radiochemical purity of the complex was assessed by instant thin layer chromatography method utilizing 0.9% NaCl as the mobile phase. 166Ho-DOTATOC was prepared with radiochemical purity of higher than 95% at the optimized condition (pH=4, temperature: 95° C, time:30 min). In 0.9% NaCl, free Ho cation was developed at Rf of 0.8 while the complex was remained at the front of the paper.

Keywords: Ho-166, neuroendocrine, octreotide, quality control

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Authors: Silvia Portarena, Chiara Anselmi, Chiara Baldacchini, Enrico Brugnoli

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Extra virgin olive oil (EVOO) is a complex matrix mainly composed by fatty acid and other minor compounds, among which carotenoids are well known for their antioxidative function that is a key mechanism of protection against cancer, cardiovascular diseases, and macular degeneration in humans. EVOO composition in terms of such constituents is generally the result of a complex combination of genetic, agronomical and environmental factors. To selectively improve the quality of EVOOs, the role of each factor on its biochemical composition need to be investigated. By selecting fruits from four different cultivars similarly grown and harvested, it was demonstrated that Raman spectroscopy, combined with chemometric analysis, is able to discriminate the different cultivars, also as a function of the harvest date, based on the relative content and composition of fatty acid and carotenoids. In particular, a correct classification up to 94.4% of samples, according to the cultivar and the maturation stage, was obtained. Moreover, by using gas chromatography and high-performance liquid chromatography as reference techniques, the Raman spectral features further allowed to build models, based on partial least squares regression, that were able to predict the relative amount of the main fatty acids and the main carotenoids in EVOO, with high coefficients of determination. Besides genetic factors, climatic parameters, such as light exposition, distance from the sea, temperature, and amount of precipitations could have a strong influence on EVOO composition of both major and minor compounds. This suggests that the Raman spectra could act as a specific fingerprint for the geographical discrimination and authentication of EVOO. To understand the influence of environment on EVOO Raman spectra, samples from seven regions along the Italian coasts were selected and analyzed. In particular, it was used a dual approach combining Raman spectroscopy and isotope ratio mass spectrometry (IRMS) with principal component and linear discriminant analysis. A correct classification of 82% EVOO based on their regional geographical origin was obtained. Raman spectra were obtained by Super Labram spectrometer equipped with an Argon laser (514.5 nm wavelenght). Analyses of stable isotope content ratio were performed using an isotope ratio mass spectrometer connected to an elemental analyzer and to a pyrolysis system. These studies demonstrate that RR spectroscopy is a valuable and useful technique for the analysis of EVOO. In combination with statistical analysis, it makes possible the assessment of specific samples’ content and allows for classifying oils according to their geographical and varietal origin.

Keywords: authentication, chemometrics, olive oil, raman spectroscopy

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Authors: Nuha Mansour Alhazmi

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Replacement of petro-based plastics by a biodegradable plastic are vastly growing process. Poly-β-hydroxybutyrate (PHB) is a biodegradable biopolymer, synthesized by some bacterial genera. The objective of the current study is to explore the ability of some fungi to biodegrade PHB. The degradation of (PHB) was detected in Petri dish by the formation of a clear zone around the fungal colonies due to the production of depolymerase enzyme which has an interesting role in the PHB degradation process. Among 10 tested fungi, the most active PHB biodegraded fungi were identified as Trichoderma asperellum using morphological and molecular characters. The highest PHB degradation was at 25°C, pH 7.5 after 7 days of incubation for the tested fungi. Finally, the depolymerase enzyme was isolated, purified using column chromatography and characterized. In conclusion, PHB can be biodegraded in solid and liquid medium using depolymerase enzyme from T. asperellum.

Keywords: degradation, depolymerase enzyme, PHB, Trichoderma asperellum

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Authors: Duygu Çimen, Nilay Bereli, Adil Denizli

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In this study is to synthesis magnetic nanoparticles for purify protein C. For this aim, N-Methacryloyl-(L)-histidine methyl ester (MAH) containing 2-hydroxyethyl methacrylate (HEMA) based magnetic nanoparticles were synthesized by using micro-emulsion polymerization technique for templating protein C via metal chelation. The obtained nanoparticles were characterized with Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), zeta-size analysis and electron spin resonance (ESR) spectroscopy. After that, they were used for protein C purification from aqueous solution to evaluate/optimize the adsorption condition. Hereby, the effecting factors such as concentration, pH, ionic strength, temperature, and reusability were evaluated. As the last step, protein C was determined with sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

Keywords: immobilized metal affinity chromatography (IMAC), magnetic nanoparticle, protein C, hydroxyethyl methacrylate (HEMA)

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Authors: Z. H. Safari, M. Anbia, G. H. Kouzegari, R. Amirkhani

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Toluene and Nitro derivatives are widely used in industry particularly in various defense applications. Tri-nitro-toluene derivative is a powerful basic explosive material that is a basis upon which to compare equivalent explosive power of similar materials. The aim of this paper is to measure the explosive power of these hazardous substances in fuels having different shelf-life and therefore optimizing their storage and maintenance. The methodology involves measuring the amounts of di- nitro- toluene and tri-nitro-toluene in the aged samples at 90 ° C by gas chromatography. Results show no significant difference in the concentration of the TNT compound over a given time while there was a significant difference in DNT compound over the same period. The underlying reason is attributed to the simultaneous production of the material with destruction of stabilizer.

Keywords: dinitrotoluene, trinitrotoluene, double-base solid propellants, artificial aging

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Authors: O. Hanita, S. A. Ainnul Hamidah, A. H. Yang Zalila, M. R. Siti Nadiah, M. H. Najihah, M. A. Hapipah

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The crude extract of the leaves of Actinodaphne sesquipedalis Hook. F. Var. Glabra (Kochummen), was taken under phytochemical investigation. The crude methanolic extract was partitioned with a different solvent system by increasing their polarities (n-hexane, dichloromethane, and methanol). The compounds were fractionated and isolated from n-hexane partition by using column chromatography with silica gel 60 or Sephadex LH-20 as a stationary phase and preparative thin layer chromatographic technique. Isolates were characterized using TLC, FTIR, UV spectrophotometer and NMR spectroscopy. The n-hexane fractionates yielded a total of four compounds namely N-methyllaurotetanine (1), dicentrine (2), β-sitosterol (3), and stigmasterol (4). The result indicates that the leaves of Actinodaphne sesquipedalis may provide a rich source of alkaloids and triterpenoids.

Keywords: actinodaphne sesquipedalis, alkaloids, phytochemical investigation, triterpenoids

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Authors: G. V. Manzane, S. J. Modise

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Uterine fibroids, also known as leiomyomas or myomas, are non-cancerous growths that develop in the muscular wall of the uterus during the reproductive years. The cause of uterine fibroids includes hormonal, genetic, growth factors, and extracellular matrix factors. Common symptoms of uterine fibroids include heavy and prolonged menstrual bleeding which can lead to a high risk of anemia, lower abdominal pains, pelvic pressure, infertility, and pregnancy loss. The growth of this tumor is a concern because of its negative impact on women’s health and the increase in their economic burden. Traditional medicinal plants have long been used in Africa for their potential therapeutic effects against various ailments. In this study, we aimed to identify and characterize bioactive compounds from selected African medicinal plants with potential anti-fibrotic properties using Fourier-transform infrared spectroscopy (FTIR) and gas chromatography-mass spectrometry (GCMS) analysis. Two medicinal plant species known for their traditional use in fibrosis-related conditions were selected for investigation. Aqueous extracts were prepared from the plant materials, and FTIR analysis was conducted to determine the functional groups present in the extracts. GCMS analysis was performed to identify the chemical constituents of the extracts. The FTIR analysis revealed the presence of various functional groups, such as phenols, flavonoids, terpenoids, and alkaloids, known for their potential therapeutic activities. These functional groups are associated with antioxidant, anti-inflammatory, and anti-fibrotic properties. The GCMS analysis identified several bioactive compounds, including flavonoids, alkaloids, terpenoids, and phenolic compounds, which are known for their pharmacological activities. The discovery of bioactive compounds in African medicinal plants that exhibit anti-fibrotic effects, opens up promising avenues for further research and development of potential treatments for fibrosis. This suggests the potential of these plants as a valuable source of novel therapeutic agents for treating fibrosis-related conditions. In conclusion, our study identified and characterized bioactive compounds from selected African medicinal plants using FTIR and GCMS analysis. The presence of compounds with known antifibrotic properties suggests that these plants hold promise as a potential source of natural products for the development of novel anti-fibrotic therapies.

Keywords: uterine fibroids, african medicinal plants, bioactive compounds, identify and characterized

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Authors: Noureddine Benharkat, Abdelkader Chouaih, Nourdine Boukabcha

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A thiourea derivative compound was synthesized and subjected to structural analysis using single-crystal X-ray diffraction (XRD). The crystallographic data unveiled its crystallization in the P21/c space group within the monoclinic system. Examination of the dihedral angles indicated a notable non-planar structure. To support and interpret these resulats, density functional theory (DFT) calculations were conducted utilizing the B3LYP functional along with a 6–311 G (d, p) basis set. Additionally, to assess the contribution of intermolecular interactions, Hirshfeld surface analysis and 2D fingerprint plots were employed. Various types of interactions, whether weak intramolecular or intermolecular, within a molecule can significantly impact its stability. The distinctive signature of non-covalent interactions can be detected solely through electron density analysis. The NCI-RDG analysis was employed to investigate both repulsive and attractive van der Waals interactions while also calculating the energies associated with intermolecular interactions and their characteristics. Additionally, a molecular docking study was studied to explain the structure-activity relationship, revealing that the title compound exhibited an affinity energy of -6.8 kcal/mol when docked with B-DNA (1BNA).

Keywords: computational chemistry, density functional theory, crystallography, molecular docking, molecular structure, powder x-ray diffraction, single crystal x-ray diffraction

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Authors: Atilla Bayram

Abstract:

This paper presents the trajectory tracking control of a spatial redundant hybrid manipulator. This manipulator consists of two parallel manipulators which are a variable geometry truss (VGT) module. In fact, each VGT module with 3-degress of freedom (DOF) is a planar parallel manipulator and their operational planes of these VGT modules are arranged to be orthogonal to each other. Also, the manipulator contains a twist motion part attached to the top of the second VGT module to supply the missing orientation of the endeffector. These three modules constitute totally 7-DOF hybrid (parallel-parallel) redundant spatial manipulator. The forward kinematics equations of this manipulator are obtained, then, according to these equations, the inverse kinematics is solved based on an optimization with the joint limit avoidance. The dynamic equations are formed by using virtual work method. In order to test the performance of the redundant manipulator and the controllers presented, two different desired trajectories are followed by using the computed force control method and a switching control method. The switching control method is combined with the computed force control method and genetic algorithm. In the switching control method, the genetic algorithm is only used for fine tuning in the compensation of the trajectory tracking errors.

Keywords: computed force method, genetic algorithm, hybrid manipulator, inverse kinematics of redundant manipulators, variable geometry truss

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Authors: M. A. Ferhat, M. N. Boukhatem, F. Chemat

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Lycopene extraction with petroleum derivatives as solvents has caused safety, health, and environmental concerns everywhere. Thus, finding a safe alternative solvent will have a strong and positive impact on environments and general health of the world population. d-limonene from the orange peel was extracted through a steam distillation procedure followed by a deterpenation process and combining this achievement by using it as a solvent for extracting lycopene from tomato fruit as a substitute of dichloromethane. Lycopene content of fresh tomatoes was determined by high-performance liquid chromatography after extraction. Yields obtained for both extractions showed that yields of d-limonene’s extracts were almost equivalent to those obtained using dichloromethane. The proposed approach using a green solvent to perform extraction is useful and can be considered as a nice alternative to conventional petroleum solvent where toxicity for both operator and environment is reduced.

Keywords: alternative solvent, d-limonene, extraction, lycopene

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Authors: M. Hakami, A. Jammaly, I. Attafi, M. Oraiby, M. Jeraiby

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We reviewed an unusual case of a 65-year-old male taking an herbal mixture containing compounds with anticholinesterase activity for a long period of time, presented with acute my myocardial infarction and multiple organ dysfunction syndrome followed by death. Clinically, there are findings correlated with anticholinesterase activity, such as bilateral miosis, diaphoresis, vomiting and fasciculation without a history of any toxic ingestion or exposure. Gas chromatography–mass spectrometry screening studies identified the presence of thymol, anethole in the herbal extract and butylated hydroxytoluene in the blood sample. Hence, with this case report, we intend to highlight the necessity of evaluating the long-term use of the herbal mixture.

Keywords: cholinesterase inhibitors, thymole, anethole, butylatedhydroxytoluene, cardiac toxicity, myocardial infarction

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Authors: Mohamed Khedr, Ahmed Farghali, Waleed El Rouby, Abdelrhman Hamdeldeen

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Pure CeO2, Sm and Gd doped CeO2 were successfully prepared via hydrothermal method. The effect of hydrothermal temperature, reaction time and precursors were investigated. The prepared nanoparticles were characterized using X-ray diffraction (XRD), FT-Raman Spectroscopy, transmission electron microscope (TEM) and field emission scanning electron microscope (FESEM). The prepared pure and doped CeO2 nanoparticles were used as photo-catalyst for the degradation of Methylene blue (MB) dye under UV light irradiation. The results showed that Gd doped CeO2 nano-particles have the best catalytic degradation effect for MB under UV irradiation. The degradation pathways of MB were followed using liquid chromatography (LC/MS) and it was found that Gd doped CeO2 was able to oxidize MB dye with a complete mineralization of carbon, nitrogen and sulfur heteroatoms into CO2, NH4+, NO3- and SO42-.

Keywords: CeO2, doped CeO2, photocatalysis, methylene blue

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Authors: C. Nobre, C. C. Castro, A.-L. Hantson, J. A. Teixeira, L. R. Rodrigues, G. De Weireld

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Fructo-oligosaccharides (FOS) are produced from sucrose by Aureobasidium pullulans in yields between 40-60% (w/w). To increase the amount of FOS it is necessary to remove the small, non-prebiotic sugars, present. Two methods for producing high-purity FOS have been developed: the use of microorganisms able to consume small saccharides; and the use of continuous chromatography to separate sugars: simulated moving bed (SMB). It is herein proposed the combination of both methods. The aim of this study is to optimize the composition of the fermentative broth (in terms of salts and sugars) that will be further purified by SMB. A yield of 0.63 gFOS.g Sucrose-1 was obtained with A. pullulans using low amounts of salts in the initial fermentative broth. By removing the small sugars, Saccharomyces cerevisiae and Zymomonas mobilis increased the percentage of FOS from around 56.0% to 83% (w/w) in average, losing only 10% (w/w) of FOS during the recovery process.

Keywords: fructo-oligosaccharides, microbial treatment, Saccharomyces cerevisiae, Zymomonas mobilis

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Authors: Roihatul Mutiah, Sukardiman, Aty Widyawaruyanti

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Calotropis gigantiea (L.) R. Br (Apocynaceae) commonly called as “Biduri” or “giant milk weed” is a well-known weed to many cultures for treating various disorders. Several studies reported that C.gigantea roots has anticancer activity. The main aim of this research was to isolate and identify an active marker compound of C.gigantea roots for quality control purpose of its extract in the development as anticancer natural product. The isolation methods was bioactivity guided column chromatography, TLC, and HPLC. Evaluated anticancer activity of there substances using MTT assay methods. Identification structure active compound by UV, 1HNMR, 13CNMR, HMBC, HMQC spectral and other references. The result showed that the marker active compound was identical as Calotropin.

Keywords: calotropin, Calotropis gigantea, anticancer, marker active

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Authors: Murast Dicleli, Ali SalemMilani

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In this paper, a summary of analytical and experimental studies into the behavior of a new hysteretic damper, designed for seismic protection of structures is presented. The Multi-directional Torsional Hysteretic Damper (MRSD) is a patented invention in which a symmetrical arrangement of identical cylindrical steel cores is so configured as to yield in torsion while the structure experiences planar movements due to earthquake shakings. The new device has certain desirable properties. Notably, it is characterized by a variable and controllable-via-design post-elastic stiffness. The mentioned property is a result of MRSD’s kinematic configuration which produces this geometric hardening, rather than being a secondary large-displacement effect. Additionally, the new system is capable of reaching high force and displacement capacities, shows high levels of damping, and very stable cyclic response. The device has gone through many stages of design refinement, multiple prototype verification tests and development of design guide-lines and computer codes to facilitate its implementation in practice. Practicality of the new device, as offspring of an academic sphere, is assured through extensive collaboration with industry in its final design stages, prototyping and verification test programs.

Keywords: seismic, isolation, damper, adaptive stiffness

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Authors: Nhat Linh Ho, Thanh-Phong Dao, Shyh-Chour Huang, Hieu Giang Le

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This paper presents a design and optimization for a compliant gripper. The gripper is constructed based on the concept of compliant mechanism with flexure hinge. A passive force regulation mechanism is presented to control the grasping force a micro-sized object instead of using a sensor force. The force regulation mechanism is designed using the planar springs. The gripper is expected to obtain a large range of displacement to handle various sized objects. First of all, the statics and dynamics of the gripper are investigated by using the finite element analysis in ANSYS software. And then, the design parameters of the gripper are optimized via Taguchi method. An orthogonal array L₉ is used to establish an experimental matrix. Subsequently, the signal to noise ratio is analyzed to find the optimal solution. Finally, the response surface methodology is employed to model the relationship between the design parameters and the output displacement of the gripper. The design of experiment method is then used to analyze the sensitivity so as to determine the effect of each parameter on the displacement. The results showed that the compliant gripper can move with a large displacement of 213.51 mm and the force regulation mechanism is expected to be used for high precision positioning systems.

Keywords: flexure hinge, compliant mechanism, compliant gripper, force regulation mechanism, Taguchi method, response surface methodology, design of experiment

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Authors: Sandeep Kaur

Abstract:

Phycoerythrin (PE) from the mesophilic filamentous cyanobacterium Nostoc piscinale PUPCCC 405.17, a good producer of phycobiliproteins, has been characterized in terms of their unit assembly and stability. The phycoerythrin was extracted by freeze-thawing the cells in water, concentrated by ammonium sulphate fractionation and purified by anion exchange chromatography. The purification process resulted in 2.90 fold increase in phycoerythrin purity reaching to 1.54. Sodium Dodecyl Sulphate- Polyacrylamide Gel Electrophoresis of purified PE demonstrated three protein bands of 14.3, 27.54 and 39.81 kDa. The native PE also showed one band of 125.87 kDa, assumed to be a dimer (αβ)2γ based on results of non-denaturing PAGE. Lyophilized powder PE was more stable compared to phycoerythrin in the solution. The half-life of dry PE is 80 days when stored at 4 °C under dark. The phycoerythrin from this organism has potential applications in food as natural colour and as a fluorescent marker.

Keywords: characterization, Nostoc piscinale, phycoerythrin, purification

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Authors: Mian Jiang, Zhenyi Wu

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We have incorporated green components into existing analytical chemistry curriculum with the aims to present a more environment benign approach in both teaching laboratory and undergraduate research. These include the use of cheap, sustainable, and market-available material; minimized waste disposal, replacement of non-aqueous media; and scale-down in sample/reagent consumption. Model incorporations have covered topics in quantitative chemistry as well as instrumental analysis, lower division as well as upper level, and research in traditional titration, spectroscopy, electrochemical analysis, and chromatography. The green embedding has made chemistry more daily life relevance, and application focus. Our approach has the potential to expand into all STEM fields to make renewable, high-impact education experience for undergraduate students.

Keywords: green analytical chemistry, pencil lead, mercury, renewable

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Authors: Norazlan Mohmad Misnan, Maizatul Hasyima Omar, Mohd Isa Wasiman

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Papaya (Carica papaya L., Caricaceae) is a tree which mainly cultivated for its fruits in many tropical regions including Australia, Brazil, China, Hawaii, and Malaysia. Beside of fruits, its leaves, seeds, and latex have also been traditionally used for treating diseases, which also reported to possess anti-cancer and anti- malaria properties. Its leaves have been reported to consist of various chemical compounds such as alkaloids, flavonoids and phenolics. Clitorin and manghaslin are among major flavonoids presence. Thus, the aim of this study is to quantify the purity of these isolated compounds (clitorin and manghsalin) by using quantitative Nuclear Magnetic Resonance (qNMR) analysis. Only fresh C. papaya leaves were used for juice extraction procedure and subsequently was freeze-dried to obtain a dark green powdered form of the extract prior to Centrifugal Partition Chromatography (CPC) separation. The CPC experiments were performed using a two-phase solvent system comprising ethyl acetate/butanol/water (1:4:5, v/v/v/v) solvent. The upper organic phase was used as the stationary phase, and the lower aqueous phase was employed as the mobile phase. Ten fractions were obtained after an hour runtime analysis. Fraction 6 and fraction 8 has been identified as clitorin (m/z 739.21 [M-H]-) and manghaslin (m/z 755.21 [M-H]-), respectively, based on LCMS data and full analysis of NMR (1H NMR, 13C NMR, HMBC, and HSQC). The 1H-qNMR measurements were carried out using a 400 MHz NMR spectrometer (JEOL ECS 400MHz, Japan) and deuterated methanol was used as a solvent. Quantification was performed using the AQARI method (Accurate Quantitative NMR) with deuterated 1,4-Bis(trimethylsilyl)benzene (BTMSB) as an internal reference substances. This AQARI protocol includes not only NMR measurement but also sample preparation that provide highest precision and accuracy than other qNMR methods. The 90° pulse length and the T1 relaxation times for compounds and BTMSB were determined prior to the quantification to give the best signal-to-noise ratio. Regions containing the two downfield signals from aromatic part (6.00–6.89 ppm), and the singlet signal, (18H) arising from BTMSB (0.63-1.05ppm) were selected for integration. The purity of clitorin and manghaslin were calculated to be 52.22% and 43.36%, respectively. Further purification is needed in order to increase its purity. This finding has demonstrated the use of qNMR for quality control and standardization of various plant extracts and which can be applied for NMR fingerprinting of other plant-based products with good reproducibility and in the case where commercial standards is not readily available.

Keywords: Carica papaya, clitorin, manghaslin, quantitative Nuclear Magnetic Resonance, Centrifugal Partition Chromatography

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Authors: Wanthani Paengsri, Thanyarat Chuesaard, Napapha Promsawan

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Spilanthes acmella Murr. was extracted with methanol, yielding methanol crude extract 5.86 %w/w. This study aimed to examine the chemical composition and antioxidant activity of methanolic crude extract. The chemical composition of methanolic crude extract was analyzed by gas chromatography-mass spectrometry (GC-MS). The predominant components were found to be palmitic acid (40.08%), 2-hexadecanoyl glycerol (6.96%) and octadecanoic acid (4.06%). Antioxidant activity was determined using 2,2-diphenyl-1-picryl hydrazyl (DPPH) free radical, for evaluating free radicle scavenging activity. The methanolic extract at 150 µg/mL showed an antioxidant activity with high of radical scavenging activity (75.23%).

Keywords: antioxidant activity, GC-MS analysis, Spilanthes, Phak-Kratt Hauwaen

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Authors: S. A. Agbalajobi, W. A. Bello

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The study carried out analysis on slope stability in an excavated gneiss rock using geological strength index (GSI) in Ilorin, Kwara State, Nigeria. A kinematic analysis of planar discontinuity sets in a gneiss deposit was carried out to ascertain the degree of slope stability. Discontinuity orientations in the rock mass were mapped using compass clinometers. The average result of physical and mechanical properties such as specific gravity, unit weight, uniaxial compressive strength, point load index, and Schmidt rebound value are 2.64 g/m3, 25.95 kN/m3, 156 MPa, 6.5 MPa, and 53.12 respectively. Also, a statistical model equation relating the rock strength was developed. The analyses states that the rock face is susceptible to wedge failures having all the geometrical conditions associated with the occurrence of such failures were noticeable. It can be concluded that analyses of discontinuity orientation in relation to cut face direction in rock excavation is essential for mine planning to forestall mine accidents. Assessment of excavated slope methods was evident that one excavation method (blasting and/or use of hydraulic hammer) is applicable for the given rock strength, the ease of excavation decreases as the rock mass quality increases, thus blasting most suitable for such operation.

Keywords: slope stability, wedge failure, geological strength index (GSI), discontinuities and excavated slope

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Authors: M'Hamed Boulakroune, Mouloud Challal, Hassiba Louazene, Saida Fentiz

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This paper presents a new ultra wideband (UWB) microstrip bandpass filter (BPF) at microwave frequencies. The first one is based on multiple-mode resonator (MMR) and rectangular-shaped defected ground structure (DGS). This filter, which is compact size of 25.2 x 3.8 mm2, provides in the pass band an insertion loss of 0.57 dB and a return loss greater than 12 dB. The second structure is a tunable bandpass filters using planar patch resonators based on diode varactor. This filter is formed by a triple mode circular patch resonator with two pairs of slots, in which the varactors are connected. Indeed, this filter is initially centered at 2.4 GHz, the center frequency of the tunable patch filter could be tuned up to 1.8 GHz simultaneously with the bandwidth, reaching high tuning ranges. Lossless simulations were compared to those considering the substrate dielectric, conductor losses, and the equivalent electrical circuit model of the tuning element in order to assess their effects. Within these variations, simulation results showed insertion loss better than 2 dB and return loss better than 10 dB over the passband. The proposed filters presents good performances and the simulation results are in satisfactory agreement with the experimentation ones reported elsewhere.

Keywords: defected ground structure, diode varactor, microstrip bandpass filter, multiple-mode resonator

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Authors: Yeonjune Kang

Abstract:

A triangulation of a planar region is a partition of that region into triangles. In the finite element method, triangulations are often used as the grid underlying a computation. In order to be suitable as a finite element mesh, a triangulation must have well-shaped triangles, according to criteria that depend on the details of the particular problem. For instance, most methods require that all triangles be small and as close to the equilateral shape as possible. Stated differently, one wants to avoid having either thin or flat triangles in the triangulation. There are many triangulation procedures, a particular one being the one known as the longest edge bisection algorithm described below. Starting with a given triangle, locate the midpoint of the longest edge and join it to the opposite vertex of the triangle. Two smaller triangles are formed; apply the same bisection procedure to each of these triangles. Continuing in this manner after n steps one obtains a triangulation of the initial triangle into 2n smaller triangles. The longest edge algorithm was first considered in the late 70’s. It was shown by various authors that this triangulation has the desirable properties for the finite element method: independently of the number of iterations the angles of these triangles cannot get too small; moreover, the size of the triangles decays exponentially. In the present paper we consider a related triangulation algorithm we refer to as the largest angle bisection procedure. As the name suggests, rather than bisecting the longest edge, at each step we bisect the largest angle. We study the properties of the resulting triangulation and prove that, while the general behavior resembles the one in the longest edge bisection algorithm, there are several notable differences as well.

Keywords: angle bisectors, geometry, triangulation, applied mathematics

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Authors: Priyesh Kumar Pandey, Zakir Husain, R. K. Jarial

Abstract:

Condition monitoring and diagnostic is important for testing of power transformer in order to estimate the remnant life. Concentration of furan content in transformer oil can be a promising indirect measurement of the aging of transformer insulation. The oil gets contaminated mainly due to ageing. The present paper introduces adaptive neuro fuzzy technique to correlate furanic compounds obtained by high performance liquid chromatography (HPLC) test and remnant life of the power transformer. The results are obtained by conducting HPLC test at TIFAC-CORE lab, NIT Hamirpur on thirteen power transformer oil samples taken from Himachal State Electricity Board, India.

Keywords: adaptive neuro fuzzy technique, furan compounds, remnant life, transformer oil

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Authors: Femy M. Makkar, S. Chandrakaran, N. Sankar

Abstract:

The concept of reinforced earth has been used in the field of geotechnical engineering since 1960s, for many applications such as, construction of road and rail embankments, pavements, retaining walls, shallow foundations, soft ground improvement and so on. Conventionally, planar geosynthetic materials such as geotextiles and geogrids were used as the reinforcing elements. Recently, the use of three dimensional reinforcements becomes one of the emerging trends in this field. So, in the present investigation, three dimensional geogrid is proposed as a reinforcing material. Laboratory scaled plate load tests are conducted on a model square footing resting on 3D geogrid reinforced sand bed. The performance of 3D geogrids in triangular and square pattern was compared with conventional geogrids and the improvement in bearing capacity and reduction in settlement and heave are evaluated. When single layer of reinforcement was placed at an optimum depth of 0.25B from the bottom of the footing, the bearing capacity of conventional geogrid reinforced soil improved by 1.85 times compared to unreinforced soil, where as 3D geogrid reinforced soil with triangular pattern and square pattern shows 2.69 and 3.05 times improvement respectively compared to unreinforced soil. Also, 3D geogrids performs better than conventional geogrids in reducing the settlement and heave of sand bed around the model footing.

Keywords: 3D reinforcing elements, bearing capacity, heavy, settlement

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Authors: Mohamed Tamer, Wink Michael

Abstract:

DNA intercalating agents increase the stability of DNA which can be demonstrated by measuring the melting temperature Tm. Tm can be determined in a spectrophotometer in which the cell temperature is increased gradually. The resulting absorption data comes as a sigmoidal curve from which melting temperature can be determined when half of the DNA has denatured. The current study aims to assess DNA intercalating activities of four pure bioactive isoquinoline alkaloids: sanguinarine, berberine, allocryptopine, and chelerythrine which were isolated from Chelidonium majus (Papaveraceae) by repeated silica gel column chromatography, recrystallization and preparative TLC. The isolated compounds were identified by comparing their physical properties and mass spectra with those of the published data. The results showed that sanguiarine is the most active intercalating agent with Tm value of 83.55 ± 0.49 followed by berberine, chelerythrine, and allocryptopine with Tm values 62.58 ± 0.47, 51.38 ± 0.37 and 50.94 ± 0.65, respectively, relative to 49.78 ± 1.05 of bacteriophage DNA alone and 86.09 ± 0.5 for ethidium bromide as a positive control.

Keywords: alkaloids, Chelidonium majus, DNA intercalation, Tm

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Authors: Muhammad A. Ado, Intan S. Ismail, Hasanah M. Ghazali, Faridah Abas

Abstract:

In this study, we have investigated the phytochemical constituents of soluble fractions of dichloromethane (DCM) of methanolic leaves extract of the Callicarpa maingayi. The phytochemicals investigation has resulted in the isolation of three triterpenoids (euscaphic acid (1), arjunic acid (2), and ursolic acid (3)) together with two flavones apigenin (4) and acacetin (5)), two phytosterols (stigmasterol 3-O-β-glycopyranoside (6) and sitosterol 3-O-β-glycopyranoside (7)), and one fatty acid (n-hexacosanoic acid (8)). Six (6) compounds isolated from this species were isolated for the first time (1, 2, 3, 4, 5, and 8). Their structures were elucidated and identified by spectral methods of one and two-dimensional NMR techniques, gas chromatography-mass spectrometry, and comparison with the previously reported literature. The biological activity of three compounds (1-3) was carried out on acetylcholinesterase inhibition activity. Compound (3) was found to displayed good inhibition against AChE with an IC₅₀ value of 21.5 ± 0.022 μM.

Keywords: acetylcholinesterase, Callicarpa maingayi, euscaphic acid, ursolic acid

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Authors: E. M. Condori-Peñaloza, S. S. Costa

Abstract:

Eleusine indica L, known as goose-grass, is considered a troublesome weed that can cause important economic losses in the agriculture worldwide. However, this grass is used as a medicinal plant in some regions of Brazil to treat influenza and pneumonia. In Africa and Asia, it is used to treat malaria and as diuretic, anti-helminthic, among other uses. Despite its therapeutic potential, little is known about the chemical composition and bioactive compounds of E. indica. Hitherto, two major flavonoids, schaftoside and vitexin, were isolated from aerial part of the species and showed inhibitory activity on lung neutrophil influxes in mice, suggesting a beneficial effect on airway inflammation. Therefore, the aim of this study was to analyze the chemical profile of aqueous extracts from aerial parts of Eleusine indica specimens using high performance liquid chromatography (HPLC-DAD) and 1H nuclear magnetic resonance spectroscopy (NMR), with emphasis on phenolic compounds. Specimens of E. indica were collected in Minas Gerais state, Brazil. Aerial parts of fresh plants were extracted by decoction (10% p/v). After spontaneous precipitation of the aqueous extract at 10-12°C for 24 hours, the supernatant obtained was frozen and lyophilized. After that, 1 g of the extract was dissolved into 25 mL of water and fractionated on a reverse phase chromatography column (RP-2), eluted with a gradient of H2O/EtOH. Five fractions were obtained. The extract and fractions had their chemical profile analyzed by using HPLC-DAD (C-18 column: 20 μL, 256 -365 nm; gradient water 0.01% phosphoric acid/ acetonitrile. The extract was also analyzed by NMR (1H, 500 MHz, D2O) in order to access its global chemical composition. HPLC-DAD analyses of crude extract allowed the identification of ten phenolic compounds. Fraction 1, eluted with 100% water, was poor in phenolic compounds and no major peak was detected. In fraction 2, eluted with 100% water, it was possible to observe one major peak at retention time (RT) of 23.75 minutes compatible with flavonoid; fraction 3, also eluted with 100% water, showed four peaks at RT= 21.47, 23.52, 24.33 and 25.84 minutes, all of them compatible with flavonoid. In fraction 4, eluted with 50%/ethanol/50% water, it was possible to observe 3 peaks compatible with flavonoids at RT=24.65, 26.81, 27.49 minutes, and one peak (28.83 min) compatible with a phenolic acid derivative. Finally, in fraction 5, eluted with 100% ethanol, no phenolic substance was detected. The UV spectra of all flavonoids detected were compatible with the flavone subclass (λ= 320-345 nm). The 1H NMR spectra of aerial parts extract showed signals in three regions: δ 0.8-3.0 ppm (aliphatic compounds), δ 3.0-5.5 ppm corresponding to carbohydrates (signals most abundant and overlapped), and δ 6.0-8.5 ppm (aromatic compounds). Signals compatible with flavonoids (rings A and B) could also be detected in the crude extract spectra. These results suggest the presence of several flavonoids in E. indica, which reinforces their therapeutic potential. The pharmacological activities of Eleusine indica extracts and fractions will be further evaluated.

Keywords: flavonoids, HPLC, NMR, phenolic compounds

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