Search results for: high perforamance liquid chromatography

Authors: Ramandeep Kaur, Ashok Kumar Malik

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Fabric Phase Sorptive Extraction (FPSE) combined with Gas chromatography Mass Spectrometry (GCMS) has been developed for the determination of nineteen organochlorine pesticides in various aqueous samples. The method consolidates the features of sol-gel derived microextraction sorbents with rich surface chemistry of cellulose fabric substrate which could directly extract sample from complex sample matrices and incredibly improve the operation with decreased pretreatment time. Some vital parameters such as kind and volume of extraction solvent and extraction time were examinedand optimized. Calibration curves were obtained in the concentration range 0.5-500 ng/mL. Under the optimum conditions, the limits of detection (LODs) were in the range 0.033 ng/mL to 0.136 ng/mL. The relative standard deviations (RSDs) for extraction of 10 ng/mL 0f OCPs were less than 10%. The developed method has been applied for the quantification of these compounds in aqueous and fruit juice samples. The results obtained proved the present method to be rapid and feasible for the determination of organochlorine pesticides in aqueous samples.

Keywords: fabric phase sorptive extraction, gas chromatography-mass spectrometry, organochlorine pesticides, sample pretreatment

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Authors: Erwin Chan, Aravind Subramaniyan, Siti Abdullah Fatehah, Steve Lian Kuling

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Foam assisted lift technology is proven across the industry to provide efficient deliquification in gas wells. Such deliquification is typically achieved by delivering the foamer chemical downhole via capillary strings. In highly liquid loaded wells where capillary strings are not readily available, foamer can be delivered via batch injection or bull-heading. The latter techniques differ from the former in that cap strings allow for liquid to be unloaded continuously, whereas foamer batches require that periodic batching be conducted for the liquid to be unloaded. Although batch injection allows for liquid to be unloaded in wells with suitable water to gas (WGR) ratio and condensate to gas (CGR) ratio without well intervention for capillary string installation, this technique comes with its own set of challenges - for foamer to de-liquify liquids, the chemical needs to reach perforation locations where gas bubbling is observed. In highly scaled perforation zones in certain wells, foamer delivered in batches is unable to reach the gas bubbling zone, thus achieving poor lift efficiency. This paper aims to discuss the techniques and challenges for unloading liquid via batch injection in scaled perforation wells X and Y, whose WGR is 6bbl/MMscf, whose scale build-up is observed at the bottom of perforation interval, whose water column is 400 feet, and whose ‘bubbling zone’ is less than 100 feet. Variables such as foamer Z dosage, batching technique, and well flow control valve opening times are manipulated during the duration of the trial to achieve maximum liquid unloading and gas rates. During the field trial, the team has found optimal values between the three aforementioned parameters for best unloading results, in which each cycle’s gas and liquid rates are compared with baselines with similar flowing tubing head pressures (FTHP). It is discovered that amongst other factors, a good agitation technique is a primary determinant for efficient liquid unloading. An average increment of 2MMscf/d against an average production of 4MMscf/d at stable FTHP is recorded during the trial.

Keywords: foam, foamer, gas lift, liquid unloading, scale, batch injection

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Authors: Ki Woong Lee

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The Center for Axion and Precision Physics Research is studying the search for dark matter using 12 tesla superconducting magnets. A dilution refrigerator is being used for search experiments, and superconducting magnets, superconducting cavities. The dilution refrigerator requires a stable cryogenic environment using liquid helium. Accordingly, a cryogenic system for a stable supply of liquid helium is to be established. This cryogenic system includes the liquefying, supply, storage, and purification of liquid helium. This article presents the basic design, construction, and operation plans for building cryogenic systems.

Keywords: cryogenic system, dilution refrigerator, superconducting magnet, helium recovery system

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Authors: S. Mousavian, A. Abedianpour, A. Khanmohammadi, S. Hematian, Gh. Eidi Veisi

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Ionic liquids are finding a wide range of applications from reaction media to separations and materials processing. In these applications, Vapor–Liquid equilibrium (VLE) is the most important one. VLE for six systems at 353 K and activity coefficients at infinite dilution 〖(γ〗_i^∞) for various solutes (alkanes, alkenes, cycloalkanes, cycloalkenes, aromatics, alcohols, ketones, esters, ethers, and water) in the ionic liquids (1-ethyl-3-methylimidazolium bis (trifluoromethylsulfonyl)imide [EMIM][BTI], 1-hexyl-3-methyl imidazolium bis (trifluoromethylsulfonyl) imide [HMIM][BTI], 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide [OMIM][BTI], and 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide [BMPYR][BTI]) have been used to train neural networks in the temperature range from (303 to 333) K. Densities of the ionic liquids, Hildebrant constant of substances, and temperature were selected as input of neural networks. The networks with different hidden layers were examined. Networks with seven neurons in one hidden layer have minimum error and good agreement with experimental data.

Keywords: ionic liquid, neural networks, VLE, dilute solution

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Authors: Meimei Wen, Chang Nyung Kim

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In the current study, three-dimensional liquid metal (LM) magneto-hydrodynamic (MHD) flows in a manifold with three sub-channels under a uniform magnetic field are numerically investigated. In the manifold, the electrical current can cross channel walls, thus having influence on the flow distribution in each sub-channel. A case with various arrangements of electric conductivity for different parts of channel walls is considered, yielding different current distributions as well as flow distributions in each sub-channel. Here, the imbalance of mass flow rates in the three sub-channels is addressed. Meanwhile, predicted are detailed behaviors of the flow velocity, pressure, current and electric potential of LM MHD flows with three sub-channels. Commercial software CFX is used for the numerical simulation of LM MHD flows.

Keywords: CFX, liquid metal, manifold, MHD flow

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Authors: Bashar Al-Sabti, Jehad Harbali

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Background: Pyridine is a reactive base that might be used in preparing sitagliptin. International Agency for Research on Cancer classifies pyridine in group 2B; this classification means that pyridine is possibly carcinogenic to humans. Therefore, pyridine should be monitored at the allowed limit in sitagliptin pharmaceutical ingredients. Objective: The aim of this study was to develop a novel ultra high performance liquid chromatography mass spectrometry (UHPLC-MS) method to estimate the quantity of pyridine impurity in sitagliptin pharmaceutical ingredients. Methods: The separation was performed on C8 shim-pack (150 mm X 4.6 mm, 5 µm) in reversed phase mode using a mobile phase of water-methanol-acetonitrile containing 4 mM ammonium acetate in gradient mode. Pyridine was detected by mass spectrometer using selected ionization monitoring mode at m/z = 80. The flow rate of the method was 0.75 mL/min. Results: The method showed excellent sensitivity with a quantitation limit of 1.5 ppm of pyridine relative to sitagliptin. The linearity of the method was excellent at the range of 1.5-22.5 ppm with a correlation coefficient of 0.9996. Recoveries values were between 93.59-103.55%. Conclusions: The results showed good linearity, precision, accuracy, sensitivity, selectivity, and robustness. The studied method was applied to test three batches of sitagliptin raw materials. Highlights: This method is useful for monitoring pyridine in sitagliptin during its synthesis and testing sitagliptin raw materials before using them in the production of pharmaceutical products.

Keywords: genotoxic impurity, pyridine, sitagliptin, UHPLC -MS

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Authors: Kane Esien, Eadaoin McCourt, Peter Nockemann, Soveig Felton

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Magnetic ionic liquids (MILs) are a class of ionic liquid incorporating one or more magnetic atoms into the anion or cation of the ionic liquid, endowing the ionic liquid with magnetic properties alongside the existing properties of ionic liquids. MILs have applications in e.g. fluid-fluid separations, electrochemistry, and polymer chemistry. In this study three different types of Bis-Lanthanoates, that exist in different phases, have been synthesised and characterised (Ln = lanthanide): 1) imidazolium lanthanide acetate – [C4Mim]2[Ln2(OAc)8] – forms a crystalline solid at room temperature, 2) phosphonium lanthanide acetate – [P666 14]2[Ln2(OAc)8] – is in a solid glassy state, and 3) phosphonium lanthanide octanoate – [P666 14]2[Ln2(Oct)8] – is an ionic liquid. X-ray diffraction of the crystalline solid imidazolium lanthanide acetate – [C4Mim]2[Ln2(OAc)8] confirm that the Ln(III) ions form dimers, bridged by carboxyl groups, but cannot yield information about samples phosphonium lanthanide acetate – [P666 14]2[Ln2(OAc)8] (glass) and phosphonium lanthanide octanoate – [P666 14]2[Ln2(Oct)8] (ionic liquid) since these lack long-range order. SQUID magnetometry studies show that all three samples have effective magnetic moments consistent with non-interacting Ln(III) ions at room temperature but deviate from this behavior in the same way below 50 K. Through modeling the magnetic response, we are able to show that we have formed magnetic dimers, in all compounds, that are weakly antiferromagnetically interacting

Keywords: dimeric ionic liquids, interactions, SQUID, structure

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Authors: Salem Abdalla

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Objective: Dipyrone is a widely used, well tolerated analgesic drug which, however, is compromised by agranulocytosis as an adverse effect. Subsequent to no enzymatic hydrolysis, the primary metabolic step is N-demethylation of 4-methylaminoantipyrine (4-MAA) to 4-aminoantipyrine (4-AA). The aim of the present study was to identify the cytochrome P-450 enzyme (CYP) mediating this reaction. Methods: We identified the relevant CYP using virus expressed isolated rat liver microsomes with chemical inhibition studies. The substrate of 4-methylaminantipyrine was employed at six different concentrations (25, 50, 100, 400, 800, and 1200 µmol/l) with varying concentrations of selective inhibitors of CYP1A2 (furafylline, fluvoxamine), CYP3A4 (ketoconazole), CYP2A6 (coumarin), CYP2D6 (quinidine), CYP2C19 (omeprazole, fluvoxamine, tranylcypromine), CYP2C9 (sulfaphenazole), and CYP1A1 (alpha-naphthoflavone). 4-MAA and 4-AA were analyzed by HPLC, and enzyme kinetic parameters (Km and Vmax) were determined by regression (Sigma plot 9.0). Results: The N-demethylation of 4-MAA by microsomes prepared from baculovirus-expressing human CYP was pronounced with CYP2C19. Intrinsic clearances of the most active enzymes were 0.092, 0.027, and 0.026 for the CYP enzymes 2C19, 2D6, and 1A2, respectively. Metabolism by rat liver microsomes was strongly inhibited by omeprazole (IC50 of 0.05). Conclusion: The enzyme CYP2C19 apparently has an important role in N-demethylation of 4-methylaminoantipyrine which should be further analyzed in clinical studies and which may also be interesting concerning the agranulocytosis.

Keywords: dipyrone, 4-methylaminoantipyrine (4-MAA), 4- aminoantipyrine (4-AA), metabolism, human CYP2C19

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Authors: Yang Luo, Chang Nyung Kim

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This study numerically analyzes a steady-state, three-dimensional liquid-metal magnetohydrodynamic flows in a conduit with multiple channels under a uniform magnetic field. The geometry of the conduit is of a four-parallel-channels system including one inflow channel and three outflow channels. The liquid-metal flows in the inflow channel, then turns 1800 in the transition segment, finally flows into three different outflow channels simultaneously. This kind of channel system can induce counter flow and co-flow, which is rarely investigated before. The axial velocity in the side layer near the first partitioning wall, which is located between the inflow channel and the first outflow channel, is the highest. ‘M-shaped’ velocity profiles are obtained in the side layers of the inflow and outflow channels. The interdependency of the current, fluid velocity, pressure, electric potential is examined in order to describe the electromagnetic characteristics of the liquid-metal flows.

Keywords: liquid-metal, multiple channels, magnetic field, magnetohydrodynamic

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Authors: Sunaitan Al Mutairi, Kumar Vallatharasu, Batool Ismaeel

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The Water Knock-Out (WKO) facility project is to handle the undesirable impact of the increasing water production rate in South and East Kuwait (S&EK) areas and break the emulsions and ensure sufficient separation of water at the new upstream facility, to reduce the load on the existing separation equipment in the Gathering Centers (GC). As the existing separation equipment in the Gathering Centers are not efficient to separate the emulsions, the Compact Electrostatic Coalescer (CEC) and Vessel Internal Electrostatic Coalescer (VIEC) technologies have been selected for enhancing the liquid-liquid separation by using the alternating voltage/frequency on electrical fields, to handle the increasing water-cut in S&EK. In the Compact Electrostatic Coalescer (CEC) technology method, the CEC equipment is installed downstream of the inlet separator externally, whereas in the Vessel Internal Electrostatic Coalescer (VIEC) technology method, the VIEC is built inside the treater vessel, downstream of the inlet separator with advanced internals for implementing electrocoalescence of water particles and hence enhancing liquids separation. The CEC and VIEC technologies used in the Water Knockout Facility project has the ability to resolve the increasing water cut in the S&EK area and able to enhance the liquid-liquid separation in the WKO facility separation equipment. In addition, the WKO facility is minimizing the load on the existing Gathering Center’s separation equipment, by tackling the high water-cut wells, upstream of each GC. The required performances at the outlet of the WKO facility are Oil in Water 100ppmv, Water in Oil 15% volume, liquid carryover in gas 0.1 US gal/MMSCFD, for the water cut ranging from 37.5 to 75% volume. The WKO facility project is used to sustain, support and maintain Greater Burgan production at 1.7 Million Barrels of Oil Per Day (MMBOPD), by handling the increasing water production rate.

Keywords: emulsion, increasing water-cut, production, separation equipment

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Authors: Adriana Muñoz-Talavera, Ana Rosa Rincón-Sánchez, Abraham Escobedo-Moratilla, María Cristina Islas-Carbajal, Miguel Ángel Gómez-Lim

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The highest rates of diabetes incidence and prevalence worldwide will increase the number of diabetic patients requiring insulin or insulin analogues. Then, current production systems would not be sufficient to meet the future market demands. Therefore, developing efficient expression systems for insulin and insulin analogues are needed. In addition, insulin analogues with better pharmacokinetics and pharmacodynamics properties and without mitogenic potential will be required. SCI-57 (single chain insulin-57) is an insulin analogue having 10 times greater affinity to the insulin receptor, higher resistance to thermal degradation than insulin, native mitogenicity and biological effect. Plants as expression platforms have been used to produce recombinant proteins because of their advantages such as cost-effectiveness, posttranslational modifications, absence of human pathogens and high quality. Immunoglobulin production with a yield of 50% has been achieved by transient expression in Nicotiana benthamiana (Nb). The aim of this study is to produce SCI-57 by transient expression in Nb. Methodology: DNA sequence encoding SCI-57 was cloned in pICH31070. This construction was introduced into Agrobacterium tumefaciens by electroporation. The resulting strain was used to infiltrate leaves of Nb. In order to isolate SCI-57, leaves from transformed plants were incubated 3 hours with the extraction buffer therefore filtrated to remove solid material. The resultant protein solution was subjected to anion exchange chromatography on an FPLC system and ultrafiltration to purify SCI-57. Detection of SCI-57 was made by electrophoresis pattern (SDS-PAGE). Protein band was digested with trypsin and the peptides were analyzed by Liquid chromatography tandem-mass spectrometry (LC-MS/MS). A purified protein sample (20µM) was analyzed by ESI-Q-TOF-MS to obtain the ionization pattern and the exact molecular weight determination. Chromatography pattern and impurities detection were performed using RP-HPLC using recombinant insulin as standard. The identity of the SCI-57 was confirmed by anti-insulin ELISA. The total soluble protein concentration was quantified by Bradford assay. Results: The expression cassette was verified by restriction mapping (5393 bp fragment). The SDS-PAGE of crude leaf extract (CLE) of transformed plants, revealed a protein of about 6.4 kDa, non-present in CLE of untransformed plants. The LC-MS/MS results displayed one peptide with a high score that matches SCI-57 amino acid sequence in the sample, confirming the identity of SCI-57. From the purified SCI-57 sample (PSCI-57) the most intense charge state was 1069 m/z (+6) on the displayed ionization pattern corresponding to the molecular weight of SCI-57 (6412.6554 Da). The RP-HPLC of the PSCI-57 shows the presence of a peak with similar retention time (rt) and UV spectroscopic profile to the insulin standard (SCI-57 rt=12.96 and insulin rt=12.70 min). The collected SCI-57 peak had ELISA signal. The total protein amount in CLE from transformed plants was higher compared to untransformed plants. Conclusions: Our results suggest the feasibility to produce insulin analogue SCI-57 by transient expression in Nicotiana benthamiana. Further work is being undertaken to evaluate the biological activity by glucose uptake by insulin-sensitive and insulin-resistant murine and human cultured adipocytes.

Keywords: insulin analogue, mass spectrometry, Nicotiana benthamiana, transient expression

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Authors: Fabio N. Moreno, Letícia B. Marinho, Beatriz D. Ruiz, Maria Helena R. B. Martins

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Brazil is a top consumer of pesticides worldwide, and the São Paulo State is one of the highest consumers among the Brazilian federative states. However, representative data about the occurrence of pesticides in surface waters of the São Paulo State is scarce. This paper aims to present the results of pesticides monitoring executed within the Water Quality Monitoring Network of CETESB (The Environmental Agency of the São Paulo State) between the 2018-2022 period. Surface water sampling points (21 to 25) were selected within basins of predominantly agricultural land-use (5 to 85% of cultivated areas). The samples were collected throughout the year, including high-flow and low-flow conditions. The frequency of sampling varied between 6 to 4 times per year. Selection of pesticide molecules for monitoring followed a prioritizing process from EMBRAPA (Brazilian Agricultural Research Corporation) databases of pesticide use. Pesticides extractions in aqueous samples were performed according to USEPA 3510C and 3546 methods following quality assurance and quality control procedures. Determination of pesticides in water (ng L-1) extracts were performed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) and by gas chromatography with nitrogen phosphorus (GC-NPD) and electron capture detectors (GC-ECD). The results showed higher frequencies (20- 65%) in surface water samples for Carbendazim (fungicide), Diuron/Tebuthiuron (herbicides) and Fipronil/Imidaclopride (insecticides). The frequency of observations for these pesticides were generally higher in monitoring points located in sugarcane cultivated areas. The following pesticides were most frequently quantified above the Aquatic life benchmarks for freshwater (USEPA Office of Pesticide Programs, 2023) or Brazilian Federal Regulatory Standards (CONAMA Resolution no. 357/2005): Atrazine, Imidaclopride, Carbendazim, 2,4D, Fipronil, and Chlorpiryfos. Higher median concentrations for Diuron and Tebuthiuron in the rainy months (october to march) indicated pesticide transport through surface runoff. However, measurable concentrations in the dry season (april to september) for Fipronil and Imidaclopride also indicates pathways related to subsurface or base flow discharge after pesticide soil infiltration and leaching or dry deposition following pesticide air spraying. With exception to Diuron, no temporal trends related to median concentrations of the most frequently quantified pesticides were observed. These results are important to assist policymakers in the development of strategies aiming at reducing pesticides migration to surface waters from agricultural areas. Further studies will be carried out in selected points to investigate potential risks as a result of pesticides exposure on aquatic biota.

Keywords: pesticides monitoring, são paulo state, water quality, surface waters

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Authors: M. O. Bayram, H. B. Gencdal, N. O. Fercan, B. Basbug

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Liquid limit, which is used as a measure of soil strength, can be detected by Casagrande and fall-cone testing methods. The two methods majorly diverge from each other in terms of operator dependency. The Casagrande method that is applied according to ASTM D4318-17 standards may give misleading results, especially if the calibration process is not performed well. To reveal the effect of calibration for drop height and amount of soil paste placement in the Casagrande cup, a series of tests were carried out by multipoint method as it is specified in the ASTM standards. The tests include the combination of 6 mm, 8 mm, 10 mm, and 12 mm drop heights and under-filled, half-filled, and full-filled Casagrande cups by kaolinite samples. It was observed that during successive tests, the drop height of the cup deteriorated; hence the device was recalibrated before and after each test to provide the accuracy of the results. Besides, the tests by under-filled and full-filled samples for higher drop heights revealed lower liquid limit values than the lower drop heights revealed. For the half-filled samples, it was clearly seen that the liquid limit values didn’t change at all as the drop height increased, and this explains the function of standard specifications.

Keywords: calibration, casagrande cup method, drop height, kaolinite, liquid limit, placing form

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Authors: I. Ben Kaddour, S. Larbaoui

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Since their first synthesis in 1984, silicoaluminophosphates have proven their effectiveness as a good adsorbent and catalyst in several environmental and energy applications. In this work, the photocatalytic reaction of the photo-degradation of a pharmaceutical product in water was carried out in the presence of a series of materials based on titanium oxide, anatase phase, supported on the microporous framework of the SAPO4-5 at different levels, under ultraviolet light. These photo-catalysts were characterized by different physicochemical analysis methods in order to determine their structural, textural, and morphological properties, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), microscopy scanning electronics (SEM), nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS). In this study, liquid chromatography coupled with spectroscopy of mass (LC-MS) was used to determine the nature of the intermediate products formed during the photocatalytic degradation of DCF.

Keywords: photocatalysis, titanium dioxide, SAPO-5, diclofenac

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Authors: Seyed Abolhasan Naeini, Mohammad Hossein Zade, E. Izadi, M. Hossein Zade

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The different seismic behavior of liquid storage tanks rather than conventional structures makes their responses more complicated. Uplifting and excessive settlement due to liquid sloshing are the most frequent damages in cylindrical liquid tanks after shell bucking failure modes. As a matter of fact, uses of liquid storage tanks because of the simple construction on compact layer of soil as a foundation are very conventional, but in some cases need to retrofit are essential. The tank seismic behavior can be improved by modifying dynamic characteristic of tank with verifying seismic loads as well as retrofitting and improving base ground. This paper focuses on a typical steel tank on loose, medium and stiff sandy soil and describes an evaluation of displacement of the tank before and after retrofitting. The Abaqus program was selected for its ability to include shell and structural steel elements, soil-structure interaction, and geometrical nonlinearities and contact type elements. The result shows considerable decreasing in settlement and uplifting in the case of retrofitted tank. Also, by increasing shear strength parameter of soil, the performance of the liquid storage tank under the case of seismic load increased.

Keywords: steel tank, soil-structure, sandy soil, seismic load

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Authors: W. Jahouach-Rabai, J. Aribi, Z. Azzouz-Berriche, R. Lahsni, F. Hosni

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Gamma irradiation applied in removing pharmaceutical contaminants from wastewater is an effective advanced oxidation process (AOP), considered as an alternative to conventional water treatment technologies. In this purpose, the degradation efficiency of several detected contaminants under gamma irradiation was evaluated. In fact, radiolysis of organic pollutants in aqueous solutions produces powerful reactive species, essentially hydroxyl radical ( ·OH), able to destroy recalcitrant pollutants in water. Pharmaceuticals considered in this study are aqueous solutions of paracetamol, ibuprofen, and diclofenac at different concentrations 0.1-1 mmol/L, which were treated with irradiation doses from 3 to 15 kGy. The catalytic oxidation of these compounds by gamma irradiation was investigated using hydrogen peroxide (H₂O₂) as a convenient oxidant. Optimization of the main parameters influencing irradiation process, namely irradiation doses, initial concentration and oxidant volume (H₂O₂) were investigated, in the aim to release high degradation efficiency of considered pharmaceuticals. Significant modifications attributed to these parameters appeared in the variation of degradation efficiency, chemical oxygen demand removal (COD) and concentration of radio-induced radicals, confirming them synergistic effect to attempt total mineralization. Pseudo-first-order reaction kinetics could be used to depict the degradation process of these compounds. A sophisticated analytical study was released to quantify the detected radio-induced radicals (electron paramagnetic resonance spectroscopy (EPR) and high performance liquid chromatography (HPLC)). All results showed that this process is effective for the degradation of many pharmaceutical products in aqueous solutions due to strong oxidative properties of generated radicals mainly hydroxyl radical. Furthermore, the addition of an optimal amount of H₂O₂ was efficient to improve the oxidative degradation and contribute to the high performance of this process at very low doses (0.5 and 1 kGy).

Keywords: AOP, COD, hydroxyl radical, EPR, gamma irradiation, HPLC, pharmaceuticals

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Authors: Weiwei Shan, Wenjing Ding, Juan Ning, Chao He, Zijuan Wang

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Gravity circulation loop for the cryopumps of the space simulator is introduced, and two phase mathematic model of flow heat transfer is analyzed as well. Based on this model, the liquid nitrogen (LN₂) gravity circulation loop including its equipment and layout is designed and has served as LN₂ feeding system for cryopumps in one large space simulator. With the help of control software and human machine interface, this system can be operated flexibly, simply, and automatically under four conditions. When running this system, the results show that the cryopumps can be cooled down and maintained under the required temperature, 120 K.

Keywords: cryopumps, gravity circulation loop, liquid nitrogen, two-phase

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Authors: Farideh Tabatabaee Yazdi, Fereshteh Falah, Alireza Vasiee

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Introduction: Gamma-aminobutyric acid (GABA) is a non-protein amino acid that is widely present in organisms. GABA is a kind of pharmacological and biological component and its application is wide and useful. Several important physiological functions of GABA have been characterized, such as neurotransmission and induction of hypotension. GABA is also a strong secretagogue of insulin from the pancreas and effectively inhibits small airway-derived lung adenocarcinoma and tranquilizer. Many microorganisms can produce GABA, and lactic acid bacteria have been a focus of research in recent years because lactic acid bacteria possess special physiological activities and are generally regarded as safe. Among them, the Lb. Brevis produced the highest amount of GABA. The major factors affecting GABA production have been characterized, including carbon sources and glutamate concentration. The use of food industry waste to produce valuable products such as amino acids seems to be a good way to reduce production costs and prevent the waste of food resources. In a dairy factory, a high volume of sludge is produced from a separator that contains useful compounds such as growth factors, carbon, nitrogen, and organic matter that can be used by different microorganisms such as Lb.brevis as carbon and nitrogen sources. Therefore, it is a good source of GABA production. GABA is primarily formed by the irreversible α-decarboxylation reaction of L-glutamic acid or its salts, catalysed by the GAD enzyme. In the present study, this aim was achieved for the fast-growing of Lb.brevis and producing GABA, using the dairy industry sludge as a suitable growth medium. Lactobacillus Brevis strains obtained from Microbial Type Culture Collection (MTCC) were used as model strains. In order to prepare dairy sludge as a medium, sterilization should be done at 121 ° C for 15 minutes. Lb. Brevis was inoculated to the sludge media at pH=6 and incubated for 120 hours at 30 ° C. After fermentation, the supernatant solution is centrifuged and then, the GABA produced was analyzed by the Thin Layer chromatography (TLC) method qualitatively and by the high-performance liquid chromatography (HPLC) method quantitatively. By increasing the percentage of dairy sludge in the culture medium, the amount of GABA increased. Also, evaluated the growth of bacteria in this medium showed the positive effect of dairy sludge on the growth of Lb.brevis, which resulted in the production of more GABA. GABA-producing LAB offers the opportunity of developing naturally fermented health-oriented products. Although some GABA-producing LAB has been isolated to find strains suitable for different fermentations, further screening of various GABA-producing strains from LAB, especially high-yielding strains, is necessary. The production of lactic acid, bacterial gamma-aminobutyric acid, is safe and eco-friendly. The use of dairy industry waste causes enhanced environmental safety. Also provides the possibility of producing valuable compounds such as GABA. In general, dairy sludge is a suitable medium for the growth of Lactic Acid Bacteria and produce this amino acid that can reduce the final cost of it by providing carbon and nitrogen source.

Keywords: GABA, Lactobacillus, HPLC, dairy sludge

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Authors: Zlatina Peteva, Stanislava Georgieva, Mona Stancheva, Lubomir Makedonsky

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Yessotoxins (YTX) and pectenotoxins (PTX) are lipophilic polyether marine biotoxins that accumulate in shellfish and are regulated in the European Union. Aim of this study is investigation of the presence of YTXs and PTXs in Black Sea mussel (Mytilus galloprovincialis) on the North Black Sea cast of Bulgaria. YTX and PTX-2 have been identified in samples of the digestive glands of wild and cultivated samples. Mussel samples are harvested from two locations in important farming area on the Bulgarian North Black Sea coast in the period September 2016 – May 2017. Samples are analyzed by liquid chromatography tandem mass spectrometry (LC–MS/MS). In about 50 % of the samples analyzed the obtained concentration of YTX ranged from 10 – 5000 pg/g hepatopancreas and PTX-2 ranged from 300-7000 pg/g hepatopancreas. This is to our knowledge the first report of occurrence of lipophilic toxins in mussels from Bulgaria.

Keywords: yessotoxins, pectenotoxins, Black sea, mussels

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Authors: Antoinette Maarawi, Zoe Anxionnaz-Minvielle, Pierre Coste, Nathalie Di Miceli Raimondi, Michel Cabassud

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Milli-structured heat exchanger/reactors have been recently widely used, especially in the chemical industry, due to their enhanced performances in heat and mass transfer compared to conventional apparatuses. In our work, the ‘DeanHex’ heat exchanger/reactor with a 2D-meandering channel is investigated both experimentally and numerically. The square cross-sectioned channel has a hydraulic diameter of 2mm. The aim of our study is to model local physico-chemical phenomena (heat and mass transfer, axial dispersion, etc.) for a liquid-liquid two-phase flow in our lab-scale meandering channel, which represents the central part of the heat exchanger/reactor design. The numerical approach of the reactor is based on a 1D model for the flow channel encapsulated in a 3D model for the surrounding solid, using COMSOL Multiphysics V5.5. The use of the 1D approach to model the milli-channel reduces significantly the calculation time compared to 3D approaches, which are generally focused on local effects. Our 1D/3D approach intends to bridge the gap between the simulation at a small scale and the simulation at the reactor scale at a reasonable CPU cost. The heat transfer process between the 1D milli-channel and its 3D surrounding is modeled. The feasibility of this 1D/3D coupling was verified by comparing simulation results to experimental ones originated from two previous works. Temperature profiles along the channel axis obtained by simulation fit the experimental profiles for both cases. The next step is to integrate the liquid-liquid mass transfer model and to validate it with our experimental results. The hydrodynamics of the liquid-liquid two-phase system is modeled using the ‘mixture model approach’. The mass transfer behavior is represented by an overall volumetric mass transfer coefficient ‘kLa’ correlation obtained from our experimental results in the millimetric size meandering channel. The present work is a first step towards the scale-up of our ‘DeanHex’ expecting future industrialization of such equipment. Therefore, a generalized scaled-up model of the reactor comprising all the transfer processes will be built in order to predict the performance of the reactor in terms of conversion rate and energy efficiency at an industrial scale.

Keywords: liquid-liquid mass transfer, milli-structured reactor, 1D/3D model, process intensification

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Authors: M. V. Bartashevich

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The problem of heat transfer at thin laminar liquid film is solved numerically. A thin film of liquid flows down an inclined surface under conditions of variable heat flux on the wall. The use of thin films of liquid allows to create the effective technologies for cooling surfaces. However, it is important to investigate the most suitable cooling regimes from a safety point of view, in order, for example, to avoid overheating caused by the ruptures of the liquid film, and also to study the most effective cooling regimes depending on the character of the distribution of the heat flux on the wall, as well as the character of the blowing of the film surface, i.e., the external shear stress on its surface. In the statement of the problem on the film surface, the heat transfer coefficient between the liquid and gas is set, as well as a variable external shear stress - the intensity of blowing. It is shown that the combination of these factors - the degree of uniformity of the distribution of heat flux on the wall and the intensity of blowing, affects the efficiency of heat transfer. In this case, with an increase in the intensity of blowing, the cooling efficiency increases, reaching a maximum, and then decreases. It is also shown that the more uniform the heating of the wall, the more efficient the heat sink. A separate study was made for the flow regime along the horizontal surface when the liquid film moves solely due to external stress influence. For this mode, the analytical solution is used for the temperature at the entrance region for further numerical calculations downstream. Also the influence of the degree of uniformity of the heat flux distribution on the wall and the intensity of blowing of the film surface on the heat transfer efficiency was also studied. This work was carried out at the Kutateladze Institute of Thermophysics SB RAS (Russia) and supported by FASO Russia.

Keywords: Heat Flux, Heat Transfer Enhancement, External Blowing, Thin Liquid Film

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Authors: Youn Young Shim, Ji Hye Kim, Jae Youl Cho, Martin JT Reaney

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Flaxseed (Linumusitatissimum L.) is gaining popularity in the food industry as a superfood due to its health-promoting properties. Linusorbs (LOs, a.k.a. Cyclolinopeptide) are bioactive compounds present in flaxseed exhibiting potential health effects. The study focused on the effects of processing and storage on the stability of flaxseed-derived LOs added to various bakery products. The flaxseed meal fortified gluten-free (GF) bakery bread was prepared, and the changes of LOs during the bread-making process (meal, fortified flour, dough, and bread) and storage (0, 1, 2, and 4 weeks) at different temperatures (−18 °C, 4 °C, and 22−23 °C) were analyzed by high-performance liquid chromatography-diode array detection. The total oxidative LOs and LO1OB2 were almost kept stable in flaxseed meals at storage temperatures of 22−23 °C, −18 °C, and 4 °C for up to four weeks. Processing steps during GF-bread production resulted in the oxidation of LOs. Interestingly, no LOs were detected in the dough sample; however, LOs appeared when the dough was stored at −18 °C for one week, suggesting that freezing destroyed the sticky structure of the dough and resulted in the release of LOs. The final product, flaxseed meal fortified bread, could be stored for up to four weeks at −18 °C and 4 °C, and for one week at 22−23 °C. All these results suggested that LOs may change during processing and storage and that flaxseed flour-fortified bread should be stored at low temperatures to preserve effective LOs components.

Keywords: linum usitatissimum L., flaxseed, linusorb, stability, gluten-free, peptides, cyclolinopeptide

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Authors: M. Javadzadeh, H. Khoshsima

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In this article, we present a layout printing way for producing Fresnel zone on 1294-1b doped liquid crystal with Methyl-Red azo dye. We made a Fresnel zone mask with 25 zones and radius of 5 mm using lithography technique. With layout printing way, we recorded mask’s pattern on cell with λ=532 nm solid-state diode pump laser. By recording Fresnel zone pattern on cell and making Fresnel pattern on the surface of cell, odd and even zones, will form. The printed pattern, because of Azo dye’s photoisomerization, was permanent. Experimentally, we saw focal length tunability from 32 cm to 43 cm.

Keywords: liquid crystal, lens, Fresnel zone, diffraction, Fresnel lens

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Authors: Masoud Gholam Ale Mohammad, Mojtaba Hafezi Birgani

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An experimental study of saturated pool boiling on a single artificial nucleation site without and with the application of an electric field on the boiling surface has been conducted. N-pentane is boiling on a copper surface and is recorded with a high speed camera providing high quality pictures and movies. The accuracy of the visualization allowed establishing an experimental bubble growth law from a large number of experiments. This law shows that the evaporation rate is decreasing during the bubble growth, and underlines the importance of liquid motion induced by the preceding bubble. Bubble rise is therefore studied: once detached, bubbles accelerate vertically until reaching a maximum velocity in good agreement with a correlation from literature. The bubbles then turn to another direction. The effect of applying an electric field on the boiling surface in finally studied. In addition to changes in the bubble shape, changes are also shown in the liquid plume and the convective structures above the surface. Lower maximum rising velocities were measured in the presence of electric fields, especially with a negative polarity.

Keywords: single and double bubbles, electric field, boiling, rising

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Authors: Tais Basaco, Stefanie Pektor, Josue A. Moreno, Matthias Miederer, Andreas Türler

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Radiopharmaceuticals based in monoclonal anti-body (mAb) via chemical linkers have become a potential tool in nuclear medicine because of their specificity and the large variability and availability of therapeutic radiometals. It is important to identify the conjugation sites and number of attached chelator to mAb to obtain radioimmunoconjugates with required immunoreactivity and radiostability. Girentuximab antibody (G250) is a potential candidate for radioimmunotherapy of clear cell carcinomas (RCCs) because it is reactive with CAIX antigen, a transmembrane glycoprotein overexpressed on the cell surface of most ( > 90%) (RCCs). G250 was conjugated with the bifunctional chelating agent DOTA (1,4,7,10-Tetraazacyclododecane-N,N’,N’’,N’’’-tetraacetic acid) via a benzyl-thiocyano group as a linker (p-SCN-Bn-DOTA). DOTA-G250 conjugates were analyzed by size exclusion chromatography (SE-HPLC) and by electrophoresis (SDS-PAGE). The potential site-specific conjugation was identified by liquid chromatography–mass spectrometry (LC/MS-MS) and the number of linkers per molecule of mAb was calculated using the molecular weight (MW) measured by matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). The average number obtained in the conjugates in non-reduced conditions was between 8-10 molecules of DOTA per molecule of mAb. The average number obtained in the conjugates in reduced conditions was between 1-2 and 3-4 molecules of DOTA per molecule of mAb in the light chain (LC) and heavy chain (HC) respectively. Potential DOTA modification sites of the chelator were identified in lysine residues. The biological activity of the conjugates was evaluated by flow cytometry (FACS) using CAIX negative (SKRC-18) and CAIX positive (SKRC-52). The DOTA-G250 conjugates were labelled with 177Lu with a radiochemical yield > 95% reaching specific activities of 12 MBq/µg. The stability in vitro of different types of radioconstructs was analyzed in human serum albumin (HSA). The radiostability of 177Lu-DOTA-G250 at high specific activity was increased by addition of sodium ascorbate after the labelling. The immunoreactivity was evaluated in vitro and in vivo. Binding to CAIX positive cells (SK-RC-52) at different specific activities was higher for conjugates with less DOTA content. Protein dose was optimized in mice with subcutaneously growing SK-RC-52 tumors using different amounts of 177Lu- DOTA-G250.

Keywords: mass spectrometry, monoclonal antibody, radiopharmaceuticals, radioimmunotheray, renal cancer

Procedia PDF Downloads 307

Authors: Merouani Djilali Redha, F. Abdelmalek, A. A. Addou

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Advanced oxidation processes (AOPs) utilizing Homogenous photocatalysis (Fenton and photo-Fenton reactions), and Heterogeneous photocatalyse (TiO2 and ZnO) were investigated for the degradation of commercial azo dye ‘Orange G’ wastewater. Fenton and photo-Fenton experimental conditions were: Hydrogen peroxide concentration (10-2 M), Ferrous ions concentration (5.10-4 M), pH (2.8 – 3), UV lamp power (6 watt). Adding more ferrous ions enhanced the oxidation rate for the H2O2/Fe2+ and UV/H2O2/Fe2+ processes. The optimum catalyst loading was found 2.0 g.L-1 in our case for both catalysts TiO2 and ZnO. A comparative study of the photocatalytic degradation showed that these two catalysts have a comparable reactivity; it follows a pseudo-first-order kinetics. The degradation trends followed the order: UV365/Fenton > UV365/TiO2 > Solar Fenton > Solar TiO2 > Fenton ~UV365/ZnO. Among AOPs, processes using Fenton type reagent are relatively cheap and easy to operate and maintain. Moreover, UV365/Fenton process has been shown as effective in the treatment of OG dye. Dye was degraded following second-order kinetics. The rate constants was 0,041 .10+6 L.M-1.min-1. The degradation was followed by spectrophotometric method, chemical oxygen demand (COD) measures and high performance liquid chromatography analyses (HPLC). Some aromatic and aliphatic degradation compounds were identified. Degradation of Orange G by UV Fenton mechanism was also proposed.

Keywords: AOPs, homogeneous catalysis, heterogeneous catalysis, acid orange 10, hydroxyl radical

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Authors: Yu-Mei Hsueh, Cheng-Shiuan Tsai, Chao-Yuan Huang

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Prostate Cancer (PC) is a malignant tumor originated in prostate and is a second common male’s cancer in the world. Incidence of PC in Asia countries, have still been rising over the past few decades. As an antioxidant, selenium can slow down prostate cancer tumor progression, but the association between plasma selenium levels and risk of aggressive prostate cancer may be modified by different genotype of selenoprotein. The aim of this study is to determine the relationship between plasma selenium, polymorphism of selenoprotein, urinaty total arsenic, and prostate cancer. Two hundred ninety five pathologically-confirmed cases of PC and 295 cancer-free controls were individually matched to case subjects by age (± 5 years) were recruited from Department of Urology of National Taiwan University Hospital, Taipei Municipal Wan Fang Hospital and Taipei Medical University Hospital. Personal interview and biospeciment of urine and blood collection from participants were conducted by well-trained interviewers after participants’ informed consent was obtained. Plasma selenium was measured by an inductively coupled plasma mass. Urinary arsenic concentration was detected using high-performance liquid chromatography-linked hydride generator and atomic absorption spectrometry. The polymorphism of SEPP1rs3797310 and SEP15 rs5859 were determined using polymerase chain reaction-restriction fragment length polymorphism method. The higher plasma selenium was the lower OR of PC with a dose-response relationship. Prostate cancer patients with high plasma selenium had low tumor stage and grade. Participants carried SEPP1rs3797310 CT+TT genotype compared to those with CC genotype had a lower OR of PC in crude model; then this relationship was disappeared after confounder was adjusted. Prostate cancer patients with high urinary total arsenic concentration had high tumor stage and grade. Urinary total arsenic concentration was significantly positively related with plasma selenium and prostate specific antigen concentration. Participants with lower plasma selenium concentration and higher urinary total arsenic concentration compared to those with higher plasma selenium concentration and lower urinary total arsenic concentration had a higher OR of PC with a dose-response relationship.

Keywords: prostate cancer, plasma selenium concentration, urinary arsenic concentration, prostate specific antigen

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Authors: T. R. Bandara, H. Jaelani, G. J. Griffin

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The conversion of lignocellulosic waste materials, such as sugar cane bagasse, to biofuels such as ethanol has attracted significant interest as a potential element for transforming transport fuel supplies to totally renewable sources. However, the refractory nature of the cellulosic structure of lignocellulosic materials has impeded progress on developing an economic process, whereby the cellulose component may be effectively broken down to glucose monosaccharides and then purified to allow downstream fermentation. Ionic liquid (IL) treatment of lignocellulosic biomass has been shown to disrupt the crystalline structure of cellulose thus potentially enabling the cellulose to be more readily hydrolysed to monosaccharides. Furthermore, conventional hydrolysis of lignocellulosic materials yields byproducts that are inhibitors for efficient fermentation of the monosaccharides. However, selective extraction of monosaccharides from an aqueous/IL phase into an organic phase utilizing a combination of boronic acids and quaternary amines has shown promise as a purification process. Hydrolysis of sugar cane bagasse immersed in an aqueous solution with IL (1-ethyl-3-methylimidazolium acetate) was conducted at different pH and temperature below 100 ºC. It was found that the use of a high concentration of hydrochloric acid to acidify the solution inhibited the hydrolysis of bagasse. At high pH (i.e. basic conditions), using sodium hydroxide, catalyst yields were reduced for total reducing sugars (TRS) due to the rapid degradation of the sugars formed. For purification trials, a supported liquid membrane (SLM) apparatus was constructed, whereby a synthetic solution containing xylose and glucose in an aqueous IL phase was transported across a membrane impregnated with phenyl boronic acid/Aliquat 336 to an aqueous phase. The transport rate of xylose was generally higher than that of glucose indicating that a SLM scheme may not only be useful for purifying sugars from undesirable toxic compounds, but also for fractionating sugars to improve fermentation efficiency.

Keywords: biomass, bagasse, hydrolysis, monosaccharide, supported liquid membrane, purification

Procedia PDF Downloads 254

Authors: Abdessalam Hijab, Hafida Boulekbache, Eric Henry

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The objective of this article is to explain the use of geographic information system (GIS) and information and communication technologies (ICTs) in the real-time processing and analysis of data on the status of an urban sanitation network by integrating professional actors in sanitation for sustainable management in urban areas. Indeed, it is a smart geo-collaboration based on the complementarity of ICTs and GIS. This multi-actor reflection was built with the objective of contributing to the development of complementary solutions to the existing technologies to better protect the urban environment, with the help of a checklist with the spatial reference "E-Géo-LD" dedicated to the "professional/professional" actors in sanitation, for intelligent monitoring of liquid sanitation networks in urban areas. In addition, this research provides a good understanding and assimilation of liquid sanitation schemes in the "Lamkansa" sampling area of the city of Casablanca, and spatially evaluates these schemes. Downstream, it represents a guide to assess the environmental impacts of the liquid sanitation scheme.

Keywords: ICT, GIS, spatial checklist, liquid sanitation, environment

Procedia PDF Downloads 235

Authors: Denis V. Axenov-Gribanov, Irina V. Voytsekhovskaya, Evgenii S. Protasov, Maxim A. Timofeyev

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Isolated ecosystems existing under specific environmental conditions have been shown to be promising sources of new strains of actinobacteria. The taiga forest of Baikal Siberia has not been well studied, and its actinobacterial population remains uncharacterized. The proximity between the huge water mass of Lake Baikal and high mountain ranges influences the structure and diversity of the plant world in Siberia. Here, we report the isolation of eighteen actinobacterial strains from male cones of Pinus sylvestris trees growing on the shore of the ancient Lake Baikal in Siberia. The actinobacterial strains were isolated on solid nutrient MS media and Czapek agar supplemented with cycloheximide and phosphomycin. Identification of actinobacteria was carried out by 16S rRNA gene sequencing and further analysis of the evolutionary history. Four different liquid and solid media (NL19, DNPM, SG and ISP) were tested for metabolite production. The metabolite extracts produced by the isolated strains were tested for antibacterial and antifungal activities. Also, antiradical activity of crude extracts was carried out. Strain Streptomyces sp. IB 2014 I 74-3 that active against Gram-negative bacteria was selected for dereplication analysis with using the high-yield liquid chromatography with mass-spectrometry. Mass detection was performed in both positive and negative modes, with the detection range set to 160–2500 m/z. Data were collected and analyzed using Bruker Compass Data Analysis software, version 4.1. Dereplication was performed using the Dictionary of Natural Products (DNP) database version 6.1 with the following search parameters: accurate molecular mass, absorption spectra and source of compound isolation. Thus, in addition to more common representative strains of Streptomyces, several species belonging to the genera Rhodococcus, Amycolatopsis, and Micromonospora were isolated. Several of the selected strains were deposited in the Russian Collection of Agricultural Microorganisms (RCAM), St. Petersburg, Russia. All isolated strains exhibited antibacterial and antifungal activities. We identified several strains that inhibited the growth of the pathogen Candida albicans but did not hinder the growth of Saccharomyces cerevisiae. Several isolates were active against Gram-positive and Gram-negative bacteria. Moreover, extracts of several strains demonstrated high antioxidant activity. The high proportion of biologically active strains producing antibacterial and specific antifungal compounds may reflect their role in protecting pollen against phytopathogens. Dereplication of the secondary metabolites of the strain Streptomyces sp. IB 2014 I 74-3 was resulted in the fact that a total of 59 major compounds were detected in the culture liquid extract of strain cultivated in ISP medium. Eight compounds were preliminarily identified based on characteristics described in the Dictionary of Natural Products database, using the search parameters Streptomyces sp. IB 2014 I 74-3 was found to produce saframycin A, Y3 and S; 2-amino-3-oxo-3H-phenoxazine-1,8-dicarboxylic acid; galtamycinone; platencin A4-13R and A4-4S; ganefromycin d1; the antibiotic SS 8201B; and streptothricin D, 40-decarbamoyl, 60-carbamoyl. Moreover, forty-nine of the 59 compounds detected in the extract examined in the present study did not result in any positive hits when searching within the DNP database and could not be identified based on available mass-spec data. Thus, these compounds might represent new findings.

Keywords: actinobacteria, Baikal Lake, biodiversity, male cones, Pinus sylvestris

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