Search results for: column chromatography

Authors: Zeineb Ben Salem, Wissem Frikha, Mounir Bouassida

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Liquefaction has been responsible for tremendous amounts of damage in historical earthquakes around the world. The installation of stone columns is widely adopted to prevent liquefaction. Stone columns provide a drainage path, and due to their high permeability, allow for the quick dissipation of earthquake generated excess pore water pressure. Several excess pore pressure generation models in silty sand have been developed and calibrated based on the results of shaking table and centrifuge tests focusing on the effect of silt content on liquefaction resistance. In this paper, the generation and dissipation of excess pore pressure variation of reinforced silty sand by stone columns during liquefaction are analyzedwith different silt content based on test results. In addition, the installation effect of stone columns is investigated. This effect is described by a decrease in horizontal permeability within a disturbed zone around the column. Obtained results show that reduced soil permeability and a larger disturbed zone around the stone column increases the generation of excess pore pressure during the cyclic loading and decreases the dissipation rate after cyclic loading. On the other hand, beneficial effects of silt content were observed in the form of a decrease in excess pore water pressure.

Keywords: stone column, liquefaction, excess pore pressure, silt content, disturbed zone, reduced permeability

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Authors: Jizhi Zhao, Qiliang Zhou, Muxuan Tao

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The calculation of the ultimate loading capacity of composite frame beams is an important step in the design of composite frame structural systems. Currently, the plastic limit theory is mainly used for this calculation in the codes adopted by many countries; however, the effective slab width recommended in most codes is based on the elastic theory, which does not accurately reflect the complex stress mechanism at the beam-column joints in the ultimate loading state. Therefore, the authors’ research group put forward the Compression-on-Column-Face mechanism and Tension-on-Transverse-Beam mechanism to explain the mechanism in the ultimate loading state. Formulae are derived for calculating the effective slab width in composite frames with rectangular/square-section columns under ultimate lateral loading. Moreover, this paper discusses the calculation method of the effective slab width for the beam-end flexural strength of composite frames with circular-section columns. The proposed design formula is suitable for exterior and interior joints. Finally, this paper compares the proposed formulae with available formulae in other literature, current design codes, and experimental results, providing the most accurate results to predict the effective slab width and ultimate loading capacity.

Keywords: composite frame structure, effective slab width, circular-section column, design formulae, ultimate loading capacity

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Authors: Ruchi B. Semwal, Deepak K. Semwal, Thobile A. N. Nkosi, Alvaro M. Viljoen

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The use of Lawsonia inermis L. (Lythraeae), commonly known as henna, has many medicinal benefits and is used as a remedy for the treatment of diarrhoea, cancer, inflammation, headache, jaundice and skin diseases in folk medicine. Although widely used for hair dyeing and temporary tattooing, henna body art has popularized over the last 15 years and changed from being a traditional bridal and festival adornment to an exotic fashion accessory. The naphthoquinone, lawsone, is one of the main constituents of the plant and responsible for its dyeing property. Henna leaves typically contain 1.8–1.9% lawsone, which is used as a marker compound for the quality control of henna products. Adulteration of henna with various toxic chemicals such as p-phenylenediamine, p-methylaminophenol, p-aminobenzene and p-toluenodiamine to produce a variety of colours, is very common and has resulted in serious health problems, including allergic reactions. This study aims to assess the quality of henna products collected from different parts of the world by determining the lawsone content, as well as the concentrations of any adulterants present. Ultra high performance liquid chromatography-mass spectrometry (UPLC-MS) was used to determine the lawsone concentrations in 172 henna products. Separation of the chemical constituents was achieved on an Acquity UPLC BEH C18 column using gradient elution (0.1% formic acid and acetonitrile). The results from UPLC-MS revealed that of 172 henna products, 11 contained 1.0-1.8% lawsone, 110 contained 0.1-0.9% lawsone, whereas 51 samples did not contain detectable levels of lawsone. High performance thin layer chromatography was investigated as a cheaper, more rapid technique for the quality control of henna in relation to the lawsone content. The samples were applied using an automatic TLC Sampler 4 (CAMAG) to pre-coated silica plates, which were subsequently developed with acetic acid, acetone and toluene (0.5: 1.0: 8.5 v/v). A Reprostar 3 digital system allowed the images to be captured. The results obtained corresponded to those from UPLC-MS analysis. Vibrational spectroscopy analysis (MIR or NIR) of the powdered henna, followed by chemometric modelling of the data, indicates that this technique shows promise as an alternative quality control method. Principal component analysis (PCA) was used to investigate the data by observing clustering and identifying outliers. Partial least squares (PLS) multivariate calibration models were constructed for the quantification of lawsone. In conclusion, only a few of the samples analysed contain lawsone in high concentrations, indicating that they are of poor quality. Currently, the presence of adulterants that may have been added to enhance the dyeing properties of the products, is being investigated.

Keywords: Lawsonia inermis, paraphenylenediamine, temporary tattooing, lawsone

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Authors: I. K. Sharma

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Over the years world over system are being developed by research labs continuously monitor under water parameters in the coastal waters of sea such as conductivity, salinity, pressure, temperature, chlorophyll and biological blooms at different levels of water column. The research institutions have developed profilers which are launched by ship connected through cable, glider type profilers following underwater trajectory, buoy any driven profilers, wire guided profilers etc. In all these years, the effect was to design autonomous profilers with no cable quality connection, simple operation and on line date transfer in terms accuracy, repeatability, reliability and consistency. Hence for the Ministry of Communication and Information Technology, India sponsored research project to National Institute of Oceanography, GOA, India to design and develop autonomous vertical profilers, it has taken system and AVP has been successfully developed and tested.

Keywords: oceanography, water column, autonomous profiler, buoyancy

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Authors: Mahacine Amrani

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This paper aims at reviewing some Moroccan industrial applications of wavelet especially in the dynamic identification of a process model using Haar wavelet mother response. Two recent Moroccan study cases are described using dynamic data originated by a distillation column and an industrial polyethylene process plant. The purpose of the wavelet scheme is to build on-line dynamic models. In both case studies, a comparison is carried out between the Haar wavelet mother response model and a linear difference equation model. Finally it concludes, on the base of the comparison of the process performances and the best responses, which may be useful to create an estimated on-line internal model control and its application towards model-predictive controllers (MPC). All calculations were implemented using AutoSignal Software.

Keywords: process performance, model, wavelets, Haar, Moroccan

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Authors: Mansour H. Alkmim, Adriano T. Fabro, Marcus V. G. De Morais

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In this paper, a global direct search optimization algorithm to reduce vibration of a tuned liquid column damper (TLCD), a class of passive structural control device, is presented. The objective is to find optimized parameters for the TLCD under stochastic load from different wind power spectral density. A verification is made considering the analytical solution of an undamped primary system under white noise excitation. Finally, a numerical example considering a simplified wind turbine model is given to illustrate the efficacy of the TLCD. Results from the random vibration analysis are shown for four types of random excitation wind model where the response PSDs obtained showed good vibration attenuation.

Keywords: generalized pattern search, parameter optimization, random vibration analysis, vibration suppression

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Authors: Stanley Ibuchukwu Onwukwe

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Most reservoir in mature oil fields are vulnerable to challenges of water and/or gas coning as the size of their oil column reduces due to long period of oil production. These often result to low oil production and excessive water and/or gas production. Since over 50 years of oil production in the Niger delta, it is apparent that most of the oil fields in the region have reached their mature stages, thereby susceptible to coning tendencies. As a result of these, a good number of wells have been shut-in and abandoned, with significant amount of oil left unproduced. Analysis of the movement of fluid contacts in the reservoir is a significant aspect of reservoir studies and can assist in the management of coning tendencies and production performance of reservoirs in a mature field. This study, therefore, seeks to evaluate the occurrence of coning through the movement of fluid contacts (GOC and OWC) and determine the critical rate for controlling coning tendencies in mature oil field. This study applies the principle of Nodal analysis to calibrate the thin oil column of a reservoir of a mature field, and was graphically evaluated using the Joshi’s equation of critical rate for gas-oil system and oil-water system respectively. A representative Proxy equation was developed and sensitivity analysis carried out to determine the trend of critical rate as the oil column is been depleted. The result shows the trend in the movement of the GOC and OWC, and the critical rate, beyond which will result in excessive water and gas production, resulting to decreasing oil production from the reservoir. This result of this study can be used as a first pass assessment in the development of mature oil field reservoirs anticipated to experience water and/or gas coning during production.

Keywords: coning, fluid contact movement, mature oil field, oil production

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Authors: Alexandre Gonzalez, Zohra Benfodda, David Bénimélis, Jean-Xavier Fontaine, Roland Molinié, Patrick Meffre

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Volatile organic compounds (VOCs) emitted by flowers play an important role in plant ecology. However, the Tillandsia genus has been scarcely studied according to the VOCs emitted by flowers. Tillandsia are epiphytic flowering plants belonging to the Bromeliaceae family. The VOCs composition of twelve unscented and two faint-scented Tillandsia species was studied. The headspace solid phase microextraction coupled with gas chromatography combined with mass spectrometry method was used to explore the chemical diversity of the VOCs. This study allowed the identification of 65 VOCs among the fourteen species, and between six to twenty-five compounds were identified in each of the species.

Keywords: tillandsia, headspace solid phase microextraction (HS-SPME), gas chromatography-mass spectrometry (GC-MS), scentless flowers, volatile organic compounds (VOCs), PCA analysis, heatmap

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Authors: Mariane G. Tadros, Shahira M. Ezzat, Maha M. Salama, Mohamed A. Farag

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In this study, the in vitro anticholinesterase activity of the volatile oils of both O. basilicum and O. africanum was investigated and both samples showed significant activity. As a result, the major constituents of the two oils were isolated using several column chromatography. Linalool, 1,8-cineol and eugenol were isolated from the volatile oil of O. basilicum and camphor was isolated from the volatile oil of O. africanum. The anticholinesterase activity of the isolated compounds were also evaluated where 1,8-cineol showed the highest inhibitory activity followed by camphor. To confirm these activities, learning and memory enhancing effects were tested in mice. Memory impairment was induced by scopolamine, a cholinergic muscarinic receptor antagonist. Anti-amnesic effects of both volatile oils and their terpenoids were investigated by the passive avoidance task in mice. We also examined their effects on brain acetylcholinesterase activity. Results showed that scopolamine-induced cognitive dysfunction was significantly attenuated by administration of the volatile oils and their terpenoids, eugenol and camphor, in the passive avoidance task and inhibited brain acetylcholinesterase activity. These results suggest that O. basilicum and O. africanum volatile oils can be good candidates for further studies on Alzheimer’s disease via their acetylcholinesterase inhibitory actions.

Keywords: Ocimum baselicum, Ocimum africanum, GC/MS analysis, anticholinesterase

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Authors: Jeong Woo Kang, MiYoung Baek, Ki-Suk Kim, Kwang-Jick Lee, ByungJae So

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Introduction: A fast, easy and sensitive detection method was developed and validated by liquid chromatography tandem mass spectrometry for the determination of marbofloxacin in pig plasma which was further applied to study the pharmacokinetics of marbofloxacin. Materials and Methods: The plasma sample (500 μL) was mixed with 1.5 ml of 0.1% formic acid in MeCN to precipitate plasma proteins. After shaking for 20 min, The mixture was centrifuged at 5,000 × g for 30 min. It was dried under a nitrogen flow at 50℃. 500 μL aliquot of the sample was injected into the LC-MS/MS system. Chromatographic analysis was carried out mobile phase gradient consisting 0.1% formic acid in D.W. (A) and 0.1% formic acid in MeCN (B) with C18 reverse phase column. Mass spectrometry was performed using the positive ion mode and the selected ion monitoring (MRM). Results and Conclusions: The method validation was performed in the sample matrix. Good linearities (R2>0.999) were observed and the quantified average recoveries of marbofloxacin were 87 - 92% at level of 10 ng g-1 -100 ng g-1. The percent of coefficient of variation (CV) for the described method was less than 10 % over the range of concentrations studied. The limits of detection (LOD) and quantification (LOQ) were 2 and 5 ng g-1, respectively. This method has also been applied successfully to pharmacokinetic analysis of marbofloxacin after intravenous (IV), intramuscular (IM) and oral administration (PO). The mean peak plasma concentration (Cmax) was 2,597 ng g-1at 0.25 h, 2,587 ng g-1at 0.44 h and 2,355 ng g-1at 1.58 h for IV, IM and PO, respectively. The area under the plasma concentration-time curve (AUC0–t) was 24.8, 29.0 and 25.2 h μg/mL for IV, IM and PO, respectively. The elimination half-life (T1/2) was 8.6, 13.1 and 9.5 for IV, IM and PO, respectively. Bioavailability (F) of the marbofloxacin in pig was 117 and 101 % for IM and PO, respectively. Based on these result, marbofloxacin does not have any obstacles as therapeutics to develop the oral formulations such as tablets and capsules.

Keywords: marbofloxacin, LC-MS/MS, pharmacokinetics, chromatographic

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Authors: Kajetan Deja, Katarzyna Draganska-Deja, Mateusz Ormanczyk, Michał Procajlo

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Two glaciated fjords on Spitsbergen (Hornsund 77°N) and Kongsfjorden (79°N) were studied for the occurrence of macroplankton (mostly euphausids, hyperiids, chaetognaths) with the use of drop down the camera. The underwater imagery demonstrates that closer to the glacier front, where turbid and freshwater occurs, most of the macroplankters leave the upper water column and descends to the bottom (about 100m depth). Concentrations of macroplankton in the immediate vicinity of the sediment reach over 500 specimens per m² - what corresponds to the biomass of 10g C/m³. Such concentrations of macroplankton are of prime interest for fish, seals and other carnivores. Conditions in the near-bottom waters are in many respects better than in the upper water column- better oxygenated, cold, fully saline and transparent waters with rich food deposited on the seabed from the surface (sinking microplankton). We suggest that near bottom occurrence of macroplankton is related to the increase of glacier melt and freshwater discharge intensity.

Keywords: arctic, ecosystem, fjords, Krill

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Authors: M. François, L. Sigot, C. Vallières

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Volatile Organic Compounds (VOCs) are a real health issue, particularly in domestic indoor environments. Among these VOCs, acetaldehyde is frequently monitored in dwellings ‘air, especially due to smoking and spontaneous emissions from the new wall and soil coverings. It is responsible for respiratory complaints and is classified as possibly carcinogenic to humans. Adsorption processes are commonly used to remove VOCs from the air. Metal-Organic Frameworks (MOFs) are a promising type of material for high adsorption performance. These hybrid porous materials composed of metal inorganic clusters and organic ligands are interesting thanks to their high porosity and surface area. The HKUST-1 (also referred to as MOF-199) is a copper-based MOF with the formula [Cu₃(BTC)₂(H₂O)₃]n (BTC = benzene-1,3,5-tricarboxylate) and exhibits unsaturated metal sites that can be attractive sites for adsorption. The objective of this study is to investigate the impact of HKUST-1 pretreatment on acetaldehyde adsorption. Thus, dynamic adsorption experiments were conducted in 1 cm diameter glass column packed with 2 cm MOF bed height. MOF were sieved to 630 µm - 1 mm. The feed gas (Co = 460 ppmv ± 5 ppmv) was obtained by diluting a 1000 ppmv acetaldehyde gas cylinder in air. The gas flow rate was set to 0.7 L/min (to guarantee a suitable linear velocity). Acetaldehyde concentration was monitored online by gas chromatography coupled with a flame ionization detector (GC-FID). Breakthrough curves must allow to understand the interactions between the MOF and the pollutant as well as the impact of the HKUST-1 humidity in the adsorption process. Consequently, different MOF water content conditions were tested, from a dry material with 7 % water content (dark blue color) to water saturated state with approximately 35 % water content (turquoise color). The rough material – without any pretreatment – containing 30 % water serves as a reference. First, conclusions can be drawn from the comparison of the evolution of the ratio of the column outlet concentration (C) on the inlet concentration (Co) as a function of time for different HKUST-1 pretreatments. The shape of the breakthrough curves is significantly different. The saturation of the rough material is slower (20 h to reach saturation) than that of the dried material (2 h). However, the breakthrough time defined for C/Co = 10 % appears earlier in the case of the rough material (0.75 h) compared to the dried HKUST-1 (1.4 h). Another notable difference is the shape of the curve before the breakthrough at 10 %. An abrupt increase of the outlet concentration is observed for the material with the lower humidity in comparison to a smooth increase for the rough material. Thus, the water content plays a significant role on the breakthrough kinetics. This study aims to understand what can explain the shape of the breakthrough curves associated to the pretreatments of HKUST-1 and which mechanisms take place in the adsorption process between the MOF, the pollutant, and the water.

Keywords: acetaldehyde, dynamic adsorption, HKUST-1, pretreatment influence

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Authors: Naureen Akhtar

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The stability of the protein in detergent-containing solution is the key for its successful crystallisation. Fluorescence-detection size-exclusion chromatography (FSEC) is a potential approach for screening monodispersity as well as the stability of protein in a detergent-containing-solution. In this present study, covalently linked Green Fluorescent Protein (GFP) to bacterial nitrate transporter, NarU from Escherichia coli was studied for pre-crystallisation trials by FSEC. Immobilised metal ion affinity chromatography (IMAC) and gel filtration were employed for their purification. The main objectives of this study were over-expression, detergent screening and crystallisation of nitrate transporter proteins. This study could not produce enough proteins that could realistically be taken forward to achieve the objectives set for this particular research. In future work, different combinations of variables like vectors, tags, creation of mutant proteins, host cells, position of GFP (N- or C-terminal) and/or membrane proteins would be tried to determine the best combination as the principle of technique is still promising.

Keywords: transporters, detergents, over-expression, crystallography

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Authors: Khalid S. Hashim, Andy Shaw, Rafid Alkhaddar

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Dissolved oxygen (DO) plays a key role in the electrocoagulation process (EC) as it oxidizes the heavy metals, ammonia, and cyanide into other forms that can be removed easily from water. Hence, many of the previous investigations used external aerators to provide the required DO inside EC reactors, especially when the water being treated had a low DO (such as leachate and high organic content waters), or when the DO depleted during the EC treatment. Although the external aeration process effectively enhances the DO concentration, it has a significant impact on energy consumption. Thus, the present project aims to fill a part of this gap in the literature by an innovative use of perforated flow columns in the design of an EC reactor (ECR1). In order to investigate the performance of ECR1, water samples with a controlled DO concentration were pumped at different flow rates (110, 220, and 440 ml/min) to the ECR1 for 10 min. The obtained results demonstrated that the ECR1 increased the DO concentration from 5.0 to 9.54, 10.53, and 11.0 mg/L, which is equivalent to 90.8%, 110.6%, and 120% at flow rates of 110, 220, and 440 mL/min respectively.

Keywords: flow column, electrocoagulation, dissolved oxygen, water treatment

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Authors: Sanja Jovanovic, Aleksandar Simic, Ognjan Skrobic, Dragan Masulovic, Aleksandra Djuric-Stefanovic

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Introduction: Achalasia is an idiopathic primary esophageal motility disorder characterized by esophageal peristalsis and impaired swallow-induced relaxation of the lower esophageal sphincter (LES). It is a rare disease that affects both genders with an incidence of 1/100.000 and a prevalence rate of 10/100,000 per year. Objective: Laparoscopic Heller myotomy (LHM) represents a therapy of choice for patients with achalasia, providing excellent outcomes. The aim of this study was to evaluate the significance of computed tomography (CT) in analyzing achalasia subtypes and timed barium esophagogram (TBE) in evaluation of LHM success, as a part of standardized diagnostic protocol. Method: Fifty-one patients with achalasia, confirmed by manometric studies, in addition to standardized diagnostic methods, underwent CT and TBE. CT was done with multiplanar reconstruction, measuring the wall thickness above the esophago-gastric junction in the axial plane. TBE was performed preoperatively and two days postoperatively swallowing low-density barium sulfate, and plane upright frontal films were performed 1, 2 and 5 minutes after the ingestion. In all patients, LHM was done, and pre and postoperative height and weight of the barium column were compared. Results: According to CT findings we divided patients into 3 subtypes of achalasia according to wall thickness: < 4mm as subtype one, between 4 - 9mm as II, and > 10 mm as subtype 3. Correlation of manometric results, as a reference values, and CT findings indicated CT sensitivity of 90% and specificity of 70 % in establishing subtypes of achalasia. The preoperative values of TBE at 1, 2 and 5 minutes were: median barium column height 17.4 ± 7.4, 15.9 ± 6.2 and 13.9 ± 6.2 cm; median column width 5 ± 1.5, 4.7 ± 1.6 and 4.5 ± 1.8 cm respectively. LHM significantly reduced these values (height 7 ± 4.6, 5.8 ± 4.2, 3.7 ± 3.4 cm; width 2.9 ± 1.3, 2.6 ± 1.3 and 2.4 ± 1.4 cm), indicating the quantitative estimates of emptying as excellent (p value < 0.01). Conclusion: CT has high sensitivity and specificity in evaluation of achalasia subtypes, and can be introduced as an additional method for standardized evaluation of these patients. The quantitative assessment of TBE based on measurements of the barium column is an accurate and beneficial method, which adequately estimates esophageal emptying success of LHM.

Keywords: achalasia, computed tomography, esophagography, myotomy

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Authors: Abdulkadir Cuneyt Aydin, Mahyar Maali, Mahmut Kılıç, Merve Sağıroğlu

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The moment-rotation curves of semi-rigid connections are the visual expressions of the actual behaviour discovered in beam-to-column connections experiments. This research was to determine the behaviour of the connection using full-scale experiments under statically loaded. The stiffeners which are typically attached to beams web or flanges to control local buckling and to increase shear capacity in a beam web are almost always used in modern designs. They must also provide sufficient moment of inertia to control out of plane deformations. This study was undertaken to analyse the influence of stiffeners in the angles and beams on the behaviour of the beam-to-column joints. In addition, the aim was to provide necessary data to improve the Eurocode 3. The main parameters observed are the evolution of the resistance, the stiffness, the rotation capacity, the ductility of a joint and the Energy Dissipation. Experimental tests show that the plastic flexural resistance and the energy dissipation increased when thickness of stiffener beam, thickness of stiffener angles were increased in the test specimens. And also, while stiffness of joints, the bending moment capacity and the maximum bending moment increased with the increasing thickness of stiffener beam, these values decreased with the increasing thickness of stiffener angles. So, it is observed that the beam stiffener of angles are important in improving resistance moment of beam-to-column semi-rigid joints.

Keywords: bolted angles connection, semi-rigid joints, ductility of a joint, angles and beams stiffeners

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Authors: Sumonthip Kongtun Janphuk

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Ten cereal grains that usually used as ingredients in healthy products were studied for phytosteryl glucoside contents. β-sitosteryl glucoside in 10 cereal grains, including Phasecolus vulgaris L. (kidney bean), Sorghum bicolor (sorghum), Moringa oleifera Lam. (drumstick), Nelumbo nucifera (lotus), Vigna radiate L. (mung bean), Coix lacrymajobi (job’tears), Oryza sativa. (red rice), Glycine max L. Merrill. (soybean),Cucurbita maschata Decne (pumpkin) and Helianthas annuus (sunflower seeds), were analyzed using Thin-layer chromatography (TLC) and High-Performance liquid chromatography (HPLC). All grains were extracted with methanol before analysis. Red bean showed the maximum phytosteryl glucoside content of 0.42% w/w. The content of others were as follows: pumpkin seed 0.173%, mung bean 0.099 %, soybean 0.07%, dried moringa seed 0.067%, lotus seed 0.044%, sorghum 0.032%, sunflower seed 0.016%, Job's tears 0.012%, and brown rice 0.006%.

Keywords: cereal grains, phytosterol, β-sitosteryl glucoside, food analysis.

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Authors: Rowan Moore, Kai Scheffler, Eugen Damoc, Jennifer Sutton, Aaron Bailey, Stephane Houel, Simon Cubbon, Jonathan Josephs

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Purpose: MS analysis of monoclonal antibodies (mAbs) at the protein and peptide levels is critical during development and production of biopharmaceuticals. The compositions of current generation therapeutic proteins are often complex due to various modifications which may affect efficacy. Intact proteins analyzed by MS are detected in higher charge states that also provide more complexity in mass spectra. Protein analysis in native or native-like conditions with zero or minimal organic solvent and neutral or weakly acidic pH decreases charge state value resulting in mAb detection at higher m/z ranges with more spatial resolution. Methods: Three commercially available mAbs were used for all experiments. Intact proteins were desalted online using size exclusion chromatography (SEC) or reversed phase chromatography coupled on-line with a mass spectrometer. For streamlined use of the LC- MS platform we used a single SEC column and alternately selected specific mobile phases to perform separations in either denaturing or native-like conditions: buffer A (20 % ACN, 0.1 % FA) with Buffer B (100 mM ammonium acetate). For peptide analysis mAbs were proteolytically digested with and without prior reduction and alkylation. The mass spectrometer used for all experiments was a commercially available Thermo Scientific™ hybrid Quadrupole-Orbitrap™ mass spectrometer, equipped with the new BioPharma option which includes a new High Mass Range (HMR) mode that allows for improved high mass transmission and mass detection up to 8000 m/z. Results: We have analyzed the profiles of three mAbs under reducing and native conditions by direct infusion with offline desalting and with on-line desalting via size exclusion and reversed phase type columns. The presence of high salt under denaturing conditions was found to influence the observed charge state envelope and impact mass accuracy after spectral deconvolution. The significantly lower charge states observed under native conditions improves the spatial resolution of protein signals and has significant benefits for the analysis of antibody mixtures, e.g. lysine variants, degradants or sequence variants. This type of analysis requires the detection of masses beyond the standard mass range ranging up to 6000 m/z requiring the extended capabilities available in the new HMR mode. We have compared each antibody sample that was analyzed individually with mixtures in various relative concentrations. For this type of analysis, we observed that apparent native structures persist and ESI is benefited by the addition of low amounts of acetonitrile and formic acid in combination with the ammonium acetate-buffered mobile phase. For analyses on the peptide level we analyzed reduced/alkylated, and non-reduced proteolytic digests of the individual antibodies separated via reversed phase chromatography aiming to retrieve as much information as possible regarding sequence coverage, disulfide bridges, post-translational modifications such as various glycans, sequence variants, and their relative quantification. All data acquired were submitted to a single software package for analysis aiming to obtain a complete picture of the molecules analyzed. Here we demonstrate the capabilities of the mass spectrometer to fully characterize homogeneous and heterogeneous therapeutic proteins on one single platform. Conclusion: Full characterization of heterogeneous intact protein mixtures by improved mass separation on a quadrupole-Orbitrap™ mass spectrometer with extended capabilities has been demonstrated.

Keywords: disulfide bond analysis, intact analysis, native analysis, mass spectrometry, monoclonal antibodies, peptide mapping, post-translational modifications, sequence variants, size exclusion chromatography, therapeutic protein analysis, UHPLC

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Authors: Jae Gon Kim, Yongchan Cho, Jungwha Lee

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Acid rock drainage (ARD) is generated by the oxidation of pyrite (FeS₂) contained in the excavated rocks upon its exposure to atmosphere and is an environmental concern at construction site due to its high acidity and high concentration of toxic elements. We developed the safe disposal method with the reduction of ARD generation by an alkali phosphate treatment. A pyrite rich andesite was collected from a railway construction site. The collected rock sample was crushed to be less than 3/8 inches in diameter using a jaw crusher. The crushed rock was filled in an acryl tube with 20 cm in diameter and 40 cm in height. Two treatments for the ARD reduction were conducted with duplicates: 1) the addition of 10mM KH₂PO₄_3% NaHCO₃ and 2) the addition of 10mM KH₂PO₄_3% NaHCO₃ and ordinary portland cement (OPC) on the top of the column. After the treatments, 500 ml of distilled water added to each column for every week for 3 weeks and then the column was flushed with 1,500 ml of distilled water in the 4th week. The pH, electrical conductivity (EC), concentrations of anions and cations of the leachates were monitored for 10 months. The pH of the leachates from the untreated column showed 2.1-3.7, but the leachates from the columns treated with the alkali phosphate solution with or without the OPC addition showed pH 6.7–8.9. The leachates from the treated columns had much lower concentrations of SO₄²⁻ and toxic elements such as Al, Mn, Fe and heavy metals than those from the untreated columns. However, the leachates from the treated columns had a higher As concentration than those from the untreated columns. There was no significant difference in chemical property between the leachates from the treated columns with and without the OPC addition. The chemistry of leachates indicates that the alkali phosphate treatment decreased the oxidation of sulfide and neutralized the acidic pore water. No significant effect of the OPC addition on the leachate chemistry has shown during 10-month experiment. However, we expect a positive effect of the OPC addition on the reduction of ARD generation in terms of long period. According to the results of this experiment, the alkali phosphate treatment of sulfide rich rock can be a promising technology for the safe disposal method with the ARD reduction.

Keywords: acid rock drainage, alkali phosphate treatment, pyrite rich rock, safe disposal

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Authors: Nabil Jallouli, Luisa M. Pastrana-Martínez, Ana R. Ribeiro, Nuno F. F. Moreira, Joaquim L. Faria, Olfa Hentati, Adrián M. T. Silva, Mohamed Ksibi

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Degradation and mineralization of ibuprofen (IBU) were investigated using Ultraviolet (UV) Light Emitting Diodes (LEDs) in TiO2 photocatalysis. Samples of ultrapure water (UP) and a secondary treated effluent of a municipal wastewater treatment plant (WWTP), both spiked with IBU, as well as a highly concentrated IBU (230 mgL-1) pharmaceutical industry wastewater (PIWW), were tested in the TiO2/UV-LED system. Three operating parameters, namely, pH, catalyst load and number of LEDs were optimized. The process efficiency was evaluated in terms of IBU removal using high performance liquid chromatography (HPLC) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Additionally, the mineralization was investigated by determining the dissolved organic carbon (DOC) content. The chemical structures of transformation products were proposed based on the data obtained using liquid chromatography with a high resolution mass spectrometer ion trap/time-of-flight (LC-MS-IT-TOF). A possible pathway of IBU degradation was accordingly proposed. Bioassays were performed using the marine bacterium Vibrio fischeri to evaluate the potential acute toxicity of original and treated wastewaters. TiO2 heterogeneous photocatalysis was efficient to remove IBU from UP and from PIWW, and less efficient in treating the wastewater from the municipal WWTP. The acute toxicity decreased by ca. 40% after treatment, regardless of the studied matrix.

Keywords: acute toxicity, Ibuprofen, UV-LEDs, wastewaters

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Authors: Erhan Zor, Funda Copur, Asli I. Dogan, Haluk Bingol

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Current trends in the wide-scale sensing technologies rely on the development of miniaturized, rapid and easy-to-use sensing platforms. Quantum dots (QDs) with strong and easily tunable luminescence and high emission quantum yields have become a well-established photoluminescent nanomaterials for sensor applications. Although the majority of the reports focused on the cadmium-based QDs which have toxic effect on biological systems and eventually would cause serious environmental problems, carbon-based quantum dots (CQDs) that do not contain any toxic class elements have attracted substantial research interest in recent years. CQDs are small carbon nanostructures (less than 10 nm in size) with various unique properties and are widely-used in different fields during the last few years. In this respect, chiral nanostructures have become a promising class of materials in various areas such as pharmacology, catalysis, bioanalysis and (bio)sensor technology due to the vital importance of chirality in living systems. We herein report the synthesis of chiral CQDs with D- or L-tartaric acid as precursor materials. The optimum experimental conditions were examined and the purification procedure was performed using ethanol/water by column chromatography. The purified chiral CQDs were characterized by UV-Vis, FT-IR, XPS, PL and TEM techniques. The resultants display different photoluminescent characteristics due to the size and conformational difference. Considering the results, it can be concluded that chiral CQDs is expected to be used as optical chiral sensor in different platforms.

Keywords: carbon quantum dots, chirality, sensor, tartaric acid

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Authors: Filip Buruiana, Alexander Hall, Reimar Hofmann, Thomas Hofmann, Silviu Ganceanu, Alexandru Tudorica

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In-memory column-stores make interactive analysis feasible for many big data scenarios. PowerDrill is a system used internally at Google for exploration in logs data. Even though it is a highly parallelized column-store and uses in memory caching, interactive response times cannot be achieved for all datasets (note that it is common to analyze data with 50 billion records in PowerDrill). In this paper, we investigate two orthogonal approaches to optimize performance at the expense of an acceptable loss of accuracy. Both approaches can be implemented as outer wrappers around existing database engines and so they should be easily applicable to other systems. For the first optimization we show that memory is the limiting factor in executing queries at speed and therefore explore possibilities to improve memory efficiency. We adapt some of the theory behind data sketches to reduce the size of particularly expensive fields in our largest tables by a factor of 4.5 when compared to a standard compression algorithm. This saves 37% of the overall memory in PowerDrill and introduces a 0.4% relative error in the 90th percentile for results of queries with the expensive fields. We additionally evaluate the effects of using sampling on accuracy and propose a simple heuristic for annotating individual result-values as accurate (or not). Based on measurements of user behavior in our real production system, we show that these estimates are essential for interpreting intermediate results before final results are available. For a large set of queries this effectively brings down the 95th latency percentile from 30 to 4 seconds.

Keywords: big data, in-memory column-store, high-performance SQL queries, approximate SQL queries

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Authors: Geetanjali Yadav, Arpit Mishra, Parthsarathi Ghosh, Ramkrishna Sen

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The world is facing problems of increasing global CO2 emissions, climate change and fuel crisis. Therefore, several renewable and sustainable energy alternatives should be investigated to replace non-renewable fuels in future. Algae presents itself a versatile feedstock for the production of variety of fuels (biodiesel, bioethanol, bio-hydrogen etc.) and high value compounds for food, fodder, cosmetics and pharmaceuticals. Microalgae are simple microorganisms that require water, light, CO2 and nutrients for growth by the process of photosynthesis and can grow in extreme environments, utilize waste gas (flue gas) and waste waters. Mixing, however, is a crucial parameter within the culture system for the uniform distribution of light, nutrients and gaseous exchange in addition to preventing settling/sedimentation, creation of dark zones etc. The overarching goal of the present study is to improve photobioreactor (PBR) design for enhancing dissolution of CO2 from ambient air (0.039%, v/v), pure CO2 and coal-fired flue gas (10 ± 2%) into microalgal PBRs. Computational fluid dynamics (CFD), a state-of-the-art technique has been used to solve partial differential equations with turbulence closure which represents the dynamics of fluid in a photobioreactor. In this paper, the hydrodynamic performance of the PBR has been characterized and compared with that of the conventional bubble column PBR using CFD. Parameters such as flow rate (Q), mean velocity (u), mean turbulent kinetic energy (TKE) were characterized for each experiment that was tested across different aeration schemes. The results showed that the modified PBR design had superior liquid circulation properties and gas-liquid transfer that resulted in creation of uniform environment inside PBR as compared to conventional bubble column PBR. The CFD technique has shown to be promising to successfully design and paves path for a future research in order to develop PBRs which can be commercially available for scale-up microalgal production.

Keywords: computational fluid dynamics, microalgae, bubble column photbioreactor, flue gas, simulation

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Authors: Raudone Lina, Raudonis Raimondas, Liaudanskas Mindaugas, Pukalskas Audrius, Viskelis Pranas, Janulis Valdimaras

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Human health fortification, its protection and disease prophylaxis are the main problems of the health care systems. Plant origin materials and their preparations are applied for the prevention of the common diseases. Oxidative stress takes part in the pathogenesis of many autoimmune, neurodegenerative, tumor and ageing processes. The antioxidants are able to protect the human body from the free radicals and to stop the progression of numerous chronic diseases. The research of plant origin materials is relevant for the search of natural antioxidants. A group of compounds that gained scientific attention due to antioxidant properties and effects on human health are phenolic compounds. Phenolic compounds are widely abundant in various parts of plants, i.e. leaves, stems, roots, flowers and fruits. Most commonly consumed fruits all over the world are apples. It is very important to analyze the antioxidant activity of apples as they are extensively used in the prevention of various diseases. The aim of this study was to determine the antioxidant profiles of Malus domestica Borkh fruit cultivars (Aldas, Auksis, Connel Red, Ligol, Lodel, Rajka) and to identify the phenolic compounds with potent contribution to antioxidant activity. Nineteen constituents were identified in apple cultivars using ultra high performance liquid chromatography coupled to quadruple and time-of-flight mass spectrometers (UPLC–QTOF–MS). Phytochemical profile was constituted of phenolic acids, procyanidins, quercetin derivatives and dihydrochalcones. Reducing and radical scavenging activities of individual constituents were determined using high performance liquid chromatography (HPLC) coupled to post-column FRAP and ABTS assay, respectively. Significant differences of total radical scavenging and reducing activity (expressed as trolox equivalents, TE µmol/g) were determined between the investigated cultivars. Chlorogenic acid and complex of procyanidins were the main contributors to antioxidant activity determining up to 35 % and 55 % of total TE values, respectively. Determined phenolic composition and antioxidant activity significantly depend on apple cultivars. It is important to determine the individual compounds that are significant for antioxidant activity and that could be investigated in vivo systems. The identification of the antioxidants provides information for the further research of standardized extracts that could be used for pharmaceutical preparations with specific phenolic traits.

Keywords: FRAP, ABTS, antioxidant, phenolic, apples, chlorogenic acid

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Authors: Tiah Rachmatiah, Subaryanti

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Plants of Lauraceae family are known to contain many chemical compounds which have potential bioactivity such as alkaloids, flavonoids, lactones, terpenes, etc. Actinodaphne macrophylla and Nectandra angustifolia are two species from Lauraceae. A previous study on the crude alkaloidal extract from the bark of Act. macrophylla and n-hexane extract from the bark of N. angustifolia showed antiplasmodial activity against Plasmodium falciparum. The study was continued to find antiplasmodial active compounds from the two extracts. The materials were obtained from Bogor Botanical Garden, West Java, Indonesia. Crude alkaloidal extract of Act. macrophylla was prepared by maceration in dichloromethane after moistened with NH4OH 25% and n-hexane extract of N. angustifolia was prepared by maceration in n-hexane. A major compound was isolated by column chromatography using silica gel and a mixture of CH2Cl2 and methanol as a gradient solvent system for the alkaloidal extract and mixture of n-hexane and ethyl acetate for n-hexane extract. Fine white needle crystals were obtained from the alkaloidal extract and rod crystals from n-hexane extract. Molecular structure of the compounds was determined by analysis of spectra of NMR, IR, MS and compared by references. In vitro bioactivity test of the compound was performed against Plasmodium falciparum. The results showed that the bark of Act. macrophylla contained an aporphine alkaloid, actinodaphnine, that had activity against P. falciparum with IC50 value of 0.095 µg/mL and the bark of N. angustifolia contained a lignan compound, sesamine, with IC50 of 0.122 µg/mL.

Keywords: actinodaphne macrophylla, alkaloid, antiplasmodial, lauraceae, lignan, nectandra angustifolia

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Authors: Metwally Abdel Aziz Ahmed, Ahmed Shaban Abdel Hay Gabr, Inas Mohamed Saleh

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The main objective of structural design is to ensure safety and functional performance requirements of a structural system for its target reliability levels. In this study, the reliability index for the reinforcement concrete slender columns with rectangular cross section is studied. The variable parameters studied include the loads, the concrete compressive strength, the steel yield strength, the dimensions of concrete cross-section, the reinforcement ratio, and the location of steel placement. Risk analysis program was used to perform the analytical study. The effect of load eccentricity on the reliability index of reinforced concrete slender column was studied and presented. The results of this study indicate that the good quality control improve the performance of slender reinforced columns through increasing the reliability index β.

Keywords: reliability, reinforced concrete, safety, slender column

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Authors: Mohammad Khalid, Mariya Munir, Jacelyn Rice Boyaue

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Highways are considered a major source of pollution to storm-water, and its runoff can introduce various contaminants, including nutrients, Indicator bacteria, heavy metals, chloride, and phosphorus compounds, which can have negative impacts on receiving waters. This study assessed the ability of biochar for contaminants removal and to improve the water holding capacity of soil biochar mixture. For this, ten commercially available biochar has been strategically selected. Lab scale batch testing was done at 3% and 6% by the weight of the soil to find the preliminary estimate of contaminants removal along with hydraulic conductivity and water retention capacity. Furthermore, from the above-conducted studies, six best performing candidate and an application rate of 6% has been selected for the column studies. Soil biochar mixture was filled in 7.62 cm assembled columns up to a fixed height of 76.2 cm based on hydraulic conductivity. A total of eight column experiments have been conducted for nutrient, heavy metal, and indicator bacteria analysis over a period of one year, which includes a drying as well as a deicing period. The saturated hydraulic conductivity was greatly improved, which is attributed to the high porosity of the biochar soil mixture. Initial data from the column testing shows that biochar may have the ability to significantly remove nutrients, indicator bacteria, and heavy metals. The overall study demonstrates that biochar could be efficiently applied with clay soil to improve the soil's hydraulic characteristics as well as remove the pollutants from the stormwater runoff.

Keywords: biochar, nutrients, indicator bacteria, storm-water treatment, sustainability

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Authors: Muneerah Jeludin, V. Sivakumar

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Numerous laboratory-based research studies on the behavior of ground improved with granular columns with respect to bearing capacity have been well-documented. However, information on its settlement performance is still scarce. Laboratory model study on the settlement behavior of soft clay reinforced with granular columns was conducted and results are presented. The investigation uses a soft kaolin clay sample of 300 mm in diameter and 400 mm in length. The clay samples were reinforced with single and multiple granular columns of various lengths using the displacement and replacement installation method. The results indicated that that no settlement reduction was achieved for a short single floating column. The settlement reduction factors reported for L/d ratios of 5.0, 7.5 and 10.0 are in the range of 1 to 2. The findings obtained in this research showed that the reduction factors are considerably less and that load-sharing mechanism between columns and surrounding clay is complex, particularly for column groups and is affected by other factors such as negative skin friction.

Keywords: ground improvement, model test, reinforced soil, settlement

Procedia PDF Downloads 437

Authors: D. S. Mohale, A. P. Dewani, A. S.tripathi, A. V. Chandewar

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Present work demonstrates the applicability of high-performance liquid chromatography (HPLC) with UV-Vis detection for the quantification of malondialdehyde as malondialdehyde-thiobarbituric acid complex (MDA-TBA) in-vivo in rats. The HPLC method for MDA-TBA was achieved by isocratic mode on a reverse-phase C18 column (250mm×4.6mm) at a flow rate of 1.0mLmin−1 followed by detection at 532 nm. The chromatographic conditions were optimized by varying the concentration and pH of water followed by changes in percentage of organic phase optimal mobile phase consisted of mixture of water (0.2% triethylamine pH adjusted to 2.3 by ortho-phosphoric acid) and acetonitrile in ratio (80:20v/v). The retention time of MDA-TBA complex was 3.7 min. The developed method was sensitive as limit of detection and quantification (LOD and LOQ) for MDA-TBA complex were (standard deviation and slope of calibration curve) 110 ng/ml and 363 ng/ml respectively. Calibration studies were done by spiking MDA into rat plasma at concentrations ranging from 500 to 1000 ng/ml. The precision of developed method measured in terms of relative standard deviations for intra-day and inter-day studies was 1.6–5.0% and 1.9–3.6% respectively. The HPLC method was applied for monitoring MDA levels in rats subjected to chronic treatment of levofloxacin (LEV) (5mg/kg/day) for 21 days. Results were compared by findings in control group rats. Mean peak areas of both study groups was subjected for statistical treatment to unpaired student t-test to find p-values. The p value was <0.001 indicating significant results and suggesting increased MDA levels in rats subjected to chronic treatment of LEV of 21 days.

Keywords: malondialdehyde-thiobarbituric acid complex, levofloxacin, HPLC, oxidative stress

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Authors: Yuta Tachibana, Ayuko Itsuki

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The three strains of bacteria (Lysinibacillus xylanilyticus, Bacillus kochii, and Enterococcus sp.) were isolated from the fermented Indigo (Polygonum tinctorium) dyeing solution using the dilution plate method and some fermentation conditions were determined. High-Performance Liquid Chromatography (HPLC) was used to determine the indigo concentration. When the isolated bacteria were cultured in the indigo liquid culture containing various sugars, starch, and ethanol, the indigo culture solutions containing galactose, mannose, ribose, and ethanol were remarkably decreased. Comparison of decreasing indigo between three strains showed that Enterococcus sp. had the fastest growth and decrease of indigo. However, decreasing indigo per unit micro biomass did not correspond to the results of decreasing indigo―Bacillus kochii had higher indigo-reducing activity than Enterococcus sp. and Lysinibacillus xylanilyticus.

Keywords: fermentation condition, high-performance liquid chromatography (HPLC), indigo dyeing solution, indigo-reducing activity

Procedia PDF Downloads 115