Search results for: column chromatography

Authors: Samy Selim

Abstract:

Natural products are still major sources of innovative therapeutic agents for various conditions, including infectious diseases. Peganum harmala L. oil had wide range uses as traditional medicinal plants. The current study was designed to evaluate the antibacterial activity of P. harmala essential oil. The chemical constitutes and toxicity of these oils was also determined to obtain further information on the correlation between the chemical contents and antibacterial activity. The antibacterial effect of the essential oils of P. harmala oil was studied against some foodborne pathogenic bacteria species. The oil of plant was subjected to gas chromatography-mass spectrometry (GC/MS). The impact of oils administration on the change in rate of weight gain and complete blood picture in hamsters were investigated. P. harmala oil had strong antibacterial effect against bacterial species especially at minimum inhibitory concentration (MIC) less than 75.0 μg/ml. From the oil of P. harmala, forty one compounds were identified, and the major constituent was 1-hexyl-2-nitrocyclohexane (9.07%). Acute toxicity test was performed on hamsters and showed complete survival after 14 days, and there were no toxicity symptoms occurred. This study demonstrated that these essential oils seemed to be destitute of toxic effect which could compromise the medicinal use of these plants in folk medicine.

Keywords: analysis mass spectrometry, antibacterial activities, acute toxicity, chemical constitutes, gas chromatography, weight gain, Peganum harmala

Procedia PDF Downloads 462

Authors: Reza Ziaie Moayed, Ehsan Azini

Abstract:

Jet grouting (JG) is one of the methods of improving and increasing the strength and bearing of soil in which the high pressure water or grout is injected through the nozzles into the soil. During this process, a part of the soil and grout particles comes out of the drill borehole, and the other part is mixed up with the grout in place, as a result of this process, a mass of modified soil is created. The purpose of this method is to change the soil into a mixture of soil and cement, commonly known as "soil-cement". In this paper, first, the principles of high pressure injection and then the effective parameters in the JG method are described. Then, the tests on the samples taken from the columns formed from the excavation around the soil-cement columns, as well as the static loading test on the created column, are discussed. In the other part of this paper, the soil behavior models for numerical modeling in PLAXIS software are mentioned. The purpose of this paper is to evaluate the results of numerical modeling based on in-situ static loading tests. The results indicate an acceptable agreement between the results of the tests mentioned and the modeling results. Also, modeling with this software as an appropriate option for technical feasibility can be used to soil improvement using JG.

Keywords: jet grouting column, soil improvement, numerical modeling, in-situ loading test

Procedia PDF Downloads 112

Authors: Ping-Hsiung Wang, Kuo-Chun Chang

Abstract:

There has been a common trend worldwide in the seismic design and evaluation of bridges towards the performance-based method where the lateral displacement or the displacement ductility of bridge column is regarded as an important indicator for performance assessment. However, the seismic response of a bridge to an earthquake is a combined result of cyclic displacements and accumulated energy dissipation, causing damage to the bridge, and hence the lateral displacement (ductility) alone is insufficient to tell its actual seismic performance. This study aims to propose a damage-based seismic design and evaluation method for reinforced concrete bridges on the basis of the newly developed capacity-based inelastic displacement spectra. The capacity-based inelastic displacement spectra that comprise an inelastic displacement ratio spectrum and a corresponding damage state spectrum was constructed by using a series of nonlinear time history analyses and a versatile, smooth hysteresis model. The smooth model could take into account the effects of various design parameters of RC bridge columns and correlates the column’s strength deterioration with the Park and Ang’s damage index. It was proved that the damage index not only can be used to accurately predict the onset of strength deterioration, but also can be a good indicator for assessing the actual visible damage condition of column regardless of its loading history (i.e., similar damage index corresponds to similar actual damage condition for the same designed columns subjected to very different cyclic loading protocols as well as earthquake loading), providing a better insight into the seismic performance of bridges. Besides, the computed spectra show that the inelastic displacement ratio for far-field ground motions approximately conforms to the equal displacement rule when structural period is larger than around 0.8 s, but that for near-fault ground motions departs from the rule in the whole considered spectral regions. Furthermore, the near-fault ground motions would lead to significantly greater inelastic displacement ratio and damage index than far-field ground motions and most of the practical design scenarios cannot survive the considered near-fault ground motion when the strength reduction factor of bridge is not less than 5.0. Finally, the spectrum formula is presented as a function of structural period, strength reduction factor, and various column design parameters for far-field and near-fault ground motions by means of the regression analysis of the computed spectra. And based on the developed spectrum formula, a design example of a bridge is presented to illustrate the proposed damage-based seismic design and evaluation method where the damage state of the bridge is used as the performance objective.

Keywords: damage index, far-field, near-fault, reinforced concrete bridge, seismic design and evaluation

Procedia PDF Downloads 109

Authors: Fatima Zohra Ibn Majdoub Hassani, Ivan Lavandera, Joseph Kreit

Abstract:

This study explored the effects of different organic solvents, temperature, and the amount of glycerol on the alcohol dehydrogenase (ADH)-catalysed stereoselective reduction of different ketones. These conversions were then analyzed by gas chromatography. It was found that when the amount of deep eutectic solvents (DES) increases, it can improve the stereoselectivity of the enzyme although reducing its ability to convert the substrate into the corresponding alcohol. Moreover, glycerol was found to have a strong stabilizing effect on the ADH from Ralstonia sp. (E. coli/ RasADH). In the case of organic solvents, it was observed that the best conversions into the alcohols were achieved with DMSO and hexane. It was also observed that temperature decreased the ability of the enzyme to convert the substrates into the products and also affected the selectivity. In addition to that, the recycling of DES up to three times gave good conversions and enantiomeric excess results and glycerol showed a positive effect in the stability of various ADHs. Using RasADH, a good conversion and enantiomeric excess into the S-alcohol were obtained. It was found that an enhancement of the temperature disabled the stabilizing effect of glycerol and decreased the stereoselectivity of the enzyme. However, for other ADHs a temperature increase had an opposite positive effect, especially with ADH-T from Thermoanaerobium sp. One of the objectives of this study was to see the effect of cofactors such as NAD(P) on the biocatlysis activities of ADHs.

Keywords: alcohol dehydrogenases, DES, gas chromatography, RasADH

Procedia PDF Downloads 166

Authors: Khalid S. Hashim, Andy Shaw, Rafid Alkhaddar, Montserrat Ortoneda Pedrola

Abstract:

A flow column has been innovatively used in the design of a new electrocoagulation reactor (ECR1) that will reduce the temperature of water being treated; where the flow columns work as a radiator for the water being treated. In order to investigate the performance of ECR1 and compare it to that of traditional reactors; 600 mL water samples with an initial temperature of 35 0C were pumped continuously through these reactors for 30 min at current density of 1 mA/cm2. The temperature of water being treated was measured at 5 minutes intervals over a 30 minutes period using a thermometer. Additional experiments were commenced to investigate the effects of initial temperature (15-35 0C), water conductivity (0.15 – 1.2 S) and current density (0.5 -3 mA/cm2) on the performance of ECR1. The results obtained demonstrated that the ECR1, at a current density of 1 mA/cm2 and continuous flow model, reduced water temperature from 35 0C to the vicinity of 28 0C during the first 15 minutes and kept the same level till the end of the treatment time. While, the temperature increased from 28.1 to 29.8 0C and from 29.8 to 31.9 0C in the batch and the traditional continuous flow models respectively. In term of initial temperature, ECR1 maintained the temperature of water being treated within the range of 22 to 28 0C without the need for external cooling system even when the initial temperatures varied over a wide range (15 to 35 0C). The influent water conductivity was found to be a significant variable that affect the temperature. The desirable value of water conductivity is 0.6 S. However, it was found that the water temperature increased rapidly with a higher current density.

Keywords: water temperature, flow column, electrocoagulation

Procedia PDF Downloads 349

Authors: Osama H. Elsayed, Mohsen M. S. Asker, Mahmoud A. Swelim, Ibrahim H. Abbas, Aziza I. Attwa, Mohamed E. El Awady

Abstract:

Hydroxy marilone C is a bioactive metabolite was produced from the culture broth of Streptomyces badius isolated from Egyptian soil. hydroxy marilone C was purified and fractionated by silica gel column with a gradient mobile phase dicloromethane (DCM) : Methanol then Sephadex LH-20 column using methanol as a mobile phase. It was subjected to many instruments as Infrared (IR), nuclear magnetic resonance (NMR), Mass spectroscopy (MS) and UV spectroscopy to the elucidation of its structure. It was evaluated for antioxidant, cytotoxicity against human alveolar basal epithelial cell line (A-549) and human breast adenocarcinoma cell line (MCF-7) and antiviral activities; showed that the maximum antioxidant activity was 78.8 % at 3000 µg/ml after 90 min. and the IC50 value against DPPH radical found about 1500 µg/ml after 60 min. By Using MTT assay the effect of the pure compound on the proliferation of A-549 cells and MCF-7 cells were 443 µg/ml and 147.9 µg/ml, respectively. While for detection of antiviral activity using Madin-Darby canine kidney (MDCK) cells the maximum cytotoxicity was at 27.9% and IC50 was 128.1µg/ml. The maximum concentration required for protecting 50% of the virus-infected cells against H1N1 viral cytopathogenicity (EC50) was 33.25% for 80 µg/ml. This results indicated that the hydroxy marilone C has a potential antitumor and antiviral activities.

Keywords: hydroxy marilone C, production, bioactive compound, Streptomyces badius

Procedia PDF Downloads 237

Authors: Sanja Podunavac-Kuzmanović, Strahinja Kovačević, Lidija Jevrić, Evgenija Djurendić, Jovana Ajduković

Abstract:

There are several methods for determination of the lipophilicity of biologically active compounds, however chromatography has been shown as a very suitable method for this purpose. Chromatographic (C18-RP-HPLC) analysis of a series of 24 17-picolyl and 17-picolinylidene androstane derivatives was carried out. The obtained retention indices (logk, methanol (90%) / water (10%)) were correlated with calculated physicochemical and lipophilicity descriptors. The QSRR analysis was carried out applying principal component regression (PCR) and partial least squares regression (PLS). The PCR and PLS model were selected on the basis of the highest variance and the lowest root mean square error of cross-validation. The obtained PCR and PLS model successfully correlate the calculated molecular descriptors with logk parameter indicating the significance of the lipophilicity of compounds in chromatographic process. On the basis of the obtained results it can be concluded that the obtained logk parameters of the analyzed androstane derivatives can be considered as their chromatographic lipophilicity. These results are the part of the project No. 114-451-347/2015-02, financially supported by the Provincial Secretariat for Science and Technological Development of Vojvodina and CMST COST Action CM1105.

Keywords: androstane derivatives, chromatography, molecular structure, principal component regression, partial least squares regression

Procedia PDF Downloads 245

Authors: P. Susheela, Mary Rosaline, R. Radha

Abstract:

This research was designed to determine the bioactive compounds present in the nest samples of the mud dauber wasp, Sceliophron caementarium. Insects and insect-based products have been used for the treatment of various ailments from a very long time. It has been found that all over the world including the western societies and the indigenous populations, the usage of insect-based medicine plays an important role in various healing practices and magic rituals. Studies on the therapeutic usage of insects are negligible when compared to plants, the. In the present scenario, it is important to explore bioactive compounds from natural sources rather than depending on synthetic drugs that have adverse effects on human body. Keeping this in view, an attempt was made to analyze and identify bioactive components from the nest sample of the mud dauber wasp, Sceliophron caementarium. The nests of the mud dauber wasp, Sceliophron caementarium were collected from Coimbatore, Tamil Nadu, India. The nest sample was extracted with ethanol for 6-8 hours using Soxhlet apparatus. The final residue was obtained by filtering the extract through Whatman filter paper No.41. The GCMS analysis of the nest sample was performed using Perkin Elmer Elite - 5 capillary column. The resultant compounds were compared with the database of National Institute Standard and Technology (NIST), WILEY8, FAME. The GC-MS analysis of the concentrated ethanol extract revealed the presence of eight constituents like Methylene chloride, Eicosanoic acid, 1, 1’:3’, 1’’-Terphenyl, 5'-Phenyl, Di-N-Decylsulfone, 1, 2-Bis (Trimethylsilyl) Benzene, Androstane-11, 17-Dione, 3-[(Trimethylsilyl) Oxy]-, 17-[O-(Phenylmethyl) O. Most of the identified compounds were reported as having biological activities viz. anti-inflammatory, antibacterial and antifungal properties that can be of pharmaceutical importance and further study of these isolated compounds may prove their medicinal importance in future.

Keywords: Sceliophron caementarium, Gas chromatography-mass spectrometry, ethanol extract, bioactive compounds

Procedia PDF Downloads 267

Authors: Franz Zirena Vilca, Nestor Cahui Galarza, Walter Alejandro Zamalloa Cuba, Edith Tello Palma, Teofilo Donaires Flores, Valdemar Luiz Tornisielo

Abstract:

The production of rainbow trout in the Lake Titicaca represents an important economic activity for Peru. The city of Puno is responsible for 83% of this production, so the use of antibiotics within the aquaculture system is not alien to this reality. Meanwhile, the waters of Lake Titicaca represent an important source for the supply of drinking water for 80% of the population of the Puno city. In this paper, twelve antibiotics for veterinary use were monitored in water samples during two seasons: dry (July 2015) and rainy (February 2016), water samples from trout production systems, near the water catching point in the lake and drinking water in the city house of Puno were considered. The samples were analyzed using liquid chromatography coupled to mass spectrometry and solid online phase extraction (On-line SPE-LC-MS/MS), all samples analyzed showed concentrations of Ciprofloxacin up to 65.2 ng L⁻¹ at the rainy season. On the other hand, 63% of water samples from the dry season and 36 % from the rainy season showed Chlortetracycline up to 8.7 and 6.1 ng L⁻¹, respectively. The presence of residues of veterinary antibiotics in drinking water means a serious health risk for 80% of the population of Puno since all these people are supplied from this source.

Keywords: chromatography, DNA damage, environmental risk, water pollution

Procedia PDF Downloads 197

Authors: Laure Wiest, Barbara Giroud, Azziz Assoumani, Francois Lestremau, Emmanuelle Vulliet

Abstract:

Due to their production at high tonnages and their extensive use, surfactants are contaminants among those determined at the highest concentrations in wastewater. However, analytical methods and data regarding their occurrence in river water are scarce and concern only a few families, mainly anionic surfactants. The objective of this study was to develop an analytical method to extract and analyze a wide variety of surfactants in a minimum of steps, with a sensitivity compatible with the detection of ultra-traces in surface waters. 27 substances, from 12 families of surfactants, anionic, cationic and non-ionic were selected for method optimization. Different retention mechanisms for the extraction by solid phase extraction (SPE) were tested and compared in order to improve their detection by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The best results were finally obtained with a C18 grafted silica LC column and a polymer cartridge with hydrophilic lipophilic balance (HLB), and the method developed allows the extraction of the three types of surfactants with satisfactory recoveries. The final analytical method comprised only one extraction and two LC injections. It was validated and applied for the quantification of surfactants in 36 river samples. The method's limits of quantification (LQ), intra- and inter-day precision and accuracy were evaluated, and good performances were obtained for the 27 substances. As these compounds have many areas of application, contaminations of instrument and method blanks were observed and considered for the determination of LQ. Nevertheless, with LQ between 15 and 485 ng/L, and accuracy of over 80%, this method was suitable for monitoring surfactants in surface waters. Application on French river samples revealed the presence of anionic, cationic and non-ionic surfactants with median concentrations ranging from 24 ng/L for octylphenol ethoxylates (OPEO) to 4.6 µg/L for linear alkylbenzenesulfonates (LAS). The analytical method developed in this work will therefore be useful for future monitoring of surfactants in waters. Moreover, this method, which shows good performances for anionic, non-ionic and cationic surfactants, may be easily adapted to other surfactants.

Keywords: anionic surfactant, cationic surfactant, LC-MS/MS, non-ionic surfactant, SPE, surface water

Procedia PDF Downloads 109

Authors: Muhammad Tariq A. Chaudhary

Abstract:

Soil-structure interaction (SSI) in bridges under seismic excitation is a complex phenomenon which involves coupling between the non-linear behavior of bridge pier columns and SSI in the soil-foundation part. It is a common practice in the study of SSI to model the bridge piers as linear elastic while treating the soil and foundation with a non-linear or an equivalent linear modeling approach. Consequently, the contribution of soil and foundation to the SSI phenomenon is disproportionately highlighted. The present study considered non-linear behavior of bridge piers in FEM model of a 4-span, pile-supported bridge that was designed for five different soil conditions in a moderate seismic zone. The FEM model of the bridge system was subjected to a suite of 21 actual ground motions representative of three levels of earthquake hazard (i.e. Design Basis Earthquake, Functional Evaluation Earthquake and Maximum Considered Earthquake). Results of the FEM analysis were used to delineate the influence of pier column non-linearity and SSI on critical design parameters of the bridge system. It was found that pier column non-linearity influenced the bridge lateral displacement and base shear more than SSI for majority of the analysis cases for the class of bridge investigated in the study.

Keywords: bridge, FEM model, reinforced concrete pier, pile foundation, seismic loading, soil-structure interaction

Procedia PDF Downloads 204

Authors: I. Sarenkova, I. Ciprovica, I. Cinkmanis

Abstract:

Lactobionic acid is a disaccharide formed from gluconic acid and galactose, and produced by oxidation of lactose. Productivity of lactobionic acid by microbial synthesis can be affected by various factors, and one of them is a presence of potassium, magnesium and manganese ions. In order to extend lactobionic acid production efficiency, it is necessary to increase the yield of lactobionic acid by optimising the fermentation conditions and available substrates for Pseudomonas taetrolens growth. The object of the research was to determinate the application of K₂HPO₄, MnSO₄, MgSO₄ × 7H₂O salts in different concentration for effective lactose oxidation to lactobionic acid by Pseudomonas taetrolens. Pseudomonas taetrolens NCIB 9396 (NCTC, England) and Pseudomonas taetrolens DSM 21104 (DSMZ, Germany) were used for the study. The acid whey was used as the study object. The content of lactose in whey samples was determined using MilcoScan^TM Mars (Foss, Denmark) and high performance liquid chromatography (Shimadzu LC 20 Prominence, Japan). The content of lactobionic acid in whey samples was determined using the high performance liquid chromatography. The impact of studied salts differs, Mn²⁺ and Mg²⁺ ions enhanced fermentation instead of K⁺ ions. Results approved that Mn²⁺ and Mg²⁺ ions are necessary for Pseudomonas taetrolens growth. The study results will help to improve the effectiveness of lactobionic acid production with Pseudomonas taetrolens NCIB 9396 and DSM 21104.

Keywords: lactobionic acid, lactose oxidation, Pseudomonas taetrolens, whey

Procedia PDF Downloads 131

Authors: Dewi Selvia Fardhyanti, Astrilia Damayanti

Abstract:

Coal tar is a liquid by-product of coal pyrolysis processes. This liquid oil mixture contains various kind of useful compounds such as benzoic aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. The coal tar was collected by pyrolysis process of coal obtained from PT Kaltim Prima Coal and Arutmin-Kalimantan. The experiments typically occurred at the atmospheric pressure in a laboratory furnace at temperatures ranging from 300 to 550oC with a heating rate of 10oC/min and a holding time of 1 hour at the pyrolysis temperature. Nitrogen gas has been used to obtain the inert condition and to carry the gaseous pyrolysis products. The pyrolysis transformed organic materials into gaseous components, small quantities of liquid, and a solid residue (coke) containing fixed amount of carbon and ash. The composition of gas which is produced from the pyrolysis is carbon monoxide, hydrogen, methane, and other hydrocarbon compounds. The gas was condensed and the liquid containing oil/tar and water was obtained. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the coal tar components. The obtained coal tar has the viscosity of 3.12 cp, the density of 2.78 g/cm3, the calorific value of 11,048.44 cal/g, and the molecular weight of 222.67. The analysis result showed that the coal tar contained more than 78 chemical compounds such as benzene, cresol, phenol, xylene, naphtalene, etc. The total phenolic compounds contained in coal tar is 33.25% (PT KPC) and 17.58% (Arutmin-Kalimantan). The total naphtalene compounds contained in coal tar is 14.15% (PT KPC) and 17.13% (Arutmin-Kalimantan).

Keywords: coal tar, pyrolysis, gas chromatography-mass spectroscopy

Procedia PDF Downloads 304

Authors: Zsolt Szilvágyi, Jakub Panuska, Orsolya Kegyes-Brassai, Ákos Wolf, Péter Tildy, Richard P. Ray

Abstract:

Near-surface loose sediments and local ground conditions in general have a major influence on seismic response of structures. It is a difficult task to model ground behavior in seismic soil-structure-foundation interaction problems, fully account for them in seismic design of structures, or even properly consider them in seismic hazard assessment. In this study, we focused on applying seismic soil investigation methods, used for determining soil stiffness and damping properties, to response analysis used in seismic design. A site in Budapest, Hungary was investigated using Multichannel Analysis of Surface Waves, Seismic Cone Penetration Tests, Bender Elements, Resonant Column and Torsional Shear tests. Our aim was to compare the results of the different test methods and use the resulting soil properties for 1D ground response analysis. Often in practice, there are little-to no data available on dynamic soil properties and estimated parameters are used for design. Therefore, a comparison is made between results based on estimated parameters and those based on detailed investigations. Ground response results are also compared to Eurocode 8 design spectra.

Keywords: MASW, resonant column test, SCPT, site response analysis, torsional shear test

Procedia PDF Downloads 383

Authors: Tengku Muhammad Rafi Nazmi Bin Tengku Razali, Habsah Alwi

Abstract:

This article based on effect of temperature towards extraction of Aquilaria Subintegra. Aquilaria Subintegra which its main habitat is in Asia-tropical and particularly often found in its native which is Thailand. There is claim which is Aquilaria Subintegra contains antipyretic properties that helps fight fever. Research nowadays also shown that paracetamol consumed bring bad effect towards consumers. This sample will first dry using Vacuum Far Infrared which provides better drying than conventional oven. Soxhlet extractor used to extract oil from sample. Gas Chromatography Mass Spectrometer used to analyze sample to determine its compound. Objective from this research was to determine the active ingredients that exist in the Aquilaria Subintegra leaves and to determine whether compound of Acetaminophen exist or not inside the leaves. Moisture content from 400C was 80%, 500C was 620% and 600C was 36%. The greater temperature resulting lower moisture content inside sample leaves. 7 components were identified in sample T=400C while only 5 components were identified in sample at T=50C and T=60C. Four components were commonly identified in three sample which is 1n-Hexadecanoic acid, 9,12,15-Octadecatrienoic acid, methyl ester (z,z,z), Vitamin E and Squalene. Further studies are needed with new series of temperature to refine the best results.

Keywords: aquilaria subintegra, vacuum far infrared, SOXHLET extractor, gas chromatography mass spectrometer, paracetamol

Procedia PDF Downloads 456

Authors: G. Dan Chépo, L. Ban-Koffi, N. Kouassi Kouakou, M. Dje Kouakou, J. Nemlin, A. Sahore Drogba, L. Kouame Patrice

Abstract:

Solanum anguivi Lam, collectively called Gnagnan in Côte d'Ivoire is an eggplant with nutritional and therapeutic potentialities more or less known. The present study was undertaken to analyze the biochemical composition of berries at the different stages of maturity. Data showed that at the first stage of maturity (green berries), fruits are rich in ascorbic acid (34.48 ± 1.7 mg / 100 g dm), phenolic compounds (956.7 ± 71.14 mg / 100 g dm), iron (467.7 ± 1.84 mg / 100 g dm), magnesium (404.6 ± 16.25 mg / 100 g dm) and potassium (404.64 ± 16.25 mg/100 g dm). However, at the last stage of maturity (red berries), fruits are rich in proteins, cellulose, total sugars, fat and potassium with the values of 22.53 ± 2 g/100 g dm, 19.12 ± 0.35 g/100 g dm, 3.7 ± 0.2 g/100 g dm, 2.65 ± 0.19 g/100 g dm and 2290.84 ± 22.24 mg / 100 g dm, respectively. The chromatography on thin layer revealed the presence of glucose, ribose, xylose, arabinose and fructose at all the maturity stages. Except for alkaloids and gallic tannins, the phytochemical sorting revealed that Gnagnan contain many pharmacological components. According to the maturity stages, orange and red berries showed a higher content in sterols and polyterpens, flavonoids and saponins. The green berries contain most of polyphenols, catechintannins and quinons. As for the yellow berries, they are rich in polyphenols and catechintannins. These data contribute to enhance clinical researches on nutritional and pharmacological properties of S. anguivi Lam.

Keywords: Gnagnan, maturity stage, chemical composition, chromatography thin layer, phytochemical sorting

Procedia PDF Downloads 467

Authors: Y. A. Prada, Fanny Guzman, Rafael Cabanzo, John J. Castillo, Enrique Mejia-Ospino

Abstract:

In this work, we show the important results about of synthesis of photoluminiscents gold nanoclusters using a small peptide as template for biosensing applications. Interestingly, we design one peptide (NBC2854) homologue to conservative domain from 215 250 residue of a galactolectin protein which can recognize the proteophosphoglycans (PPG) from Leishmania. Peptide was synthetized by multiple solid phase synthesis using FMoc group methodology in acid medium. Finally, the peptide was purified by High-Performance Liquid Chromatography using a Vydac C-18 preparative column and the detection was at 215 nm using a Photo Diode Array detector. Molecular mass of this peptide was confirmed by MALDI-TOF and to verify the α-helix structure we use Circular Dichroism. By means of the methodology used we obtained a novel fluorescents gold nanoclusters (AuNC) using NBC2854 as a template. In this work, we described an easy and fast microsonic method for the synthesis of AuNC with ≈ 3.0 nm of hydrodynamic size and photoemission at 630 nm. The presence of cysteine residue in the C-terminal of the peptide allows the formation of Au-S bond which confers stability to Peptide-based gold nanoclusters. Interactions between the peptide and gold nanoclusters were confirmed by X-ray Photoemission and Raman Spectroscopy. Notably, from the ultrafine spectra shown in the MALDI-TOF analysis which containing only 3-7 KDa species was assigned to Au₈-₁₈[NBC2854]₂ clusters. Finally, we evaluated the Peptide-gold nanocluster as an optical biosensor based on fluorescence spectroscopy and the fluorescence signal of PPG (0.1 µg-mL⁻¹ to 1000 µg-mL⁻¹) was amplified at the same wavelength emission (≈ 630 nm). This can suggest that there is a strong interaction between PPG and Pep@AuNC, therefore, the increase of the fluorescence intensity can be related to the association mechanism that take place when the target molecule is sensing by the Pep@AuNC conjugate. Further spectroscopic studies are necessary to evaluate the fluorescence mechanism involve in the sensing of the PPG by the Pep@AuNC. To our best knowledge the fabrication of an optical biosensor based on Pep@AuNC for sensing biomolecules such as Proteophosphoglycans which are secreted in abundance by parasites Leishmania.

Keywords: biosensing, fluorescence, Leishmania, peptide-gold nanoclusters, proteophosphoglycans

Procedia PDF Downloads 144

Authors: V. Khosravi, F. D. Ardejani, A. Aryafar, M. Sedighi

Abstract:

Heavy metals have a damaging impact for the environment, animals and humans due to their extreme toxicity and removing them from wastewaters is a very important and interesting task in the field of water pollution control. Biosorption is a relatively new method for treatment of wastewaters and recovery of heavy metals. In this study, a continuous fixed bed study was carried out by using Bacillus thuringiensis as a biosorbent for the removal of Cu and Mn ions from Sarcheshmeh Acid Mine Drainage (AMD). The effect of operating parameters such as flow rate and bed height on the sorption characteristics of B. thuringiensis was investigated at pH 6.0 for each metal ion. The experimental results showed that the breakthrough time decreased with increasing flow rate and decreasing bed height. The data also indicated that the equilibrium uptake of both metals increased with decreasing flow rate and increasing bed height. BDST, Thomas, and Yoon–Nelson models were applied to experimental data to predict the breakthrough curves. All models were found suitable for describing the whole dynamic behavior of the column with respect to flow rate and bed height. In order to regenerate the adsorbent, an elution step was carried out with 1 M HCl and five adsorption-desorption cycles were carried out in continuous manner.

Keywords: acid mine drainage, bacillus thuringiensis, biosorption, cu and mn ions, fixed bed

Procedia PDF Downloads 379

Authors: Ian Walsh, Terry Nguyen-Khuong, Christopher H. Taron, Pauline M. Rudd

Abstract:

Glycoproteins and their covalently bonded glycans play critical roles in the immune system, cell communication, disease and disease prognosis. Ultra performance liquid chromatography (UPLC) coupled with mass spectrometry is conventionally used to qualitatively and quantitatively characterise glycan structures in a given sample. Exoglycosidases are enzymes that catalyze sequential removal of monosaccharides from the non-reducing end of glycans. They naturally have specificity for a particular type of sugar, its stereochemistry (α or β anomer) and its position of attachment to an adjacent sugar on the glycan. Thus, monitoring the peak movements (both in the UPLC and MS1) after application of exoglycosidases provides a unique and effective way to annotate sugars with high detail - i.e. differentiating positional and linkage isomers. Manual annotation of an exoglycosidase experiment is difficult and time consuming. As such, with increasing sample complexity and the number of exoglycosidases, the analysis could result in manually interpreting hundreds of peak movements. Recently, we have implemented pattern recognition software for automated interpretation of UPLC-MS1 exoglycosidase digestions. In this work, we explain the software, indicate how much time it will save and provide example usage showing the annotation of positional and linkage isomers in Immunoglobulin G, apolipoprotein J, and simple glycan standards.

Keywords: bioinformatics, automated glycan assignment, liquid chromatography, mass spectrometry

Procedia PDF Downloads 174

Authors: Sudhanshu Sharma

Abstract:

Lisinopril, 1-[N-{(s)-I-carboxy-3 phenyl propyl}-L-proline dehydrate is a lysine analog of enalaprilat, the active metabolite of enalapril. It is long-acting, non-sulhydryl angiotensin-converting enzyme (ACE) inhibitor that is used for the treatment of hypertension and congestive heart failure in daily dosage 10-80 mg. Pharmacological activity of lisinopril has been proved in various experimental and clinical studies. Owing to its importance and widespread use, efforts have been made towards the development of simple and reliable analytical methods. As per our literature survey, lisinopril in pharmaceutical formulations has been determined by various analytical methodologies like polaragraphy, potentiometry, and spectrophotometry, but most of these analytical methods are not too suitable for the Identification of lisinopril from clinical samples because of the interferences caused by the amino acids and amino groups containing metabolites present in biological samples. This report is an attempt in the direction of developing a simple and reliable method for on plate identification and quantification of lisinopril in pharmaceutical formulations as well as from human urine samples using silica gel H layers developed with a new mobile phase comprising of micellar solutions of N-cetyl-N, N, N-trimethylammonium bromide (CTAB). Micellar solutions have found numerous practical applications in many areas of separation science. Micellar liquid chromatography (MLC) has gained immense popularity and wider applicability due to operational simplicity, cost effectiveness, relatively non-toxicity and enhanced separation efficiency, low aggressiveness. Incorporation of aqueous micellar solutions as mobile phase was pioneered by Armstrong and Terrill as they accentuated the importance of TLC where simultaneous separation of ionic or non-ionic species in a variety of matrices is required. A peculiarity of the micellar mobile phases (MMPs) is that they have no macroscopic analogues, as a result the typical separations can be easily achieved by using MMPs than aqueous organic mobile phases. Previously MMPs were successfully employed in TLC based critical separations of aromatic hydrocarbons, nucleotides, vitamin K1 and K5, o-, m- and p- aminophenol, amino acids, separation of penicillins. The human urine analysis for identification of selected drugs and their metabolites has emerged as an important investigation tool in forensic drug analysis. Among all chromatographic methods available only thin layer chromatography (TLC) enables a simple fast and effective separation of the complex mixtures present in various biological samples and is recommended as an approved testing for forensic drug analysis by federal Law. TLC proved its applicability during successful separation of bio-active amines, carbohydrates, enzymes, porphyrins, and their precursors, alkaloid and drugs from urine samples.

Keywords: lisnopril, surfactant, chromatography, micellar solutions

Procedia PDF Downloads 341

Authors: Ying Liang, Na Li

Abstract:

Lipo-alkaloid is a kind of C19-norditerpenoid alkaloids existed in Aconitum species, which usually contains an aconitane skeleton and one or two fatty acid residues. The structures are very similar to that of diester-type alkaloids, which are considered as the main bioactive components in Aconitum carmichaelii. They have anti-inflammatory, anti-nociceptive, and anti-proliferative activities. So far, more than 200 lipo-alkaloids were reported from plants, semisynthesis, and biotransformations. In our research, by the combination of ultra-high performance liquid chromatography-quadruple-time of flight mass spectrometry (UHPLC-Q-TOF-MS) and an in-house database, 148 lipo-alkaloids were identified from A. carmichaelii, including 93 potential new compounds and 38 compounds with oxygenated fatty acid moieties. To our knowledge, this is the first time of the reporting of the oxygenated fatty acids as the side chains in naturally-occurring lipo-alkaloids. Considering the fatty acid residues in lipo-alkaloids should come from the free acids in the plant, the fatty acids and their relationship with lipo-alkaloids were further investigated by GC-MS and LC-MS. Among 17 fatty acids identified by GC-MS, 12 were detected as the side chains of lipo-alkaloids, which accounted for about 1/3 of total lipo-alkaloids, while these fatty acid residues were less than 1/4 of total fatty acid residues. And, total of 37 fatty acids were determined by UHPCL-Q-TOF-MS, including 18 oxidized fatty acids firstly identified from A. carmichaelii. These fatty acids were observed as the side chains of lipo-alkaloids. In addition, although over 140 lipo-alkaloids were identified, six lipo-alkaloids, 8-O-linoleoyl-14-benzoylmesaconine (1), 8-O-linoleoyl-14-benzoylaconine (2), 8-O-palmitoyl-14-benzoylmesaconine (3), 8-O-oleoyl-14-benzoylmesaconine (4), 8-O-pal-benzoylaconine (5), and 8-O-ole-Benzoylaconine (6), were found to be the main components, which accounted for over 90% content of total lipo-alkaloids. Therefore, using these six components as standards, a UHPLC-Triple Quadrupole-MS (UHPLC-QQQ-MS) approach was established to investigate the influence of processing on the contents of lipo-alkaloids. Although it was commonly supposed that the contents of lipo-alkaloids increased after processing, our research showed that no significant change was observed before and after processing. Using the same methods, the lipo-alkaloids in the lateral roots of A. carmichaelii and the roots of A. kusnezoffii were determined and quantified. The contents of lipo-alkaloids in A. kusnezoffii were close to that of the parent roots of A. carmichaelii, while the lateral roots had less lipo-alkaloids than the parent roots. This work was supported by Macao Science and Technology Development Fund (086/2013/A3 and 003/2016/A1).

Keywords: Aconitum carmichaelii, fatty acids, GC-MS, LC-MS, lipo-alkaloids

Procedia PDF Downloads 271

Authors: Mei Hong, Wei Liu, Xuemin Dai, Yanxiong Pan, Xiangling Ji

Abstract:

Polyamic acid (PAA) is the precursor of polyimide (PI) prepared by a two-step method, its molecular weight and molecular weight distribution not only play an important role during the preparation and processing, but also influence the final performance of PI. However, precise characterization on molecular weight of PAA is still a challenge because of the existence of very complicated interactions in the solution system, including the electrostatic interaction, hydrogen bond interaction, dipole-dipole interaction, etc. Thus, it is necessary to establisha suitable strategy which can completely suppress these complex effects and get reasonable data on molecular weight. Herein, the gel permeation chromatography (GPC) coupled with differential refractive index (RI) and multi-angle laser light scattering (MALLS) detectors were applied to measure the molecular weight of (6FDA-DMB) PAA using different mobile phases, LiBr/DMF, LiBr/H3PO4/THF/DMF, LiBr/HAc/THF/DMF, and LiBr/HAc/DMF, respectively. It was found that combination of LiBr with HAc can shield the above-mentioned complex interactions and is more conducive to the separation of PAA than only addition of LiBr in DMF. LiBr/HAc/DMF was employed for the first time as a mild mobile phase to effectively separate PAA and determine its molecular weight. After a series of conditional experiments, 0.02M LiBr/0.2M HAc/DMF was fixed as an optimized mobile phase to measure the relative and absolute molecular weights of (6FDA-DMB) PAA prepared, and the obtained Mw from GPC-MALLS and GPC-RI were 35,300 g/mol and 125,000 g/mol, respectively. Particularly, such a mobile phase is also applicable to other PAA samples with different structures, and the final results on molecular weight are also reproducible.

Keywords: Polyamic acids, Polyelectrolyte effects, Gel permeation chromatography, Mobile phase, Molecular weight

Procedia PDF Downloads 27

Authors: Kristine Vike-Jonas, Susana V. Gonzalez, Olav L. Bakkerud, Karoline S. Gjelstad, Shazia N. Aslam, Øyvind Mikkelsen, Alexandros Asimakopoulos

Abstract:

P-hydrobenzoic acid esters (parabens), paraben metabolites, and triclocarban (TCC) are a group of synthetic antimicrobials classified as endocrine disrupting chemicals (EDCs) and emerging pollutants. The aim of this study was to investigate the levels of these compounds in sediment near the effluent of a wastewater treatment plant (WWTP) in the Trondheim Fjord, Norway. Paraben, paraben metabolites, and TCC are high volume production chemicals that are found in a range of consumer products, especially pharmaceuticals and personal care products (PCPs). In this study, six parabens (methyl paraben; MeP, ethyl paraben; EtP, propyl paraben; PrP, butyl paraben; BuP, benzyl paraben; BezP, heptyl paraben; HeP), four paraben metabolites (4-hydroxybenzoic acid; 4-HB, 3,4-dihydroxybenzoic acid; 3,4-DHB, methyl protocatechuic acid; OH-MeP, ethyl protocatechuic acid; OH-EtP) and TCC were determined by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in 64 sediment samples from 10 different locations outside Trondheim, Norway. Of these 11 target analytes, four were detected in 40 % or more of the samples. The sum of six parabens (∑Parabens), four paraben metabolites (∑Metabolites) and TCC in sediment ranged from 4.88 to 11.56 (mean 6.81) ng/g, 52.16 to 368.28 (mean 93.89) ng/g and 0.53 to 3.65 (mean 1.50) ng/g dry sediment, respectively. Pearson correlation coefficients indicated that TCC was positively correlated with OH-MeP, but negatively correlated with 4-HB. To the best of the author’s knowledge, this is the first time parabens, paraben metabolites and TCC have been reported in the Trondheim Fjord.

Keywords: parabens, liquid chromatography, sediment, tandem mass spectrometry

Procedia PDF Downloads 100

Authors: Mahmoud F. Awad-Allah, Mohammed Rabeih, Eman Abdel Baseer

Abstract:

Soft to very soft soil deposits are widely speared in some areas of Egypt such as East Port Said, Damietta, Kafr El-Sheik, Alexandria, etc. The construction projects in these areas have faced the challenge of the presence of extended deep layers of soft and very soft clays which reach to depths of 40 to 60 m from the ground level. Stone columns are commonly used to support structures overlying soft ground soils and surcharged by embankment type loading. Therefore, this paper introduces a wide comparison numerical study between the ordinary stone columns (OSC) versus the geosynthetic encased stone columns (ESC) installed in soft clay soil deposit using finite element method (FEM). Parametric study of an embankment on soft soils reinforced with stone columns is performed using commercial computer program based on the finite element technique (PLAXIS 2D). The investigation will present the influence of the following parameters: diameter of stone columns, stiffness of geosynthetic encasement, embedded depth of stone column from ground level, and the length encasement of the stone column on the consolidation time, vertical settlement, and lateral displacement of soft clay soil formations.

Keywords: finite element method, geosynthetic, lateral displacement, settlement, soft clay

Procedia PDF Downloads 181

Authors: Thanida Sritangthong, Suksun Amornraksa

Abstract:

By-product upgrading is crucial in hydrocarbon industries as it can increase overall profit margin of the business. Microwave-assisted pyrolysis is relatively new technique which induces heat directly to raw materials. This results in a more energy saving and more energy-efficient process. It is also a promising method to enhance and accelerate chemical reactions, thus reducing the pyrolysis reaction time and increasing the quality of value-added products from different kinds of feedstocks. In this study, upgrading opportunity of fuel oil by-product from an olefins plant is investigated by means of microwave pyrolysis. The experiment was conducted in a lab-scale quartz reactor placed inside a 1,100 watts household microwave oven. Operating temperature was varied from 500 to 900C to observe the consequence on the quality of pyrolysis products. Several microwave receptors i.e. activated carbon, silicon carbide (SiC) and copper oxide (CuO) were used as a material to enhance the heating and reaction in the reactor. The effect of residence time was determined by adjusting flow rate of N2 carrier gas. The chemical composition and product yield were analyzed by using gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). The results showed that hydrogen, methane, ethylene, and ethane were obtained as the main gaseous products from all operating temperatures while the main liquid products were alkane, cycloalkane and polycyclic aromatic groups. The results indicated that microwave pyrolysis has a potential to upgrade low value hydrocarbons to high value products.

Keywords: fuel oil, heavy hydrocarbons, microwave pyrolysis, pyrolysis

Procedia PDF Downloads 292

Authors: P. S. Seboletswe, Z. Mkhize, L. M. Katata-Seru

Abstract:

Protorhus longifolia is known as a medicinal plant that has been used traditionally to treat various ailments such as hemiplegic paralysis, blood clotting related diseases, diarrhoea, heartburn, etc. The study reports a High-Performance Thin Layer Chromatography (HPTLC) fingerprint profile of Protorhus longifolia methanolic extract and its qualitative analysis of gallic acid, rutin, and quercetin. HPTLC analysis was achieved using CAMAG HPTLC system equipped with CAMAG automatic TLC sampler 4, CAMAG Automatic Developing Chamber 2 (ADC2), CAMAG visualizer 2, CAMAG Thin Layer Chromatography (TLC) scanner and visionCATS CAMAG HPTLC software. Mobile phase comprising toluene, ethyl acetate, formic acid (21:15:3) was used for qualitative analysis of gallic acid and revealed eight peaks while the mobile phase containing ethyl acetate, water, glacial acetic acid, formic acid (100:26:11:11) for qualitative analysis of rutin and quercetin revealed six peaks. HPTLC sillica gel 60 F254 glass plates (10 × 10) were used as the stationary phase. Gallic acid was detected at the R_f = 0.35; while rutin and quercetin were not evident in the extract. Further studies will be performed to quantify gallic acid in Protorhus longifolia leaves and also identify other biomarkers.

Keywords: biomarkers, fingerprint profiling, gallic acid, HPTLC, Protorhus longifolia

Procedia PDF Downloads 117

Authors: Waleed A. El-Said, Dina M. Fouad, Mohamed H. Aly, Mohamed A. El-Gahami

Abstract:

Green synthesis of nanomaterials has received increasing attention as an eco-friendly technology in materials science. Here, we have used two types of extractions from green tea leaf (i.e. total extraction and tannin extraction) as reducing agents for a rapid, simple and one step synthesis method of mesoporous silica nanoparticles (MSNPs)/iron oxide (Fe3O4) nanocomposite based on deposition of Fe3O4 onto MSNPs. MSNPs/Fe3O4 nanocomposite were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray, vibrating sample magnetometer, N2 adsorption, and high-resolution transmission electron microscopy. The average mesoporous silica particle diameter was found to be around 30 nm with high surface area (818 m2/gm). MSNPs/Fe3O4 nanocomposite was used for removing lindane pesticide (an environmental hazard material) from aqueous solutions. Fourier transform infrared, UV-vis, High-performance liquid chromatography and gas chromatography techniques were used to confirm the high ability of MSNPs/Fe3O4 nanocomposite for sensing and capture of lindane molecules with high sorption capacity (more than 89%) that could develop a new eco-friendly strategy for detection and removing of pesticide and as a promising material for water treatment application.

Keywords: green synthesis, mesoporous silica, magnetic iron oxide NPs, adsorption Lindane

Procedia PDF Downloads 409

Authors: Ayat Bani Rashaid, Zain Khasawneh, Mazin Alqhazo, Shreen Nusair, Mohammad El-Khateeb, Mahmoud Bashtawi

Abstract:

Autism Spectrum disorder (ASD) is a psychiatric disorder with unknown etiology that mainly affects children in the first three years of life. Alterations of amino acid levels are believed to contribute to ASD. The levels of six essential amino acids (methionine, histidine, valine, leucine, threonine, and phenylalanine), five conditional amino acids (proline, tyrosine, glutamine, cysteine, and cystine), and five non-essential amino acids (asparagine, aspartic acid, alanine, serine, and glutamic acid) in hair samples of children with ASD (n = 25) were analyzed and compared to corresponding levels in healthy age-matched controls (n = 25). The results showed that the levels of methionine, alanine, and asparagine were significantly lower in the hair samples of ASD group compared to those of the control group (p ≤ 0.05). However, the levels of glutamic acid were significantly higher in the ASD group than the control group (p ≤ 0.05). The current findings could contribute towards further understanding of ASD etiology and provide specialists with a hair amino acid profile utilized as a biomarker for early diagnosis of ASD. Such biomarkers could participate in future developments of therapies that reduce ASD-related symptoms.

Keywords: autism spectrum disorder, amino acids, liquid chromatography-tandem mass spectrometry, human hair

Procedia PDF Downloads 111

Authors: G. La Scalia, M. Enea, R. Micale, O. Corona, L. Settanni

Abstract:

The quality and condition of perishable products delivered to the market and their subsequent selling prices are directly affected by the care taken during harvesting and handling. Mechanical injury, in fact, occurs at all stages, from pre-harvest operations through post-harvest handling, packing and transport to the market. The main implications of this damage are the reduction of the product’s quality and economical losses related to the shelf life diminution. For most perishable products, the shelf life is relatively short and it is typically dictated by microbial growth related to the application of dynamic and static loads during transportation. This paper presents the correlation between vibration levels and microbiological growth on strawberries and woodland strawberries and detects the presence of volatile organic compounds (VOC) in order to develop an intelligent logistic unit capable of monitoring VOCs using a specific sensor system. Fresh fruits were exposed to vibrations by means of a vibrating table in a temperature-controlled environment. Microbiological analyses were conducted on samples, taken at different positions along the column of the crates. The values obtained were compared with control samples not exposed to vibrations and the results show that different positions along the column influence the development of bacteria, yeasts and filamentous fungi.

Keywords: microbiological analysis, shelf life, transport damage, volatile organic compounds

Procedia PDF Downloads 399

Authors: R. Kumaravelu, S. Poornima, Sunil Kumar Kashyap

Abstract:

The optimized and digitalized restoration of the information from the old and used manual jacquard punched card in textile industry is referred to as Jacquard Punch Card (JPC) reader. In this paper, we present a novel design and development of photo electronics based system for reading old and used punched cards and storing its binary information for transforming them into an effective image file format. In our textile industry the jacquard punched cards holes diameters having the sizes of 3mm, 5mm and 5.5mm pitch. Before the adaptation of computing systems in the field of textile industry those punched cards were prepared manually without digital design source, but those punched cards are having rich woven designs. Now, the idea is to retrieve binary information from the jacquard punched cards and store them in digital (Non-Graphics) format before processing it. After processing the digital format (Non-Graphics) it is converted into an effective image file format through either by Row major or Column major parsing technique.To accomplish these activities, an embedded system based device and software integration is developed. As part of the test and trial activity the device was tested and installed for industrial service at Weavers Service Centre, Kanchipuram, Tamilnadu in India.

Keywords: file system, SPI. UART, ARM controller, jacquard, punched card, photo LED, photo diode

Procedia PDF Downloads 141