Search results for: high performance liquid chromatography (HPLC)

Authors: Alija Uzunovic, Sasa Pilipovic, Aida Sapcanin, Zahida Ademovic, Berina Pilipović

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Capsaicin is a naturally occurring alkaloid extracted from capsicum fruit extracts of different of Capsicum species. It has been employed topically to treat many diseases such as rheumatoid arthritis, osteoarthritis, cancer pain and nerve pain in diabetes. The high degree of pre-systemic metabolism of intragastrical capsaicin and the short half-life of capsaicin by intravenous administration made topical application of capsaicin advantageous. In this study, we have evaluated differences in the dissolution characteristics of capsaicin patch 11 mg (purchased from market) at different dissolution rotation speed. The proposed patch area is 308 cm2 (22 cm x 14 cm; it contains 36 µg of capsaicin per square centimeter of adhesive). USP Apparatus 5 (Paddle Over Disc) is used for transdermal patch testing. The dissolution study was conducted using USP apparatus 5 (n=6), ERWEKA DT800 dissolution tester (paddle-type) with addition of a disc. The fabricated patch of 308 cm2 is to be cut into 9 cm2 was placed against a disc (delivery side up) retained with the stainless-steel screen and exposed to 500 mL of phosphate buffer solution pH 7.4. All dissolution studies were carried out at 32 ± 0.5 °C and different rotation speed (50± 5; 100± 5 and 150± 5 rpm). 5 ml aliquots of samples were withdrawn at various time intervals (1, 4, 8 and 12 hours) and replaced with 5 ml of dissolution medium. Withdrawn were appropriately diluted and analyzed by reversed-phase liquid chromatography (RP-LC). A Reversed Phase Liquid Chromatography (RP-LC) method has been developed, optimized and validated for the separation and quantitation of capsaicin in a transdermal patch. The method uses a ProntoSIL 120-3-C18 AQ 125 x 4,0 mm (3 μm) column maintained at 600C. The mobile phase consisted of acetonitrile: water (50:50 v/v), the flow rate of 0.9 mL/min, the injection volume 10 μL and the detection wavelength 222 nm. The used RP-LC method is simple, sensitive and accurate and can be applied for fast (total chromatographic run time was 4.0 minutes) and simultaneous analysis of capsaicin and dihydrocapsaicin in a transdermal patch. According to the results obtained in this study, we can conclude that the relative difference of dissolution rate of capsaicin after 12 hours was elevated by increase of dissolution rotation speed (100 rpm vs 50 rpm: 84.9± 11.3% and 150 rpm vs 100 rpm: 39.8± 8.3%). Although several apparatus and procedures (USP apparatus 5, 6, 7 and a paddle over extraction cell method) have been used to study in vitro release characteristics of transdermal patches, USP Apparatus 5 (Paddle Over Disc) could be considered as a discriminatory test. would be able to point out the differences in the dissolution rate of capsaicin at different rotation speed.

Keywords: capsaicin, in vitro, patch, RP-LC, transdermal

Procedia PDF Downloads 227

Authors: S. Chikh, S. Boulifa

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The present study addresses the problem of ammonia evaporation during filling of a vertical cylindrical tank and the influence of various external factors on the stability of storage by determining the conditions for minimum evaporation. Numerical simulation is carried out by solving the governing equations namely, continuity, momentum, energy, and diffusion of species. The effect of temperature of surrounding air, the filling speed of the reservoir and the temperature of the filling liquid ammonia on the evaporation rate is investigated. Results show that the temperature of the filling liquid has little effect on the liquid ammonia for a short period, which, in fact, is function of the filling speed. The evaporation rate along the free surface of the liquid is non-uniform. The inlet temperature affects the vapor ammonia temperature because of pressure increase. The temperature of the surrounding air affects the temperature of the vapor phase rather than the liquid phase. The maximum of evaporation is reached at the final step of filling. In order to minimize loss of ammonia vapors automatically causing losses in quantity of the liquid stored, it is suggested to ensure the proper insulation for the walls and roof of the reservoir and to increase the filling speed.

Keywords: evaporation, liquid ammonia, storage tank, numerical simulation

Procedia PDF Downloads 288

Authors: Serkan Sayin, Songul F. Varol

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High attention on the organic light-emitting diodes has been paid since their efficient properties in the flat panel displays, and solid-state lighting was realized. Because of their high efficient electroluminescence, brightness and providing eminent in the emission range, organic light emitting diodes have been preferred a material compared with the other materials consisting of the liquid crystal. Calixarenes obtained from the reaction of p-tert-butyl phenol and formaldehyde in a suitable base have been potentially used in various research area such as catalysis, enzyme immobilization, and applications, ion carrier, sensors, nanoscience, etc. In addition, their tremendous frameworks, as well as their easily functionalization, make them an effective candidate in the applied chemistry. Herein, a calix[4]arene derivative has been synthesized, and its structure has been fully characterized using Fourier Transform Infrared Spectrophotometer (FTIR), proton nuclear magnetic resonance (¹H-NMR), carbon-13 nuclear magnetic resonance (¹³C-NMR), liquid chromatography-mass spectrometry (LC-MS), and elemental analysis techniques. The calixarene derivative has been employed as an emitting layer in the fabrication of the organic light-emitting diodes. The optical and electrochemical features of calixarane-contained organic light-emitting diodes (Clx-OLED) have been also performed. The results showed that Clx-OLED exhibited blue emission and high external quantum efficacy. As a conclusion obtained results attributed that the synthesized calixarane derivative is a promising chromophore with efficient fluorescent quantum yield that provides it an attractive candidate for fabricating effective materials for fluorescent probes and labeling studies. This study was financially supported by the Scientific and Technological Research Council of Turkey (TUBITAK Grant no. 117Z402).

Keywords: calixarene, OLED, supramolecular chemistry, synthesis

Procedia PDF Downloads 253

Authors: Amit Kumar, Jaikumar V, Pradeep AG, Shivakumar Bhavi

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Reducing sloshing is one of the major challenges in industries where transporting of liquid involved. The present study investigates the sloshing effect for different liquid levels 25%, 50%, and 75% of the tank capacity. CFD simulation for three different liquid levels has been carried out using a time-based multiphase Volume of fluid (VOF) scheme. Baffles were introduced to examine the sloshing effect inside the tank. Results were compared against the baseline case to assess the effectiveness of baffles. Maximum liquid height over the period of the simulation was considered as the parameter for measuring the sloshing effect inside the tank. It was found that the addition of baffles reduced the sloshing effect inside the tank as compared to the baseline model.

Keywords: sloshing, CFD, VOF, baffles

Procedia PDF Downloads 254

Authors: Kyoung Lee

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Numerous aerobic bacteria have the ability to form multicellular communities on the surface layer of the air-liquid (A-L) interface as a biofilm called a pellicle. Pellicles occupied at the A-L interface will benefit from the utilization of oxygen from air and nutrient from liquid. Buoyancy of cells can be obtained by high surface tension at the A-L interface. Thus, formation of pellicles is an adaptive advantage in utilization of excess nutrients in the standing culture where oxygen depletion is easily set up due to rapid cell growth. In natural environments, pellicles are commonly observed on the surface of lake or pond contaminated with pollutants. Previously, we have shown that when cultured in standing LB media an alkylphenol-degrading bacteria Pseudomonas alkylphenolia KL28 forms pellicles in a diameter of 0.3-0.5 mm with a thickness of ca 40 µm. The pellicles have unique features for possessing flatness and unusual rigidity. In this study, the biogenesis of the circular pellicles has been investigated by observing the cell organization at early stages of pellicle formation and cell arrangements in pellicle, providing a clue for highly organized cellular arrangement to be adapted to the air-liquid niche. Here, we first monitored developmental patterns of pellicle from monolayer to multicellular organization. Pellicles were shaped by controlled growth of constituent cells which accumulate extracellular polymeric substance. The initial two-dimensional growth was transited to multilayers by a constraint force of accumulated self-produced extracellular polymeric substance. Experiments showed that pellicles are formed by clonal growth and even with knock-out of genes for flagella and pilus formation. In contrast, the mutants in the epm gene cluster for alginate-like polymer biosynthesis were incompetent in cell alignment for initial two-dimensional growth of pellicles. Electron microscopic and confocal laser scanning microscopic studies showed that the fully matured structures are highly packed by matrix-encased cells which have special arrangements. The cells on the surface of the pellicle lie relatively flat and inside longitudinally cross packed. HPLC analysis of the extrapolysaccharide (EPS) hydrolysate from the colonies from LB agar showed a composition with L-fucose, L-rhamnose, D-galactosamine, D-glucosamine, D-galactose, D-glucose, D-mannose. However, that from pellicles showed similar neutral and amino sugar profile but missing galactose. Furthermore, uronic acid analysis of EPS hydrolysates by HPLC showed that mannuronic acid was detected from pellicles not from colonies, indicating the epm-derived polymer is critical for pellicle formation as proved by the epm mutants. This study verified that for the circular pellicle architecture P. alkylphenolica KL28 cells utilized EPS building blocks different from that used for colony construction. These results indicate that P. alkylphenolica KL28 is a clever architect that dictates unique cell arrangements with selected EPS matrix material to construct sophisticated building, circular biofilm pellicles.

Keywords: biofilm, matrix, pellicle, pseudomonas

Procedia PDF Downloads 152

Authors: B. Guezzen, M.A. Didi, B. Medjahed

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A factorial design of experiments and a response surface methodology were implemented to investigate the liquid-liquid extraction process of zinc (II) from acetate medium using the 1-Butyl-imidazolium di(2-ethylhexyl) phosphate [BIm⁺][D2EHP^-]. The optimization process of extraction parameters such as the initial pH effect (2.5, 4.5, and 6.6), ionic liquid concentration (1, 5.5, and 10 mM) and salt effect (0.01, 5, and 10 mM) was carried out using a three-level full factorial design (3³). The results of the factorial design demonstrate that all these factors are statistically significant, including the square effects of pH and ionic liquid concentration. The results showed that the order of significance: IL concentration > salt effect > initial pH. Analysis of variance (ANOVA) showing high coefficient of determination (R² = 0.91) and low probability values (P < 0.05) signifies the validity of the predicted second-order quadratic model for Zn (II) extraction. The optimum conditions for the extraction of zinc (II) at the constant temperature (20 °C), initial Zn (II) concentration (1mM) and A/O ratio of unity were: initial pH (4.8), extractant concentration (9.9 mM), and NaCl concentration (8.2 mM). At the optimized condition, the metal ion could be quantitatively extracted.

Keywords: ionic liquid, response surface methodology, solvent extraction, zinc acetate

Procedia PDF Downloads 374

Authors: Sathish K. Gurupatham, Farhad Sayedzada, Naji Dauk, Valmiki Sooklal, Laura Ruhala

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It was shown recently that small particles and powders spontaneously disperse on liquid surfaces when they come into contact with the interface for the first time. This happens due to the combined effect of the capillary force, buoyant weight of the particle and the viscous drag that the particle experiences in the liquid. The particle undergoes oscillations normal to the interface before it comes to rest on the interface. These oscillations, in turn, induce a flow on the interface which disperses the particles radially outward. This phenomenon has a significant role in the pollination of sea plants such as Ruppia in which the formation of ‘pollen rafts’ is the first step. This paper investigates, experimentally, the influence of the temperature of the liquid on which this dispersion occurs. It was observed that the frequency of oscillations of the particles decreased with the increase in the temperature of the liquid. It is because the magnitude of capillary force also decreased when the temperature of the liquid increased.

Keywords: particle dispersion, capillary force, viscous drag, oscillations

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Authors: Roya Moradifar, Naser Agharezaee

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In this paper corrosion in the liquid sulphur storage tank at South pars gas complex phases 2&3 is presented. This full hot insulated field-erected storage tanks are used for the temporary storage of 1800m3 of molten sulphur. Sever corrosion inside the tank roof was observed during over haul inspections, in the direction of roof gradient. Investigation shown, in spite of other parts of tank there was no insulation around these manholes. Internal steam coils do not maintain a sufficiently high tank roof temperature in the vapor space. Sulphur and formation of liquid water at cool metal surface, this combination leads to the formation of iron sulfide. By employing a distributed external heating system, the temperatures of any point of the tank roof should be based on ambient dew point and the liquid storage solidification point. Also other construction and operation of tank is more important. This paper will review potential corrosion mechanism and operational case study which illustrate the importance of heating systems.

Keywords: tank, steam, corrosion, sulphur

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Authors: S. Mousavian, F. Mousavian, V. Nikkhah Rashidabad

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Cubic equations of state like Redlich–Kwong (RK) EOS have been proved to be very reliable tools in the prediction of phase behavior. Despite their good performance in compositional calculations, they usually suffer from weaknesses in the predictions of saturated liquid density. In this research, RK equation was modified. The result of this study shows that modified equation has good agreement with experimental data.

Keywords: equation of state, modification, ammonia, genetic algorithm

Procedia PDF Downloads 382

Authors: A. D. Susanti, W. B. Sediawan, S. K. Wirawan, Budhijanto, Ritmaleni

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Rice bran oil contains significant amounts of oryzanol, a natural antioxidant that considered has higher antioxidant activity than vitamin E (tocopherol). Oryzanol reviewed has several health properties and interested in pharmacy, nutrition, and cosmetics. For practical usage, isolation and purification would be necessary due to the low concentration of oryzanol in crude rice bran oil (0.9-2.9%). Batch chromatography has proved as a promising process for the oryzanol recovery, but productivity was still low and scale-up processes of industrial interest have not yet been described. In order to improve productivity of batch chromatography, a continuous chromatography design namely Simulated Moving Bed (SMB) concept have been proposed. The SMB concept has interested for continuous commercial scale separation of binary system (oryzanol and rice bran oil), and rice bran oil still obtained as side product. Design of SMB chromatography for oryzanol separation requires quantification of its equilibrium. In this study, equilibrium of oryzanol separation conducted in batch adsorption using silica as the adsorbent and n-hexane/acetone (9:1) as the eluent. Three isotherm models, namely the Henry, Langmuir, and Freundlich equations, have been applied and modified for the experimental data to establish appropriate correlation for each sample. It turned out that the model quantitatively describe the equilibrium experimental data and will directed for design of SMB chromatography.

Keywords: adsorption, equilibrium, oryzanol, rice bran oil, simulated moving bed

Procedia PDF Downloads 283

Authors: Chol Min Yu, Sok Chol Ri

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The optimization of formation and growth of metallic nuggets during self-reduction of coal composite briquette (CCB here) is essential to increase the yield of valuable metals. The formation of metallic nuggets was investigated theoretically and experimentally during the reduction of coal composite briquette made from stainless steel dust and coal. The formation of metallic nuggets is influenced by slag viscosity and interfacial tension between the liquid metal and the slag in the reduced product. Surface tensions of liquid metal and slag are rather strong, respectively, due to the high basicity of its slag. Strong surface tensions of them lead to increase of interfacial tension between the liquid metal and the slag to be favorable to the growth of metallic nuggets. The viscosity of slag and interfacial tension between the liquid metal and the slag depends on the temperature and composition of the slag. The formation and the growth of metallic nuggets depend on carbon to oxygen ratio FC/O and temperature.

Keywords: stainless steel dust, coal-composite briquette, temperature, high basicity, interfacial tension

Procedia PDF Downloads 80

Authors: B. Y. Danjuma, A. Archibong-Eso, Aliyu M. Aliyu, H. Yeung

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In this experimental investigation, a new data for slugging frequency for high viscosity oil-gas flow are reported. Scale experiments were carried out using a mixture of air and mineral oil as the liquid phase in a 17 m long horizontal pipe with 0.0762 ID. The data set was acquired using two high-speed Gamma Densitometers at a data acquisition frequency of 250 Hz over a time interval of 30 seconds. For the range of flow conditions investigated, increase in liquid oil viscosity was observed to strongly influence the slug frequency. A comparison of the present data with prediction models available in the literature revealed huge discrepancies. A new correlation incorporating the effect of viscosity on slug frequency has been proposed for the horizontal flow, which represents the main contribution of this work.

Keywords: gamma densitometer, flow pattern, pressure gradient, slug frequency

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Authors: Stefano Frassinelli, Alessandro Niccolai, Riccardo E. Zich

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Sport performance analysis is a technique that is becoming every year more important for athletes of every level. Many techniques have been developed to measure and analyse efficiently the performance of athletes in some sports, but in combat sports these techniques found in many times their limits, due to the high interaction between the two opponents during the competition. In this paper the problem will be framed. Moreover the physical performance measurement problem will be analysed and three different techniques to manage it will be presented. All the techniques have been used to analyse the performance of 22 high level Judo athletes.

Keywords: sport performance, physical performance, judo, performance coefficients

Procedia PDF Downloads 413

Authors: B. Medjahed, M. A. Didi, B. Guezzen

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In the present work, emulsion liquid membrane (ELM) technique was applied for the extraction of cadmium(II) present in aqueous samples. Aliquat 336 (Chloride tri-N-octylmethylammonium) was used as carrier to extract cadmium(II). The main objective of this work is to investigate the influence of various parameters affected the ELM formation and its stability and testing the performance of the prepared ELM on removal of cadmium by using synthetic solution with different concentrations. Experiments were conducted to optimize pH of the feed solution and it was found that cadmium(II) can be extracted at pH 6.5. The influence of the carrier concentration and treat ratio on the extraction process was investigated. The obtained results showed that the optimal values are respectively 3% (Aliquat 336) and a ratio (feed: emulsion) equal to 1:1.

Keywords: cadmium, carrier, emulsion liquid membrane, surfactant

Procedia PDF Downloads 406

Authors: Siriporn Okonogi, Pimpak Phumat, Sakornrat Khongkhunthian

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Piper betle has been extensively reported for various pharmacological effects including antimicrobial activity. 4-Allylpyrocatechol (AC) is a principle active compound found in P. betle. However, AC has a problem of solubility in water. The aims of the present study were to prepare AC loaded polymeric micelles for enhancing its water solubility and to evaluate its anti-biofilm activity against oral phathogenic bacteria. AC was loaded in polymeric micelles (PM) of Pluronic F127 by using thin film hydration method to obtain AC loaded PM (PMAC). The results revealed that AC in the form of PMAC possessed high water solubility. PMAC particles were characterized using a transmission electron microscope and photon correlation spectroscopy. Determination of entrapment efficiency (EE) and loading capacity (LC) of PMAC was done by using high-performance liquid chromatography. The highest EE (86.33 ± 14.27 %) and LC (19.25 ± 3.18 %) of PMAC were found when the weight ratio of polymer to AC was 4 to 1. At this ratio, the particles showed spherical in shape with the size of 38.83 ± 1.36 nm and polydispersity index of 0.28 ± 0.10. Zeta potential of the particles is negative with the value of 16.43 ± 0.55 mV. Crystal violet assay and confocal microscopy were applied to evaluate the effects of PMAC on Streptococcus mutans biofilms using chlorhexidine (CHX) as a positive control. PMAC contained 1.5 mg/mL AC could potentially inhibit (102.01 ± 9.18%) and significantly eradicate (85.05 ± 2.03 %) these biofilms (p < 0.05). Comparison with CHX, PMAC showed slightly similar biofilm inhibition but significantly stronger biofilm eradication (p < 0.05) than CHX. It is concluded that PMAC can enhance water solubility and anti-biofilm activity of AC.

Keywords: pluronic, polymeric micelles, solubility, 4-allylpyrocathecol, Streptococcus mutans, anti-biofilm

Procedia PDF Downloads 144

Authors: Jian Yu

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Carbo dioxide (CO2) from fossil fuel combustion is a prime green-house gas emission. It can be mitigated by microalgae through conventional photosynthesis. The algal oil is a feedstock of biodiesel, a carbon neutral liquid fuel for transportation. The conventional CO2 fixation, however, is quite slow and affected by the intermittent solar irradiation. It is also a technical challenge to reform the bio-oil into a drop-in liquid fuel that can be directly used in the modern combustion engines with expected performance. Here, an artificial photosynthesis system is presented to produce a biopolyester and liquid fuels from CO2, water, and solar power. In this green process, solar energy is captured using photovoltaic modules and converted into hydrogen as a stable energy source via water electrolysis. The solar hydrogen is then used to fix CO2 by Cupriavidus necator, a hydrogen-oxidizing bacterium. Under the autotrophic conditions, CO2 was reduced to glyceraldehyde-3-phosphate (G3P) that is further utilized for cell growth and biosynthesis of polyhydroxybutyrate (PHB). The maximum cell growth rate reached 10.1 g L-1 day-1, about 25 times faster than that of a typical bio-oil-producing microalga (Neochloris Oleoabundans) under stable indoor conditions. With nitrogen nutrient limitation, a large portion of the reduced carbon is stored in PHB (C4H6O2)n, accounting for 50-60% of dry cell mass. PHB is a biodegradable thermoplastic that can find a variety of environmentally friendly applications. It is also a platform material from which small chemicals can be derived. At a high temperature (240 - 290 oC), the biopolyester is degraded into crotonic acid (C4H6O2). On a solid phosphoric acid catalyst, PHB is deoxygenated via decarboxylation into a hydrocarbon oil (C6-C18) at 240 oC or so. Aromatics and alkenes are the major compounds, depending on the reaction conditions. A gasoline-grade liquid fuel (77 wt% oil) and a biodiesel-grade fuel (23 wt% oil) were obtained from the hydrocarbon oil via distillation. The formation routes of hydrocarbon oil from crotonic acid, the major PHB degradation intermediate, are revealed and discussed. This work shows a novel green process from which biodegradable plastics and high-grade liquid fuels can be directly produced from carbon dioxide, water and solar power. The productivity of the green polyester (5.3 g L-1 d-1) is much higher than that of microalgal oil (0.13 g L-1 d-1). Other technical merits of the new green process may include continuous operation under intermittent solar irradiation and convenient scale up in outdoor.

Keywords: bioplastics, carbon dioxide fixation, drop-in liquid fuels, green process

Procedia PDF Downloads 189

Authors: Emad A. Shalaby

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Cancer is a disease that causes abnormal cell proliferation and invades nearby tissues. Lung cancer is the second most frequent cancer worldwide. Natural anti-cancer drugs have been developed with low side effects and toxicity. Citrus peels and extracts have been demonstrated to have significant pharmacological and physiological effects as a result of the high concentration of phenolic compounds found in citrus fruits, particularly peels. Tangerine peels can serve as an effective source of bioactive substances such as phenolics, flavonoids, and catechins, which have antioxidant, antibacterial, anticancer, and anti-inflammatory properties. Consequently, this work aims to determine the anticancer activity of ethanol extract of Tangerine peels against the A549 cell line and identify the phenolic compound profile (19 compounds) by using HPLC. Anticancer and antioxidant potentials of the extract were evaluated by MTT assay and TLC- TLC-bioautography sprayed with DPPH reagent, respectively. The obtained results revealed that tangerine peel extract showed significant activity against the A549 cell line with IC50 of 97.66 μg/mL. HPLC analysis proved that the highest concentration is naringenin 464.05 mg/g. More studies indicate that naringenin has significant anticancer potential on A549 cancer cells. The results showed that naringenin binds t0 EGFR protein in A549 with high binding affinity and thus may reduce lung cancer cell migration and enhance the apoptosis of cancer cells. From the obtained results it could be concluded that tangerine peel extract is an effective anti-cancer agent that may potentially serve as a natural therapeutic option for lung cancer treatment.

Keywords: tangerine peel, A549 cell line, anticancer, naringenin, HPLC analysis, naringenin, TLC bioautography

Procedia PDF Downloads 62

Authors: N. Bourayou, A. -H. Meniai, A. Gouaoura

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The presence of salt can either raise or lower the distribution coefficient of a solute acetic acid in liquid- liquid equilibria. The coefficient of solute is defined as the ratio of the composition of solute in solvent rich phase to the composition of solute in diluents (water) rich phase. The phenomena are known as salting–out or salting-in, respectively. The effect of monovalent salt, sodium chloride and the bivalent salt, sodium sulfate on the distribution of acetic acid between 1-butanol and water at 298.15K were experimentally shown to be effective in modifying the liquid-liquid equilibrium of water/acetic acid/1-butanol system in favour of the solvent extraction of acetic acid from an aqueous solution with 1-butanol, particularly at high salt concentrations of both salts. All the two salts studied are found to have to salt out effect for acetic acid in varying degrees. The experimentally measured data were well correlated by Eisen-Joffe equation. NRTL model for solvent mixtures containing salts was able to provide good correlation of the present liquid-liquid equilibrium data. Using the regressed salt concentration coefficients for the salt-solvent interaction parameters and the solvent-solvent interaction parameters obtained from the same system without salt. The calculated phase equilibrium was in a quite good agreement with the experimental data, showing the ability of NRTL model to correlate salt effect on the liquid-liquid equilibrium.

Keywords: activity coefficient, Eisen-Joffe, NRTL model, sodium chloride

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Authors: Indra Bahadur Bhandari, Narayan Panthi, Ishwar Koirala, Devendra Adhikari

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We have used a theoretical model based on the assumption of compound formation in binary alloys to study the thermodynamic, microscopic, and surface properties of Bi-Pb and In-Pb liquid alloys. A review of the phase diagrams for these alloys shows that one of the stable complexes for Bi-Pb liquid alloy is BiPb3; also, that InPb is a stable phase in liquid In-Pb alloys. Using the same interaction parameters that are fitted for the free energy of mixing, we have been able to compute the bulk and thermodynamic properties of the alloys. From our observations, we are able to show that the Bi-Pb liquid alloy exhibits compound formation over the whole concentration range and the In-Pb alloys undergo phase separation. With regards to surface properties, Pb segregates more to the surface in In-Pb alloys than in Bi-Pb alloys. The viscosity isotherms have a positive deviation from ideality for both Bi-Pb and In-Pb alloys.

Keywords: asymmetry, Bi-Pb, deviation, In-Pb, interaction parameters

Procedia PDF Downloads 160

Authors: Namsoo Kim, So-Hee Son, Jin-Soo Maeng, Yong-Jin Cho, Chong-Tai Kim

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It has been reported that some enzymes such as trypsin and Alcalase 2.4L are tolerant to a medium high pressure of 300 MPa and preparation of protein hydrolyzates under 300 MPa was advantageous with regard to hydrolysis rate and thus production yield compared with the counterpart under ambient pressure.1,2) In this study, nine fish comprising halibut, soft shell clam and carp were hydrolyzed using Flavourzyme 500MG only, and the combination of Flavourzyme 500 mg, Alcalase 2.4 L, Marugoto E, and Protamex under 300 MPa. Then, the effects of single and multiple protease treatments were determined with respect to contents of soluble solid (SS) and soluble nitrogen, sensory attributes, electrophoretic profiles, and HPLC peak patterns of the fish hydrolyzates (FHs) from various species. The contents of SS of the FHs were quite species-specific and the hydrolyzates of halibut showed the highest SS contents. At this point, multiple protease treatment increased SS content conspicuously in all fish tested. The contents of total soluble nitrogen and TCA-soluble nitrogen were well correlated with those of SS irrespective of fish species and methods of enzyme treatment. Also, it was noticed that multiple protease treatment improved sensory attributes of the FHs considerably. Electropherograms of the FHs showed fast migrating peptide bands that had the molecular masses mostly lower than 1 kDa and this was confirmed by peptide patterns from HPLC analysis for some FHs that had good sensory quality.

Keywords: production, fish hydrolyzates, protease treatments, high pressure

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Authors: Esmaeil Abbaszadeh Molaei, Zongyan Zhou, Aibing Yu

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The applications of liquid fluidizations have been increased in many parts of industries such as particle classification, backwashing of granular filters, crystal growth, leaching and washing, and bioreactors due to high-efficient liquid–solid contact, favorable mass and heat transfer, high operation flexibilities, and reduced back mixing of phases. In most of these multiphase operations the particles properties, i.e. size, density, and shape, may change during the process because of attrition, coalescence or chemical reactions. Previous studies, either experimentally or numerically, mainly have focused on studies of liquid-solid fluidized beds containing spherical particles; however, the role of particle shape on the hydrodynamics of liquid fluidized beds is still not well-known. A three-dimensional Discrete Element Model (DEM) and Computational Fluid Dynamics (CFD) are coupled to study the influence of particles shape on particles and liquid flow patterns in liquid-solid fluidized beds. In the simulations, ellipsoid particles are used to study the shape factor since they can represent a wide range of particles shape from oblate and sphere to prolate shape particles. Different particle shapes from oblate (disk shape) to elongated particles (rod shape) are selected to investigate the effect of aspect ratio on different flow characteristics such as general particles and liquid flow pattern, pressure drop, and particles orientation. First, the model is verified based on experimental observations, then further detail analyses are made. It was found that spherical particles showed a uniform particle distribution in the bed, which resulted in uniform pressure drop along the bed height. However for particles with aspect ratios less than one (disk-shape), some particles were carried into the freeboard region, and the interface between the bed and freeboard was not easy to be determined. A few particle also intended to leave the bed. On the other hand, prolate particles showed different behaviour in the bed. They caused unstable interface and some flow channeling was observed for low liquid velocities. Because of the non-uniform particles flow pattern for particles with aspect ratios lower (oblate) and more (prolate) than one, the pressure drop distribution in the bed was not observed as uniform as what was found for spherical particles.

Keywords: CFD, DEM, ellipsoid, fluidization, multiphase flow, non-spherical, simulation

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Authors: Natalia C. E. S. Nascimento, Mercia L. Oliveira, Fernando R. A. Lima, Leonardo T. C. do Nascimento, Marina B. Silveira, Brigida G. A. Schirmer, Andrea V. Ferreira, Carlos Malamut, Juliana B. da Silva

Abstract:

Tissue hypoxia is a common characteristic of solid tumors leading to decreased sensitivity to radiotherapy and chemotherapy. In the clinical context, tumor hypoxia assessment employing the positron emission tomography (PET) tracer ¹⁸F-fluoromisonidazole ([¹⁸F]FMISO) is helpful for physicians for planning and therapy adjusting. The aim of this work was to implement the synthesis of 18F-FMISO in a TRACERlab® MXFDG module and also to establish the quality control procedure. [¹⁸F]FMISO was synthesized at Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN/Brazil) using an automated synthesizer (TRACERlab® MXFDG, GE) adapted for the production of [¹⁸F]FMISO. The FMISO chemical standard was purchased from ABX. 18O- enriched water was acquired from Center of Molecular Research. Reagent kits containing eluent solution, acetonitrile, ethanol, 2.0 M HCl solution, buffer solution, water for injections and [¹⁸F]FMISO precursor (dissolved in 2 ml acetonitrile) were purchased from ABX. The [¹⁸F]FMISO samples were purified by Solid Phase Extraction method. The quality requirements of [¹⁸F]FMISO are established in the European Pharmacopeia. According to that reference, quality control of [¹⁸F]FMISO should include appearance, pH, radionuclidic identity and purity, radiochemical identity and purity, chemical purity, residual solvents, bacterial endotoxins, and sterility. The duration of the synthesis process was 53 min, with radiochemical yield of (37.00 ± 0.01) % and the specific activity was more than 70 GBq/µmol. The syntheses were reproducible and showed satisfactory results. In relation to the quality control analysis, the samples were clear and colorless at pH 6.0. The spectrum emission, measured by using a High-Purity Germanium Detector (HPGe), presented a single peak at 511 keV and the half-life, determined by the decay method in an activimeter, was (111.0 ± 0.5) min, indicating no presence of radioactive contaminants, besides the desirable radionuclide (¹⁸F). The samples showed concentration of tetrabutylammonium (TBA) < 50μg/mL, assessed by visual comparison to TBA standard applied in the same thin layer chromatographic plate. Radiochemical purity was determined by high performance liquid chromatography (HPLC) and the results were 100%. Regarding the residual solvents tested, ethanol and acetonitrile presented concentration lower than 10% and 0.04%, respectively. Healthy female mice were injected via lateral tail vein with [¹⁸F]FMISO, microPET imaging studies (15 min) were performed after 2 h post injection (p.i), and the biodistribution was analyzed in five-time points (30, 60, 90, 120 and 180 min) after injection. Subsequently, organs/tissues were assayed for radioactivity with a gamma counter. All parameters of quality control test were in agreement to quality criteria confirming that [¹⁸F]FMISO was suitable for use in non-clinical and clinical trials, following the legal requirements for the production of new radiopharmaceuticals in Brazil.

Keywords: automatic radiosynthesis, hypoxic tumors, pharmacopeia, positron emitters, quality requirements

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Authors: M. Y. Ismail, M. Inam

Abstract:

This paper presents the design and analysis of Liquid Crystal (LC) based tunable reflect array antenna with different design configurations within X-band frequency range. The effect of LC volume used for unit cell element on frequency tunability and reflection loss performance has been investigated. Moreover different slot embedded patch element configurations have been proposed for LC based tunable reflect array antenna design with enhanced performance. The detailed fabrication and measurement procedure for different LC based unit cells has been presented. The waveguide scattering parameter measured results demonstrated that by using the circular slot embedded patch elements, the frequency tunability and dynamic phase range can be increased from 180 MHz to 200 MHz and 120° to 124° respectively. Furthermore the circular slot embedded patch element can be designed at 10 GHz resonant frequency with a patch volume of 2.71 mm3 as compared to 3.47 mm3 required for rectangular patch without slot.

Keywords: liquid crystal, tunable reflect array, frequency tunability, dynamic phase range

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Authors: S. Jain, R. Savalia, V. Saini

Abstract:

A simple, accurate, precise, sensitive and specific RP-HPLC method was developed and validated for simultaneous estimation of Metoprolol Succinate and Olmesartan Medoxomil in bulk and tablet dosage form. The RP-HPLC method has shown adequate separation for Metoprolol Succinate and Olmesartan Medoxomil from its degradation products. The separation was achieved on a Phenomenex luna ODS C18 (250mm X 4.6mm i.d., 5μm particle size) with an isocratic mixture of acetonitrile: 50mM phosphate buffer pH 4.0 adjusted with glacial acetic acid in the ratio of 55:45 v/v. The mobile phase at a flow rate of 1.0ml/min, Injection volume 20μl and wavelength of detection was kept at 225nm. The retention time for Metoprolol Succinate and Olmesartan Medoxomil was 2.451±0.1min and 6.167±0.1min, respectively. The linearity of the proposed method was investigated in the range of 5-50μg/ml and 2-20μg/ml for Metoprolol Succinate and Olmesartan Medoxomil, respectively. Correlation coefficient was 0.999 and 0.9996 for Metoprolol Succinate and Olmesartan Medoxomil, respectively. The limit of detection was 0.2847μg/ml and 0.1251μg/ml for Metoprolol Succinate and Olmesartan Medoxomil, respectively and the limit of quantification was 0.8630μg/ml and 0.3793μg/ml for Metoprolol and Olmesartan, respectively. Proposed methods were validated as per ICH guidelines for linearity, accuracy, precision, specificity and robustness for estimation of Metoprolol Succinate and Olmesartan Medoxomil in commercially available tablet dosage form and results were found to be satisfactory. Thus the developed and validated stability indicating method can be used successfully for marketed formulations.

Keywords: metoprolol succinate, olmesartan medoxomil, RP-HPLC method, validation, ICH

Procedia PDF Downloads 315

Authors: ChunLoon Cha, HoYeon Lee, SangSoon Hwang

Abstract:

Mild combustion is characterized with its distinguished features, such as suppressed pollutant emission, homogeneous temperature distribution, reduced noise and thermal stress. However, most studies for MILD combustion have been focused on gas phase fuel. Therefore further study on MILD combustion using liquid fuel is needed for the application to liquid fueled gas turbine especially. In this work, we will focus on numerical simulation of the effects of diluent gas velocity on the formation of liquid fuel MILD combustion used in gas turbine area. A series of numerical simulations using Ansys fluent 18.2 have been carried out in order to investigate the detail effect of the flow field in the furnace on the formation of MILD combustion. The operating conditions were fixed at relatively lower heat intensity of 1.28 MW/m³ atm and various global equivalence ratios were changed. The results show that the local high temperature region was decreased and the flame temperature was uniformly distributed due to high velocity of diluted burnt gas. The increasing of diluted burnt gas velocity can be controlled by open ratio of adapter size. It was found that the maximum temperature became lower than 1800K and the average temperature was lower than 1500K that thermal NO formation was suppressed.

Keywords: MILD combustion, spray combustion, liquid fuel, diluent gas velocity, low NOx emission

Procedia PDF Downloads 231

Authors: K. Hiro, T. Wada

Abstract:

Thermodynamic properties of liquids under negative pressures are interesting and important in fields of scienceand technology. Here, phase transitions of a thermotropic liquid crystal are investigatedin a range from positive to negative pressures with a metal Berthelot tube using a commercial pressure transducer.Two co-existinglines, namely crystal (Kr) – nematic (N), and isotropic liquid (I) - nematic (N) lines, weredrawn in a pressure - temperature plane. The I-N line was drawn to ca. -5 (MPa).

Keywords: Berthelot method, liquid crystal, negative pressure, phase transitions

Procedia PDF Downloads 403

Authors: Bashar Al-Sabti, Jehad Harbali

Abstract:

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

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

Procedia PDF Downloads 95

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

Abstract:

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

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

Procedia PDF Downloads 420

Authors: Totik Sri Mariani, Sukrasno Isna, Tet Fatt Chia

Abstract:

Purwoceng (Pimpinella pruatjan Molk) is a legend plant used for increasing stamina by Kings in Java Island, Indonesia. Purpose of this study was to perform meristem culture and detected its stigmasterol by thin layer chromatography (TLC). Our result show that meristem culture could be propagated and grew into plantlet. After extracting intact acclimatized plant derived from meristem culture by hexane, we could detected stigmasterol by TLC. For suggestion, our extraction and TLC method could be used for detecting stigmasterol in others plant.

Keywords: purwoceng (pimpinella pruatjan), meristem culture, extraction, thin layer chromatography

Procedia PDF Downloads 430

Authors: Roihatul Mutiah, Sukardiman, Aty Widyawaruyanti

Abstract:

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

Keywords: calotropin, Calotropis gigantea, anticancer, marker active

Procedia PDF Downloads 333