Search results for: haloacetic acids
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 824

Search results for: haloacetic acids

644 Spectroscopic (Ir, Raman, Uv-Vis) and Biological Study of Copper and Zinc Complexes and Sodium Salt with Cichoric Acid

Authors: Renata Swislocka, Grzegorz Swiderski, Agata Jablonska-Trypuc, Wlodzimierz Lewandowski

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Forming a complex of a phenolic compound with a metal not only alters the physicochemical properties of the ligand (including increase in stability or changes in lipophilicity), but also its biological activity, including antioxidant, antimicrobial and many others. As part of our previous projects, we examined the physicochemical and antimicrobial properties of phenolic acids and their complexes with metals naturally occurring in foods. Previously we studied the complexes of manganese(II), copper(II), cadmium(II) and alkali metals with ferulic, caffeic and p-coumaric acids. In the framework of this study, the physicochemical and biological properties of cicoric acid, its sodium salt, and complexes with copper and zinc were investigated. Cichoric acid is a derivative of both caffeic acid and tartaric acid. It has first been isolated from Cichorium intybus (chicory) but also it occurs in significant amounts in Echinacea, particularly E. purpurea, dandelion leaves, basil, lemon balm and in aquatic plants, including algae and sea grasses. For the study of spectroscopic and biological properties of cicoric acid, its sodium salt, and complexes with zinc and copper a variety of methods were used. Studies of antioxidant properties were carried out in relation to selected stable radicals (method of reduction of DPPH and reduction of FRAP). As a result, the structure and spectroscopic properties of cicoric acid and its complexes with selected metals in the solid state and in the solutions were defined. The IR and Raman spectra of cicoric acid displayed a number of bands that were derived from vibrations of caffeic and tartaric acids moieties. At 1746 and 1716 cm-1 the bands assigned to the vibrations of the carbonyl group of tartaric acid occurred. In the spectra of metal complexes with cichoric these bands disappeared what indicated that metal ion was coordinated by the carboxylic groups of tartaric acid. In the spectra of the sodium salt, a characteristic wide-band vibrations of carboxylate anion occurred. In the spectra of cicoric acid and its salt and complexes, a number of bands derived from the vibrations of the aromatic ring (caffeic acid) were assigned. Upon metal-ligand attachment, the changes in the values of the wavenumbers of these bands occurred. The impact of metals on the antioxidant properties of cicoric acid was also examined. Cichoric acid has a high antioxidant potential. Complexation by metals (zinc, copper) did not significantly affect its antioxidant capacity. The work was supported by the National Science Centre, Poland (grant no. 2015/17/B/NZ9/03581).

Keywords: chicoric acid, metal complexes, natural antioxidant, phenolic acids

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643 Proximate Analysis of Muscle of Helix aspersa Living in Konya, Turkey

Authors: Ozcan Baris Citil

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The aim of the present study is the determination of the effects of variations in the proximate analysis, cholesterol content and fatty acid compositions of Helix aspersa. Garden snails (Helix aspersa) were picked up by hand from the Central Anatolia Region of Turkey, in autumn (November) in 2015. Fatty acid methyl esters (FAMEs) and cholesterol analysis were analyzed by gas chromatography (GC). The protein contents of snail muscle were determined with Kjeldahl distillation units. Statistical comparisons were made by using SPSS Software (version 16.0). Thirty different fatty acids of different saturation levels were detected. As the predominant fatty acids, stearic acid (C18:0), oleic acid (C18:1ω9), linoleic acid (C18:2ω6), palmitic acid (C16:0), arachidonic acid (C20:4ω6), eicosadienoic acid (C20:2) and linolenic acid (C18:3ω3) were found in Helix aspersa. Palmitic acid (C16:0) was identified as the major SFA in autumn. Linoleic acid (C18:2ω6), eicosadienoic acid (C20:2) and arachidonic acid (C20:4ω6) have the highest levels among the PUFAs. In the present study, ω3 were found 5.48% in autumn. Linolenic acid and omega-3 fatty acid amounts in the autumn decreased significantly but cholesterol content was not affected in Helix aspersa in autumn (November) in 2015.

Keywords: Helix aspersa, fatty acid, SFA, PUFA, cholesterol

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642 Utilization of Oat in Rabbit Feed for the Development of Healthier Rabbit Meat and Its Impact on Human Blood Lipid Profile

Authors: Muhammad Rizwan Tariq, Muhammad Issa Khan, Zulfiqar Ahmad, Muhammad Adnan Nasir, Muhammad Sameem Javed, Sheraz Ahmed

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Functional foods may be a good tool that can be simply utilized in reducing community health expenses. Regular consumption of rabbit meat can offer patrons with bioactive components because the manipulation in rabbit feed is much successful to raise the levels of conjugated linoleic acid, ecosapentaenoic acid, decosahexaenoic acid, polyunsaturated fatty acids, selenium, tocopherol etc. and to reduce the ω-3/ω-6 ratio which is performing a major role in curing of cardiovascular and several other diseases. In comparison to the meats of other species, rabbit meat has higher amounts of protein with essential amino acids, especially in the muscles and low cholesterol contents that also have elevated digestibility. The present study was carried out to develop the functional rabbit meat by modifying feed ingredient of rabbit diet. Thirty-day old rabbits were fed with feeds containing 2 % and 4 % oat. The feeding trial was carried out for eight weeks. Rabbits were divided into three different groups and reared for the period of two months. T0 rabbits were considered control group while T1 rabbits were reared on 4% oat, and T2 were on 2% oat in the feed. At the end of the 8 weeks, the rabbits were slaughtered. Results presented in this study concluded that 4 % oat seed supplementation enhanced n-3 PUFA in meat. It was observed that oat seed supplementation also reduced fat percentage in the meat. Utilization of oat in the feed of rabbits significantly affected the pH, protein, fat, textural and concentration of polyunsaturated fatty acids. A study trial was conducted in order to examine the impact of functional meat on the blood lipid profile of human subjects. They were given rabbit meat in comparison to the chicken meat for the period of one month. The cholesterol, triglycerides and low density lipoprotein were found to be lower in blood serum of human subject group treated with 4 % oat meat.

Keywords: functional food, functional rabbit meat, meat quality, rabbit

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641 Benzoxaboralone: A Boronic Acid with High Oxidative Stability and Utility in Biological Contexts

Authors: Brian J. Graham, Ronald T. Raines

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The presence of a nearly vacant p orbital on boron endows boronic acids with unique abilities as a catalyst and ligand. An organocatalytic process has been developed for the conversion of biomass-derived sugars to 5-hydroxymethylfurfural, which is a platform chemical. Specifically, 2-carboxyphenylboronic acid (2-CPBA) has been shown to be an optimal catalyst for this process, promoting the desired transformation in the absence of metals. The attributes of 2-CPBA as a catalyst led to additional investigations of its structure and reactivity. 2-CPBA was found to exist as a cyclized benzoxaborolone adduct rather than a free carboxylic acid. This cyclization has profound consequences for the oxidative stability of the boronic acid. Stereoelectronic effects within the oxaborolone ring destabilize the oxidation transition state by reducing electron donation from the cyclic oxygen to the developing p orbital on boron. That leads to a 10,000-fold increase in oxidative stability while maintaining the normal reactivity of boronic acids toward diols (e.g., carbohydrates) and nucleophiles in proteins while also presenting numerous hydrogen-bond accepting and donating groups. Thus, benzoxaborolones are useful in catalysis, chemical biology, medicinal chemistry, and allied fields.

Keywords: bioisosteres, boronic acid, catalysis, oxidative stability, pharmacophore, stereoelectronic effects

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640 Increase Daily Production Rate of Methane Through Pasteurization Cow Dung

Authors: Khalid Elbadawi Elshafea, Mahmoud Hassan Onsa

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This paper presents the results of the experiments to measure the impact of pasteurization cows dung on important parameter of anaerobic digestion (retention time) and measure the effect in daily production rate of biogas, were used local materials in these experiments, two experiments were carried out in two bio-digesters (1 and 2) (18.0 L), volume of the mixture 16.0-litre and the mass of dry matter in the mixture 4.0 Kg of cow dung. Pasteurization process has been conducted on the mixture into the digester 2, and put two digesters under room temperature. Digester (1) produced 268.5 liter of methane in period of 49 days with daily methane production rate 1.37L/Kg/day, and digester (2) produced 302.7-liter of methane in period of 26 days with daily methane production rate 2.91 L/Kg/day. This study concluded that the use of system pasteurization cows dung speed up hydrolysis in anaerobic process, because heat to certain temperature in certain time lead to speed up chemical reactions (transfer Protein to Amino acids, Carbohydrate to Sugars and Fat to Long chain fatty acids), this lead to reduce the retention time an therefore increase the daily methane production rate with 212%.

Keywords: methane, cow dung, daily production, pasteurization, increase

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639 Design of Black-Seed Pulp biomass-Derived New Bio-Sorbent by Combining Methods of Mineral Acids and High-Temperature for Arsenic Removal

Authors: Mozhgan Mohammadi, Arezoo Ghadi

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Arsenic is known as a potential threat to the environment. Therefore, the aim of this research is to assess the arsenic removal efficiency from an aqueous solution, with a new biosorbent composed of a black seed pulp (BSP). To treat BSP, the combination of two methods (i.e. treating with mineral acids and use at high temperature) was used and designed bio-sorbent called BSP-activated/carbonized. The BSP-activated and BSP-carbonized were also prepared using HCL and 400°C temperature, respectively, to compare the results of each three methods. Followed by, adsorption parameters such as pH, initial ion concentration, biosorbent dosage, contact time, and temperature were assessed. It was found that the combination method has provided higher adsorption capacity so that up to ~99% arsenic removal was observed with BSP-activated/carbonized at pH of 7.0 and 40°C. The adsorption capacity for BSP-carbonized and BSP-activated were 87.92% (pH: 7, 60°C) and 78.50% (pH: 6, 90°C), respectively. Moreover, adsorption kinetics data indicated the best fit with the pseudo-second-order model. The maximum biosorption capacity, by the Langmuir isotherm model, was also recorded for BSP-activated/carbonized (53.47 mg/g). It is notable that arsenic adsorption on studied bio sorbents takes place as spontaneous and through chemisorption along with the endothermic nature of the biosorption process and reduction of random collision in the solid-liquid phase.

Keywords: black seed pulp, bio-sorbents, treatment of sorbents, adsorption isotherms

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638 Effect of Sodium Chloride in the Recovery of Acetic Acid from Aqueous Solutions

Authors: Aidaoui Ahleme, Hasseine Abdelmalek

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Acetic acid is one of the simplest and most widely used carboxylic acids having many important chemical and industrial applications. Total worldwide production of acetic acid is about 6.5 million tonnes per year. A great deal of efforts has been made in developing feasible and economic method for recovery of carboxylic acids. Among them, Liquid-liquid extraction using aqueous two-phase systems (ATPS) has been demonstrated to be a highly efficient separation technique. The study of efficiently separating and recovering Acetic acid from aqueous solutions is an important significance on industry and environmentally sustainable development. Many research groups in different countries are working in this field and some methods are proposed in the literature. In this work, effect of sodium chloride with different content (5%, 10% and 20%) on the liquid-liquid equilibrium data of (water+ acetic acid+ DCM) system is investigated. The addition of the salt in an aqueous solution introduces ionic forces which affect liquid-liquid equilibrium and which influence directly the distribution coefficient of the solute. From the experimental results, it can be concluded that when the percentage of salt increases in the aqueous solution, the equilibrium between phases is modified in favor of the extracted phase.

Keywords: acetic acid recovery, aqueous solution, salting-effect, sodium chloride

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637 Flotation of Rare Earth Oxides from Iron-Oxide Silicate Rich Tailings Using Fatty Acids

Authors: George B. Abaka-Wood, Massimiliano Zanin, Jonas Addai-Mensah, William Skinner

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The versatility of froth flotation has made it vital in the beneficiation of rare earth elements minerals from either high or low-grade ores. There has been a significant increase in the quantity of iron oxide silicate-rich tailings generated from the extraction of primary commodities such as copper and gold in Australia, which have been identified to contain very low-grade rare earth oxides (≤ 1%). There is a vast knowledge gap in the beneficiation of rare earth oxides from such tailings. The aim of this research is to investigate the feasibility of using fatty acids as collectors for the flotation recovery and upgrade of rare earth oxides from selected iron-oxide silicate-rich tailings. Two forms of fatty acid collectors (oleic acid and sodium oleate) were tested in this investigation. Flotation tests were carried out using a 1.2 L Denver D-12 cell. The effects of pulp pH, fatty acid dosage, particle size distribution (-150 +75 µm, -75 +38 µm and -38 µm) and conventional depressants (sodium silicate and starch) dosage on flotation recovery of rare earth oxides were investigated. A comparison of the flotation results indicated that sodium oleate was the more efficient fatty acid for rare earth oxides flotation at all the pulp pH investigated. The flotation performance was found to be particle size-dependent. Both sodium silicate and starch were unselective in decreasing the recovery of iron oxides and silicate minerals, respectively with the corresponding decrease in rare earth oxides recovery. Generally, iron oxides and silicate minerals formed the substantial fraction of the flotation concentrates obtained, both in the absence and presence of depressants, resulting in a generally low rare earth oxides upgrade, even though rare earth oxides recoveries were high. The flotation tests carried out on the tailings sample suggest the feasibility of rare earth oxides recovery using fatty acids, although particle size distribution and minerals liberation are key limiting factors in achieving selective rare earth oxides upgrade.

Keywords: depressants, flotation, oleic acid, sodium oleate

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636 Heterogeneous Catalytic Hydroesterification of Soybean Oil to Develop a Biodiesel Formation

Authors: O. Mowla, E. Kennedy, M. Stockenhuber

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Finding alternative renewable resources of energy has attracted the attentions in consequence of limitation of the traditional fossil fuel resources, increasing of crude oil price and environmental concern over greenhouse gas emissions. Biodiesel (or Fatty Acid Methyl Esters (FAME)), an alternative energy source, is synthesised from renewable sources such as vegetable oils and animal fats and can be produced from waste oils. FAME can be produced via hydroesterification of oils. The process involves two stages. In the first stage of this process, fatty acids and glycerol are being obtained by hydrolysis of the feed stock oil. In the second stage, the recovered fatty acids are then esterified with an alcohol to methyl esters. The presence of a catalyst accelerates the rate of the hydroesterification reaction of oils. The overarching aim of this study is to find the effect of using zeolite as a catalyst in the heterogeneous hydroesterification of soybean oil. Both stages of the catalytic hydroesterification of soybean oil had been conducted at atmospheric and high-pressure conditions using reflux glass reactor and Parr reactor, respectively. The effect of operating parameters such as temperature and reaction time on the overall yield of biodiesel formation was also investigated.

Keywords: biodiesel, heterogeneous catalytic hydroesterification, soybean oil, zeolite

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635 Liquid-Liquid Extraction of Uranium(vi) from Aqueous Solution Using 1-Hydroxyalkylidene-1,1-Diphosphonic Acids

Authors: M. Bouhoun Ali, A. Y. Badjah Hadj Ahmed, M. Attou, A. Elias, M. A. Didi

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The extraction of uranium(VI) from aqueous solutions has been investigated using 1-hydroxyhexadecylidene-1,1-diphosphonic acid (HHDPA) and 1-hydroxydodecylidene-1,1-diphosphonic acid (HDDPA), which were synthesized and characterized by elemental analysis and by FT-IR, 1H NMR, 31P NMR spectroscopy. In this paper, we propose a tentative assignment for the shifts of those two ligands and their specific complexes with uranium(VI). We carried out the extraction of uranium(VI) by HHDPA and HDDPA from [carbon tetrachloride + 2-octanol (v/v: 90%/10%)] solutions. Various factors such as contact time, pH, organic/aqueous phase ratio and extractant concentration were considered. The optimum conditions obtained were: contact time= 20 min, organic/aqueous phase ratio = 1, pH value = 3.0 and extractant concentration = 0.3M. The extraction yields are more significant in the case of the HHDPA which is equipped with a hydrocarbon chain, longer than that of the HDDPA. Logarithmic plots of the uranium(VI) distribution ratio vs. pHeq and the extractant concentration showed that the ratio of extractant to extracted uranium(VI) (ligand/metal) is 2:1. The formula of the complex of uranium(VI) with the HHDPA and the DHDPA is UO2(H3L)2 (HHDPA and DHDPA are denoted as H4L). A spectroscopic analysis has showed that coordination of uranium(VI) takes place via oxygen atoms.

Keywords: liquid-liquid extraction, uranium(vi), 1-hydroxyalkylidene-1, 1-diphosphonic acids, hhdpa, hddpa, aqueous solution

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634 Recovery and Εncapsulation of Μarine Derived Antifouling Agents

Authors: Marina Stramarkou, Sofia Papadaki, Maria Kaloupi, Ioannis Batzakas

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Biofouling is a complex problem of the aquaculture industry, as it reduces the efficiency of the equipment and causes significant losses of cultured organisms. Nowadays, the current antifouling methods are proved to be labor intensive, have limited lifetime and use toxic substances that result in fish mortality. Several species of marine algae produce a wide variety of biogenic compounds with antibacterial and antifouling properties, which are effective in the prevention and control of biofouling and can be incorporated in antifouling coatings. In the present work, Fucus spiralis, a species of macro algae, and Chlorella vulgaris, a well-known species of microalgae, were used for the isolation and recovery of bioactive compounds, belonging to groups of fatty acids, lipopeptides and amides. The recovery of the compounds was achieved through the application of the ultrasound- assisted extraction, an environmentally friendly method, using green, non-toxic solvents. Moreover, the coating of the antifouling agents was done by innovative encapsulation and coating methods, such as electro-hydrodynamic process. For the encapsulation of the bioactive compounds natural matrices were used, such as polysaccharides and proteins. Water extracts that were incorporated in protein matrices were considered the most efficient antifouling coating.

Keywords: algae, electrospinning, fatty acids, ultrasound-assisted extraction

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633 Malachite Green and Red Congo Dyes Adsorption onto Chemical Treated Sewage Sludge

Authors: Zamouche Meriem, Mehcene Ismahan, Temmine Manel, Bencheikh Lehocine Mosaab, Meniai Abdeslam Hassen

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In this study, the adsorption of Malachite Green (MG) by chemical treated sewage sludge has been studied. The sewage sludge, collected from drying beds of the municipal wastewater treatment station of IBN ZIED, Constantine, Algeria, was treated by different acids such us HNO₃, H₂SO₄, H₃PO₄ for modifying its aptitude to removal the MG from aqueous solutions. The results obtained shows that the sewage sludge activated by sulfuric acid give the highest elimination amounts of MG (9.52 mg/L) compared by the other acids used. The effects of operation parameters have been investigated, the results obtained show that the adsorption capacity per unit of adsorbent mass decreases from 18.69 to 1.20 mg/g when the mass of the adsorbent increases from 0.25 to 4 g respectively, the optimum mass for which a maximum of elimination of the dye is equal to 0.5g. The increasing in the temperature of the solution results in a slight decrease in the adsorption capacity of the chemically treated sludge. The highest amount of dye adsorbed by CSSS (9.56 mg/g) was observed for the optimum temperature of 25°C. The chemical activated sewage sludge proved its effectiveness for the removal of the Red Congo (RC), but by comparison the adsorption of the two dyes studies, we noted that the sludge has more affinity to adsorb the (MG).

Keywords: adsorption, chemical activation, malachite green, sewage sludge

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632 Two Step Biodiesel Production from High Free Fatty Acid Spent Bleaching Earth

Authors: Rajiv Arora

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Biodiesel may be economical if produced from inexpensive feedstock which commonly contains high level of free fatty acids (FFA) as an inhibitor in production of methyl ester. In this study, a two-step process for biodiesel production from high FFA spent bleach earth oil in a batch reactor is developed. Oil sample extracted from spent bleaching earth (SBE) was utilized for biodiesel process. In the first step, FFA of the SBE oil was reduced to 1.91% through sulfuric acid catalyzed esterification. In the second step, the product prepared from the first esterification process was carried out transesterification with an alkaline catalyst. The influence of four variables on conversion efficiency to methyl ester, i.e., methanol/ SBE oil molar ratio, catalyst amount, reaction temperature and reaction time, was studied in the second stage. The optimum process variables in the transesterification were methanol/oil molar ratio 6:1, heterogeneous catalyst conc. 5 wt %, reaction temperature 65 °C and reaction time 60 minutes to produce biodiesel. Major fuel properties of SBE biodiesel were measured to comply with ASTM and EN standards. Therefore, an optimized process for production of biodiesel from a low-cost high FFA source was accomplished.

Keywords: biodiesel, esterification, free fatty acids, residual oil, spent bleaching earth, transesterification

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631 Homeostatic Analysis of the Integrated Insulin and Glucagon Signaling Network: Demonstration of Bistable Response in Catabolic and Anabolic States

Authors: Pramod Somvanshi, Manu Tomar, K. V. Venkatesh

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Insulin and glucagon are responsible for homeostasis of key plasma metabolites like glucose, amino acids and fatty acids in the blood plasma. These hormones act antagonistically to each other during the secretion and signaling stages. In the present work, we analyze the effect of macronutrients on the response from integrated insulin and glucagon signaling pathways. The insulin and glucagon pathways are connected by DAG (a calcium signaling component which is part of the glucagon signaling module) which activates PKC and inhibits IRS (insulin signaling component) constituting a crosstalk. AKT (insulin signaling component) inhibits cAMP (glucagon signaling component) through PDE3 forming the other crosstalk between the two signaling pathways. Physiological level of anabolism and catabolism is captured through a metric quantified by the activity levels of AKT and PKA in their phosphorylated states, which represent the insulin and glucagon signaling endpoints, respectively. Under resting and starving conditions, the phosphorylation metric represents homeostasis indicating a balance between the anabolic and catabolic activities in the tissues. The steady state analysis of the integrated network demonstrates the presence of a bistable response in the phosphorylation metric with respect to input plasma glucose levels. This indicates that two steady state conditions (one in the homeostatic zone and other in the anabolic zone) are possible for a given glucose concentration depending on the ON or OFF path. When glucose levels rise above normal, during post-meal conditions, the bistability is observed in the anabolic space denoting the dominance of the glycogenesis in liver. For glucose concentrations lower than the physiological levels, while exercising, metabolic response lies in the catabolic space denoting the prevalence of glycogenolysis in liver. The non-linear positive feedback of AKT on IRS in insulin signaling module of the network is the main cause of the bistable response. The span of bistability in the phosphorylation metric increases as plasma fatty acid and amino acid levels rise and eventually the response turns monostable and catabolic representing diabetic conditions. In the case of high fat or protein diet, fatty acids and amino acids have an inhibitory effect on the insulin signaling pathway by increasing the serine phosphorylation of IRS protein via the activation of PKC and S6K, respectively. Similar analysis was also performed with respect to input amino acid and fatty acid levels. This emergent property of bistability in the integrated network helps us understand why it becomes extremely difficult to treat obesity and diabetes when blood glucose level rises beyond a certain value.

Keywords: bistability, diabetes, feedback and crosstalk, obesity

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630 Synthesis, Density Functional Theory (DFT) and Antibacterial Studies of Highly Functionalized Novel Spiropyrrolidine 4-Quinolone-3-Carboxylic Acids Derived from 6-Acetyl Quinolone

Authors: Thangaraj Arasakumar, Athar Ata, Palathurai Subramaniam Mohan

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A series of novel 4-quinolone-3-carboxylic acid grafted spiropyrrolidines as new type of antibacterial agents were synthesized via multicomponent 1,3-dipolar cycloaddition reaction of an azomethine ylides with a newly prepared (E)-4-oxo-6-(3-phenyl-acryloyl)-1,4-dihydro-quinoline-3-carboxylic acids in high regioselectivity with good yields. The structure of cycloadduct characterized by FT IR, mass, 1H, 13C, 2D NMR techniques and elemental analysis. Structure and spectrometry of compound 8a has been investigated theoretically by using HF and DFT approach at B3LYP, M05-2x/6-31G* levels of theories. The optimized geometries and calculated vibrational frequencies are evaluated via comparison with experimental values. A good agreement is found between the measured and calculated values. The DFT studies support the molecular mechanism of this cycloaddition reaction and determine the molecular electrostatic potential and thermodynamic properties. Furthermore, the antibacterial activities of synthesized compounds were evaluated against Gram-positive bacteria (Staphylococcus aureus, Bacillus subtilis) and Gram-negative bacteria strains (Escherichia coli, Klebsiella pneumoniae). Among 21 compounds screened, 8f and 8p were found to be more active against tested bacteria.

Keywords: antibacterial activity, azomethine ylide, DFT calculation, spirooxindole

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629 Dipeptide Functionalized Nanoporous Anodic Aluminium Oxide Membrane for Capturing Small Molecules

Authors: Abdul Mutalib Md Jani, Abdul Hadi Mahmud, Mohd Tajuddin Mohd Ali

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The rapid growth of interest in surface modification of nanostructures materials that exhibit improved structural and functional properties is attracting more researchers. The unique properties of highly ordered nanoporous anodic aluminium oxide (NAAO) membrane have been proposed as a platform for biosensing applications. They exhibit excellent physical and chemical properties with high porosity, high surface area, tunable pore sizes and excellent chemical resistance. In this study, NAAO was functionalized with 3-aminopropyltriethoxysilane (APTES) to prepared silane-modified NAAO. Amine functional groups are formed on the surface of NAAO during silanization and were characterized using Fourier Transform Infrared spectroscopy (FTIR). The synthesis of multi segment of peptide on NAAO surfaces can be realized by changing the surface chemistry of the NAAO membrane via click chemistry. By click reactions, utilizing alkyne terminated with amino group, various peptides tagged on NAAO can be envisioned from chiral natural or unnatural amino acids using standard coupling methods (HOBt, EDCI and HBTU). This strategy seemly versatile since coupling strategy of dipeptide with another amino acids, leading to tripeptide, tetrapeptide or pentapeptide, can be synthesized without purification. When an appropriate terminus is selected, multiple segments of amino acids can be successfully synthesized on the surfaces. The immobilized NAAO should be easily separated from the reaction medium by conventional filtration, thus avoiding complicated purification methods. Herein, we proposed to synthesize multi fragment peptide as a model for capturing and attaching various small biomolecules on NAAO surfaces and can be also applied as biosensing device, drug delivery systems and biocatalyst.

Keywords: nanoporous anodic aluminium oxide, silanization, peptide synthesise, click chemistry

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628 Effect of Chitosan and Ascorbic Acid Coating on the Refrigerated Tilapia Fish Fillet (Oreochromis niliticus)

Authors: Jau-Shya Lee, Rossita Shapawi, Vin Cent Pua

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Tilapia is a popular cultured fresh-water fish in Malaysia. The highly perishable nature of the fish and increasing demand for high-quality ready-to-cook fish has intensified the search for better fish preservation method. Chitosan edible coating has been evident to extend the shelf life of fish fillet. This work was attempted to explore the potential of ascorbic acid in enhancing the shelf life extension ability of chitosan coated Tilapia fillet under refrigeration condition (4 ± 1oC). A 3 2 Factorial Design which comprising of three concentrations of chitosan (1, 1.5 and 2%) and two concentrations of ascorbic acids (2.5 and 5%) was used. The fish fillets were analyzed for total viable count, thiobarbituric acid (TBA) value, pH, aw and colour changes at 3-day interval over 15-day storage. The shelf life of chitosan coated (1.5% and 2%) fillet was increased to 15 days as compared to uncoated fish fillet which can only last for nine days. The inhibition of microbial growth of fish fillet was enhanced with the addition of 5% of ascorbic acids in 2% of chitosan. The TBA value, pH and aw for chitosan coated samples were found lower than that of uncoated sample (p<0.05). The colour stability of the fish fillet was also improved by the composite coating. Overall, 2% of chitosan and 5% of ascorbic acid formed the most effective coating to enhance the quality and to lengthen the shelf life of refrigerated Tilapia fillet.

Keywords: ascorbic acid, chitosan, edible coating, fish fillet

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627 Food Waste and Sustainable Management

Authors: Farhana Nosheen, Moeez Ahmad

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Throughout the food chain, the food waste from initial agricultural production to final household consumption has become a serious concern for global sustainability because of its adverse impacts on food security, natural resources, the environment, and human health. About a third of tomatoes (Lycopersicon esculentum L.) delivered to processing plants end as processing waste. The amount of such waste material is estimated to have increased with the emergence of mechanical harvesting. Experiments were made to determine the nutritional profile and antioxidant activity of tomato processing waste and to explore the bioactive compound in tomato waste, i.e., Lycopene. Tomato Variety of ‘SAHARA F1’ was used to make tomato waste. The tomatoes were properly cleaned, and then unwanted impurities were removed properly. The tomatoes were blanched at 90 ℃ for 5 minutes. After which, the skin of the tomatoes was removed, and the remaining part passed through the electric pulper. The pulp and seeds were collected separately. The seeds and skin of tomatoes were mixed and saved in a sterilized jar. The samples of tomato waste were found to contain 89.11±0.006 g/100g moisture, 10.13±0.115 g/100g protein, 2.066±0.57 g/100g fat, 4.81±0.10 g/100g crude fiber, and 4.06±0.057 g/100g ash and NFE 78.92±0.066 g/100g. The results confirmed that tomato waste contains a considerable amount of Lycopene 51.0667±0.00577 mg/100g and exhibited good antioxidant properties. Total phenolics showed average contents of 122.9600±0.01000 mg GAE/100g, of which flavonoids accounted for 41.5367±0.00577 mg QE/100g. Antioxidant activity of tomato processing waste was found 0.6833±0.00577 mmol Trolox/100g. Unsaturated fatty acids represent the major portion of total fatty acids, Linoleic acid being the major one. The mineral content of tomato waste showed a good amount of potassium 3030.1767 mg/100g and calcium 131.80 mg/100g, respectively were present in it. These findings suggest that tomato processing waste is rich in nutrients, antioxidants, fatty acids, and minerals. I recommend that this waste should be sun-dried to be used in the combination of feed of the animals. It can also be used in making some other products like lycopene tea or several other health-beneficial products.

Keywords: food waste, tomato, bioactive compound, sustainable management

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626 Oxidative Stability of an Iranian Ghee (Butter Fat) Versus Soybean Oil During Storage at Different Temperatures

Authors: Kooshan Nayebzadeh, Maryam Enteshari

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In this study, the oxidative stability of soybean oil under different storage temperatures (4 and 25 ˚C) and during 6-month shelf-life was investigated by various analytical methods and headspace-liquid phase microextraction (HS-LPME) coupled to gas chromatography-mass spectrometry (GC-MS). Oxidation changes were monitored by analytical parameters consisted of acid value (AV), peroxide value (PV), p-Anisidine value (p-AV), thiobarbituric acid value (TBA), fatty acids profile, iodine value (IV) and oxidative stability index (OSI). In addition, concentrations of hexanal and heptanal as secondary volatile oxidation compounds were determined by HS-LPME/GC-MS technique. Rate of oxidation in soybean oil which stored at 25 ˚C was so higher. The AV, p-AV, and TBA were gradually increased during 6 months, while the amount of unsaturated fatty acids, IV, and OSI decreased. Other parameters included concentrations of both hexanal and heptanal, and PV exhibited increasing trend during primitive months of storage; then, at the end of third and fourth months a sudden decrement was understood for the concentrations of hexanal and heptanal and the amount of PV, simultaneously. The latter parameters increased again until the end of shelf-time. As a result, the temperature and time were effective factors in oxidative stability of soybean oil. Also intensive correlations were found for soybean oil at 4 ˚C between AV and TBA (r2=0.96), PV and p-AV (r2=0.9), IV and TBA (-r2=0.9), and for soybean oil stored at 4 ˚C between p-AV and TBA (r2=0.99).

Keywords: headspace-liquid phase microextraction, oxidation, shelf-life, soybean oil

Procedia PDF Downloads 365
625 Phenolic Rich Dry Extracts and Their Antioxidant Activity

Authors: R. Raudonis, L. Raudonė, V. Janulis, P. Viškelis

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Pharmacological and clinical studies demonstrated that phenolic compounds particularly flavonoids and phenolic acids are responsible for a wide spectrum of therapeutic activities. Flavonoids and phenolic acids are regarded as natural antioxidants that play an important role in protecting cells from oxidative stress. Qualitatively prepared dry extracts possess high stability and concentration of bio active compounds, facility of standardization and quality control. The aim of this work was to determine the phenolic and antioxidant profiles of Hippophaë rhamnoides L., Betula pendula Roth., Tilia cordata Mill., Sorbus aucuparia L. leaves dry extracts and to identify markers of antioxidant activity. Extracts were analyzed using high-performance liquid chromatography (HPLC) with FRAP post-column assay. Dry extracts are versatile forms possessing wide area of applications, final product ensure consistent phytochemical and functional properties. Seven flavonoids: rutin, hyperoside, isorhamnetin 3-O-rutinoside, isorhamnetin 3-O-glucoside, quercetin, kaempferol, isorhamnetin were identified in dry extract of Hippophaë rhamnoides L. leaves. Predominant compounds were flavonol glycosides which were chosen as markers for quantitative control of dry extracts. Chlorogenic acid, hyperoside, rutin, quercetin, isorhamnetin were prevailing compounds in Betula pendula Roth. leaves extract, whereas strongest ferric reducing activity was determined for chlorogenic acid and hyperoside. Notable amounts of protocatechuic acid and flavonol glycosides, rutin, hyperoside, quercitrin, isoquercitrin were identified in the chromatographic profile of Tilia cordata Mill. Neochlorogenic and chlorogenic acids were significantly dominant compounds in antioxidant profile in dry extract of Sorbus aucuparia L. leaves. Predominant compounds of antioxidant profiles could be proposed as functional markers of quality of phenolic rich raw materials. Dry extracts could be further used for manufacturing of pharmaceutical and nutraceuticals.

Keywords: dry extract, FRAP, antioxidant activity, phenolic

Procedia PDF Downloads 470
624 Protecting Physicochemical Properties of Black Cumin Seed (Nigella sativa) Oil and Developing Value Added Products

Authors: Zeliha Ustun, Mustafa Ersoz

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In the study, a traditional herbal supplement black cumin seed (Nigella sativa) oil properties has been studied to protect the main quality parameters by a new supplement application. Black cumin seed and its oil is used as a dietary supplement and preferred traditional remedy in Africa, Asia and Middle East for centuries. Now it has been consuming by millions of people in America and Europe as natural supplements and/or phytotherapeutic agents to support immune system, asthma, allergic rinnitis etc. by the scientists’ advices. With the study, it is aimed to prove that soft gelatin capsules are a new and more practical way of usage for Nigella sativa oil that has a longer stability. With the study soft gelatin capsules formulation has been developed to protect cold pressed black cumin seed oil physicochemical properties for a longer period. The product design has been developed in laboratory and implemented in pilot scale soft gelatin capsule manufacturing. Physicochemical properties (peroxide value, free fatty acids, fatty acid composition, refractive index, iodine value, saponification value, unsaponifiable matters) of Nigella sativa oil soft gelatin capsules and Nigella sativa oil in liquid form in amber glass bottles have been compared and followed for 8 months. The main parameters for capsules and liquid form found that for free fatty acids 2.29±0.03, 3.92±0.11 % oleic acid, peroxide 23.11±1.18, 27.85±2.50 meqO2/kg, refractive index at 20 0C 1.4738±0.00, 1.4737±0.00, soap 0 ppm, moisture and volatility 0.32±0.01, 0.36±0.01 %, iodine value 123.00±0.00, 122.00±0.00 wijs, saponification value 196.25±0.46, 194.13±0.35 mg KOH/g and unsaponifiable matter 7.72±0.13, 6.88±0.36 g/kg respectively. The main fatty acids are found that linoleic acid 56.17%, oleic acid 24.64%, palmitic acid 11,94 %. As a result, it is found that cold pressed Nigella sativa oil soft gelatin capsules physicochemical properties are more stable than the Nigella sativa oil stored in glass bottles.

Keywords: black cumin seed (Nigella sativa) oil, cold press, nutritional supplements, soft gelatin capsule

Procedia PDF Downloads 334
623 Effects of Excess-Iron Stress on Symbiotic Nitrogen Fixation Efficiency of Yardlong-Bean Plants

Authors: Hong Li, Tingxian Li, Xudong Wang, Qinghuo Lin

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Excess-iron (Fe) stresses involved in legume symbiotic nitrogen fixation are not understood. Our objectives were to investigate the tolerance of yardlong-bean plants to soil excess-Fe stress and antagonistic effects of organic amendments and rhizobial inoculants on plant root nodulation and stem ureide formation. The study was conducted in the tropical Hainan Island during 2012-2013. The soil was strongly acidic (pH 5.3±0.4) and highly variable in Fe concentrations(596±79 mg/kg). The treatments were arranged in a split-plot design with three blocks. The treatment effects were significant on root nodulation, stem ureide, amino acids, plant N/Fe accumulation and bean yields (P<0.05). The yardlong-bean stem allantoin, amino acids and nitrate concentrations and relative ureide % declined with high soil Fe concentrations (>300 mg/kg). It was concluded that the co-variance of excess Fe stress could inhibit legume symbiotic N fixation efficiency. Organic amendments and rhizobial inoculants could help improve crop tolerance to excess Fe stress.

Keywords: atmospheric N fixation, root nodulation, soil Fe co-variance, stem ureide, yardlong-bean plants

Procedia PDF Downloads 247
622 Transition in Protein Profile, Maillard Reaction Products and Lipid Oxidation of Flavored Ultra High Temperature Treated Milk

Authors: Muhammad Ajmal

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- Thermal processing and subsequent storage of ultra-heat treated (UHT) milk leads to alteration in protein profile, Maillard reaction and lipid oxidation. Concentration of carbohydrates in normal and flavored version of UHT milk is considerably different. Transition in protein profile, Maillard reaction and lipid oxidation in UHT flavored milk was determined for 90 days at ambient conditions and analyzed at 0, 45 and 90 days of storage. Protein profile, hydroxymethyl furfural, furosine, Nε-carboxymethyl-l-lysine, fatty acid profile, free fatty acids, peroxide value and sensory characteristics were determined. After 90 days of storage, fat, protein, total solids contents and pH were significantly less than the initial values determined at 0 day. As compared to protein profile normal UHT milk, more pronounced changes were recorded in different fractions of protein in UHT milk at 45 and 90 days of storage. Tyrosine content of flavored UHT milk at 0, 45 and 90 days of storage were 3.5, 6.9 and 15.2 µg tyrosine/ml. After 45 days of storage, the decline in αs1-casein, αs2-casein, β-casein, κ-casein, β-lactoglobulin, α-lactalbumin, immunoglobulin and bovine serum albumin were 3.35%, 10.5%, 7.89%, 18.8%, 53.6%, 20.1%, 26.9 and 37.5%. After 90 days of storage, the decline in αs1-casein, αs2-casein, β-casein, κ-casein, β-lactoglobulin, α-lactalbumin, immunoglobulin and bovine serum albumin were 11.2%, 34.8%, 14.3%, 33.9%, 56.9%, 24.8%, 36.5% and 43.1%. Hydroxy methyl furfural content of UHT milk at 0, 45 and 90 days of storage were 1.56, 4.18 and 7.61 (µmol/L). Furosine content of flavored UHT milk at 0, 45 and 90 days of storage intervals were 278, 392 and 561 mg/100g protein. Nε-carboxymethyl-l-lysine content of UHT flavored milk at 0, 45 and 90 days of storage were 67, 135 and 343mg/kg protein. After 90 days of storage of flavored UHT milk, the loss of unsaturated fatty acids 45.7% from the initial values. At 0, 45 and 90 days of storage, free fatty acids of flavored UHT milk were 0.08%, 0.11% and 0.16% (p<0.05). Peroxide value of flavored UHT milk at 0, 45 and 90 days of storage was 0.22, 0.65 and 2.88 (MeqO²/kg). Sensory analysis of flavored UHT milk after 90 days indicated that appearance, flavor and mouth feel score significantly decreased from the initial values recorded at 0 day. Findings of this investigation evidenced that in flavored UHT milk more pronounced changes take place in protein profile, Maillard reaction products and lipid oxidation as compared to normal UHT milk.

Keywords: UHT flavored milk , hydroxymethyl furfural, lipid oxidation, sensory properties

Procedia PDF Downloads 173
621 Preliminary Study of Fermented Pickle of Tabah Bamboo Shoot: Gigantochloa nigrociliata (Buese) Kurz

Authors: Luh Putu T. Darmayanti, A. A. Duwipayana, I. Nengah K. Putra, Nyoman S. Antara

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Tabah Bamboo (Gigantochloa nigrociliata (Buese) Kurz) is the indigenous bamboo species which grows in District of Pupuan, Tabanan at Province of Bali. Compared to the others, this shoot has low concentration of hydrocyanide acid (HCN). However, as found for almost of bamboo shoot, its seasonal availability, perishable in nature, and short-lived. This study aimed to gather information about total of lactic acid bacteria (LAB), pH, total acidity, HCN content, detection of LAB’s type involved during fermentation, and organic acids’ profiles of fermented pickles of Tabah bamboo shoot. The pickle was made by natural fermentation with 6 % salt concentration and fermentation conducted for 13 days. The result showed during the fermentation time, in the fourth day we found LAB’s number was highest as much as 72 x 107 CFU/ml and the lowest pH was 3.09. We also found decreasing in HCN from 37.8 ppm at the beginning to 20.52 ppm at the end of fermentation process. The total number of indigenous LAB isolated from the pickle are 48 strains we found 18 out of these had rod shape. For the preliminary study, all of the LAB with rod shape were detected by PCR as member of Lactobacillus spp., in which 17 strains detected as L. plantarum. The organic acids detected during the fermentation were lactic acid with the highest concentration was 0.0546 g/100 g and small amount of acetic acid.

Keywords: fermentation, LAB, pickle, Tabah Bamboo shoot

Procedia PDF Downloads 315
620 Flow-Through Supercritical Installation for Producing Biodiesel Fuel

Authors: Y. A. Shapovalov, F. M. Gumerov, M. K. Nauryzbaev, S. V. Mazanov, R. A. Usmanov, A. V. Klinov, L. K. Safiullina, S. A. Soshin

Abstract:

A flow-through installation was created and manufactured for the transesterification of triglycerides of fatty acids and production of biodiesel fuel under supercritical fluid conditions. Transesterification of rapeseed oil with ethanol was carried out according to two parameters: temperature and the ratio of alcohol/oil mixture at the constant pressure of 19 MPa. The kinetics of the yield of fatty acids ethyl esters (FAEE) was determined in the temperature range of 320-380 °C at the alcohol/oil molar ratio of 6:1-20:1. The content of the formed FAEE was determined by the method of correlation of the resulting biodiesel fuel by its kinematic viscosity. The maximum FAEE yield (about 90%) was obtained within 30 min at the ethanol/oil molar ratio of 12:1 and a temperature of 380 °C. When studying of transesterification of triglycerides, a kinetic model of an isothermal flow reactor was used. The reaction order implemented in the flow reactor has been determined. The first order of the reaction was confirmed by data on the conversion of FAEE during the reaction at different temperatures and the molar ratios of the initial reagents (ethanol/oil). Using the Arrhenius equation, the values of the effective constants of the transesterification reaction rate were calculated at different reaction temperatures. In addition, based on the experimental data, the activation energy and the pre-exponential factor of the transesterification reaction were determined.

Keywords: biodiesel, fatty acid esters, supercritical fluid technology, transesterification

Procedia PDF Downloads 80
619 Drug Delivery Nanoparticles of Amino Acid Based Biodegradable Polymers

Authors: Sophio Kobauri, Tengiz Kantaria, Temur Kantaria, David Tugushi, Nina Kulikova, Ramaz Katsarava

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Nanosized environmentally responsive materials are of special interest for various applications, including targeted drug to a considerable potential for treatment of many human diseases. The important technological advantages of nanoparticles (NPs) usage as drug carriers (nanocontainers) are their high stability, high carrier capacity, feasibility of encapsulation of both hydrophilic or hydrophobic substances, as well as a high variety of possible administration routes, including oral application and inhalation. NPs can also be designed to allow controlled (sustained) drug release from the matrix. These properties of NPs enable improvement of drug bioavailability and might allow drug dosage decrease. The targeted and controlled administration of drugs using NPs might also help to overcome drug resistance, which is one of the major obstacles in the control of epidemics. Various degradable and non-degradable polymers of both natural and synthetic origin have been used for NPs construction. One of the most promising for the design of NPs are amino acid-based biodegradable polymers (AABBPs) which can clear from the body after the fulfillment of their function. The AABBPs are composed of naturally occurring and non-toxic building blocks such as α-amino acids, fatty diols and dicarboxylic acids. The particles designed from these polymers are expected to have an improved bioavailability along with a high biocompatibility. The present work deals with a systematic study of the preparation of NPs by cost-effective polymer deposition/solvent displacement method using AABBPs. The influence of the nature and concentration of surfactants, concentration of organic phase (polymer solution), and the ratio organic phase/inorganic (water) phase, as well as of some other factors on the size of the fabricated NPs have been studied. It was established that depending on the used conditions the NPs size could be tuned within 40-330 nm. As the next step of this research an evaluation of biocompatibility and bioavailability of the synthesized NPs has been performed, using two stable human cell culture lines – HeLa and A549. This part of study is still in progress now.

Keywords: amino acids, biodegradable polymers, nanoparticles (NPs), non-toxic building blocks

Procedia PDF Downloads 409
618 Peach as a Potential Functional Food: Biological Activity and Important Phenolic Compound Source

Authors: Luís R. Silva, Catarina Bento, Ana C. Gonçalves, Fábio Jesus, Branca M. Silva

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Nowadays, the general population is more and more concerned about nutrition and the health implications of an unbalanced diet. Current knowledge regarding the health benefits and antioxidant properties of certain foods such as fruits and vegetables has gained the interest of both the general public and scientific community. Peach (Prunus persica (L.) Batsch) is one of the most consumed fruits worldwide, with low sugar contents and a broad range of nutrients essential to the normal functioning of the body. Six different peach cultivars from the Fundão region in Portugal were evaluated regarding their phenolic composition by LC-DAD and biological activity. The prepared extracts’ capacity to scavenge free-radicals was tested through the stable free radical DPPH• and nitric oxide (•NO). Additionally, antidiabetic potential and protective effects against peroxyl radical (ROO•) induced damage to erythrocytes were also tested. LC-DAD analysis allowed the identification of 17 phenolic compounds, among which 5-O-caffeoylquinic acids and 3-O-caffeoylquinic acids are pointed out as the most abundant. Regarding the antioxidant activity, all cultivars displayed concentration-dependent free-radical scavenging activity against both nitrogen species and DPPH•. In respect to α-glucosidase inhibitory activity, Royal Magister and Royal Glory presented the highest inhibitory activity (IC50 = 11.7 ± 1.4 and 17.1 ± 1.7 μg/mL, respectively), nevertheless all six cultivars presented higher activity than the control acarbose. As for the protective effect of Royal Lu extract on the oxidative damage induced in erythrocytes by ROO•, the results were quite promising showing inhibition IC50 values of 110.0 ± 4.5 μg/mL and 83.8 ± 6.5 μg/mL for hemolysis and hemoglobin oxidation, respectively. The demonstrated activity is of course associated to the peaches’ phenolic profile, rich in phenolic acids and flavonoids with high hydrogen donating capacity. These compounds have great industrial interest for the manufacturing of natural products. The following step would naturally be the extraction and isolation from the plant tissues and large-scale production through biotechnology techniques.

Keywords: antioxidants, functional food, phenolic compounds, peach

Procedia PDF Downloads 262
617 Using Human-Digestive Simulator to Harbor Encapsulated Lactobacillus casei 01 along with Pasteurized-Purple-Rice Drinks for Examination of the Health-Promoting Effects

Authors: Srivilai Worametrachanon, Arunee Apichartsrangkoon, Jiranat Techarang, Boonrak Phanchaisri

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A human-digestive simulator consisted of four colon compartments, i.e., stomach, small intestine, proximal colon and distal colon used to harbor L. casei 01 plus either pasteurized ordinary-purple-rice drinks or germinated-purple-rice drinks. Accordingly, three treatment compositions had been set up and the effects of treatments on colon bacterial communities including their by-products were thoroughly examined. L. casei 01 plus purple-rice drinks gave rise to significantly high formation (P ≤ 0.05) of short-chain-fatty acids (SCFA) of which highest acetic acid was found followed by propionic and butyric acids, while the germinated-rice drink showed the greatest impact. Moreover, the effect was more pronounced upon prolonged fermentation. In addition, the influence of treatments on colon microbes was also demonstrated. Accordingly, desirable bacteria including colon Lactobacilli and Bifidobacteria were significantly increased (P ≤ 0.05) in both colons in comparison with the control and the effect was more prominent after adding purple-rice drink. On the other hand, undesirable Clostridia and coliforms were apparently diminished by the influence of treatment conditions, in which both compartments exhibited similar results.

Keywords: human-digestive simulator, Lactobacillus casei 01, Pasteurized-purple-rice drinks

Procedia PDF Downloads 191
616 Development and Total Error Concept Validation of Common Analytical Method for Quantification of All Residual Solvents Present in Amino Acids by Gas Chromatography-Head Space

Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

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Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

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615 Liquid-Liquid Extraction of Uranium (VI) from Aqueous Solution Using 1-Hydroxyalkylidene-1,1-Diphosphonic Acids

Authors: Mustapha Bouhoun Ali, Ahmed Yacine Badjah Hadj Ahmed, Mouloud Attou, Abdel Hamid Elias, Mohamed Amine Didi

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The extraction of uranium(VI) from aqueous solutions has been investigated using 1-hydroxyhexadecylidene-1,1-diphosphonic acid (HHDPA) and 1-hydroxydodecylidene-1,1-diphosphonic acid (HDDPA), which were synthesized and characterized by elemental analysis and by FT-IR, 1H NMR, 31P NMR spectroscopy. In this paper, we propose a tentative assignment for the shifts of those two ligands and their specific complexes with uranium(VI). We carried out the extraction of uranium(VI) by HHDPA and HDDPA from [carbon tetrachloride + 2-octanol (v/v: 90%/10%)] solutions. Various factors such as contact time, pH, organic/aqueous phase ratio and extractant concentration were considered. The optimum conditions obtained were: contact time = 20 min, organic/aqueous phase ratio = 1, pH value = 3.0 and extractant concentration = 0.3M. The extraction yields are more significant in the case of the HHDPA which is equipped with a hydrocarbon chain, longer than that of the HDDPA. Logarithmic plots of the uranium(VI) distribution ratio vs. pHeq and the extractant concentration showed that the ratio of extractant to extracted uranium(VI) (ligand/metal) is 2:1. The formula of the complex of uranium(VI) with the HHDPA and the DHDPA is UO2(H3L)2 (HHDPA and DHDPA are denoted as H4L). A spectroscopic analysis has showed that coordination of uranium(VI) takes place via oxygen atoms.

Keywords: liquid-liquid extraction, uranium(VI), 1-hydroxyalkylidene-1, 1-diphosphonic acids, HHDPA, HDDPA, aqueous solution

Procedia PDF Downloads 492