Search results for: high perforamance liquid chromatography

Authors: Olufunmilola A. Abiodun, Adegbola O. Dauda, Ayobami Ojo, Samson A. Oyeyinka

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Serendipity berry (Dioscoreophyllum cumminsii diel) is a tropical dioecious rainforest vine and native to tropical Africa. The vine grows during the raining season and is used mainly as sweetener. The sweetener in the berry is known as monellin which is sweeter than sucrose. The sweetener is extracted from the fruits and the seed is discarded. The discarded seeds contain bitter principles but had high yield of oil. Serendipity oil was extracted using three methods (N-hexane, expression and expression/n-hexane). Fatty acids and physicochemical properties of the oil obtained were determined. The oil obtained was clear, liquid and have odour similar to hydrocarbon. The percentage oil yield was 38.59, 12.34 and 49.57% for hexane, expression and expression-hexane method respectively. The seed contained high percentage of oil especially using combination of expression and hexane. Low percentage of oil was obtained using expression method. The refractive index values obtained were 1.443, 1.442 and 1.478 for hexane, expression and expression-hexane methods respectively. Peroxide value obtained for expression-hexane was higher than those for hexane and expression. The viscosities of the oil were 125.8, 128.76 and 126.87 cm³/s for hexane, expression and expression-hexane methods respectively which showed that the oil from expression method was more viscous than the other oils. The major fatty acids in serendipity seed oil were oleic acid (62.81%), linoleic acid (22.65%), linolenic (6.11%), palmitic acid (5.67%), stearic acid (2.21%) in decreasing order. Oleic acid which is monounsaturated fatty acid had the highest value. Total unsaturated fatty acids were 91.574, 92.256 and 90.426% for hexane, expression, and expression-hexane respectively. Combination of expression and hexane for extraction of serendipity oil produced high yield of oil. The oil could be refined for food and non-food application.

Keywords: serendipity seed oil, expression method, fatty acid, hexane

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Authors: R. Vetrimurugan, Terry Lim, M. J. Goodson, R. Nagarajan

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This study investigates the cleaning performance of high intensity 360 kHz frequency on the removal of nano-dimensional and sub-micron particles from various surfaces, uniformity of the cleaning tank and run to run variation of cleaning process. The uniformity of the cleaning tank was measured by two different methods i.e 1. ppbTM meter and 2. Liquid Particle Counting (LPC) technique. In the second method, aluminium metal spacer components was placed at various locations of the cleaning tank (such as centre, top left corner, bottom left corner, top right corner, bottom right corner) and the resultant particles removed by 360 kHz frequency was measured. The result indicates that the energy was distributed more uniformly throughout the entire cleaning vessel even at the corners and edges of the tank when megasonic sweeping technology is applied. The result also shows that rinsing the parts with 360 kHz frequency at final rinse gives lower particle counts, hence higher cleaning efficiency as compared to other frequencies. When megasonic sweeping technology is applied each piezoelectric transducers will operate at their optimum resonant frequency and generates stronger acoustic cavitational force and higher acoustic streaming velocity. These combined forces are helping to enhance the particle removal and at the same time improve the overall cleaning performance. The multiple extractions study was also carried out for various frequencies to measure the cleaning potential and asymptote value.

Keywords: power distribution, megasonic sweeping, cavitation intensity, particle removal, laser particle counting, nano, submicron

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Authors: S. Ramteke, K. S. Patel

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Aerosols are complex mixture of particulate matters (PM) inclusive of carbons, silica, elements, various salts, etc. Aerosols get deep into the human lungs and cause a broad range of health effects, in particular, respiratory and cardiovascular illnesses. They are one of the major culprits for the climate change. They are emitted by the high thermal processes i.e. vehicles, steel, sponge, cement, thermal power plants, etc. Raipur (22˚33'N to 21˚14'N and 82˚6'E) to 81˚38'E) is a growing industrial city in central India with population of two million. In this work, the distribution of inorganics (i.e. Cl⁻, NO³⁻, SO₄²⁻, NH₄⁺, Na⁺, K⁺, Mg²⁺, Ca²⁺, Al, Cr, Mn, Fe, Ni, Cu, Zn, and Pb) associated to the PM in the ambient air is described. The PM₁₀ in ambient air of Raipur city was collected for duration of one year (December 2014 - December 2015). The PM₁₀ was segregated into nine modes i.e. PM₁₀.₀₋₉.₀, PM₉.₀₋₅.₈, PM₅.₈₋₄.₇, PM₄.₇₋₃.₃, PM₃.₃₋₂.₁, PM₂.₁₋₁.₁, PM₁.₁₋₀.₇, PM₀.₇₋₀.₄ and PM₀.₄ to know their emission sources and health hazards. The analysis of ions and metals was carried out by techniques i.e. ion chromatography and TXRF. The PM₁₀ concentration (n=48) was ranged from 100-450 µg/m³ with mean value of 73.57±20.82 µg/m³. The highest concentration of PM₄.₇₋₃.₃, PM₂.₁₋₁.₁, PM₁.₁₋₀.₇ was observed in the commercial, residential and industrial area, respectively. The effect of meteorology i.e. temperature, humidity, wind speed and wind direction in the PM₁₀ and associated elemental concentration in the air is discussed.

Keywords: ambient aerosol, ions, metals, segregation

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Authors: Karol Rodriguez-Peña, Martha L. Macias-Rubalcava, Leticia Rocha-Zavaleta, Sergio Sanchez

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A bioassay-guided study for anti-cancer compounds from endophytes of the Mexican medicinal plant Amphipteryygium adstringens resulted in the isolation of a streptomycete capable of producing a group of compounds with high cytotoxic activity. Microorganisms from surface sterilized samples of various sections of the plant were isolated and all the actinomycetes found were evaluated for their potential to produce compounds with cytotoxic activity against cancer cell lines MCF7 (breast cancer) and HeLa (cervical cancer) as well as the non-tumoural cell line HaCaT (keratinocyte). The most active microorganism was picked for further evaluation. The identification of the microorganism was carried out by 16S rDNA gene sequencing, finding the closest proximity to Streptomyces scabrisporus, but with the additional characteristic that the strain isolated in this study was capable of producing colorful compounds never described for this species. Crude extracts of dichloromethane and ethyl acetate showed IC50 values of 0.29 and 0.96 μg/mL for MCF7, 0.51 and 1.98 μg/mL for HeLa and 0.96 and 2.7 μg/mL for HaCaT. Scaling the fermentation to 10 L in a bioreactor generated 1 g of total crude extract, which was fractionated by silica gel open column to yield 14 fractions. Nine of the fractions showed cytotoxic activity. Fraction 4 was chosen for subsequent purification because of its high activity against cancerous cell lines, lower activity against keratinocytes. HPLC-UV-MS/ESI was used for the evaluation of this fraction, finding at least 10 different compounds with high values of m/z (≈588). Purification of the compounds was carried out by preparative thin-layer chromatography. The prevalent compound was Steffimycin B, a molecule known for its antibiotic and cytotoxic activities and also for its low solubility in aqueous solutions. Along with steffimycin B, another five compounds belonging to the steffimycin family were isolated and at this moment their structures are being elucidated, some of which display better solubility in water: an attractive property for the pharmaceutical industry. As a conclusion to this study, the isolation of endophytes resulted in the discovery of a strain capable of producing compounds with high cytotoxic activity that need to be studied for their possible utilization.

Keywords: amphipterygium adstringens, cytotoxicity, streptomyces scabrisporus, steffimycin

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Authors: Sylvain Caillol

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Uncertainty in terms of price and availability of petroleum, in addition to global political and institutional tendencies toward the principles of sustainable development, urge chemical industry to a sustainable chemistry and particularly the use of renewable resources in order to synthesize biobased chemicals and products. We propose a platform approach for the synthesis of various building blocks from cardanol in one or two-steps syntheses. Cardanol, which is a natural phenol, is issued from Cashew Nutshell Liquid (CNSL), a non-edible renewable resource, co-produced from cashew industry in large commercial volumes. Cardanol is particularly interesting to replace fossil aromatic groups in polymers and materials. Our team studied various routes for the synthesis of cardanol-derived biobased building blocks used after that in polymer syntheses. For example, we used phenolation to dimerize/oligomerize cardanol to propose increase functionality of cardanol. Thio-ene was used to synthesize new reactive amines. Epoxidation and (meth)acrylation were also used to insert oxirane or (meth)acrylate groups in order to synthesize polymers and materials.

Keywords: cardanol, cashew nutshell liquid, epoxy, vinyl ester, latex, emulsion

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Authors: Cristina Munoz-Shuguli, Francisco Rodriguez, Julio Bruna, M. Jose Galotto, Abel Guarda

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The microbial contamination in fruits due to the presence of fungal is the most important cause of their deterioration and loss. The development of active food packaging materials with antifungal properties has been proposed as an innovative strategy in order to prevent this problem. In this way, natural compounds as the essential oils or their derivatives, also called volatile compounds (VC), can be incorporated in the food packaging materials to control the fungal growth during fruit packaging. However, if the VC is incorporated directly in the packaging material, it is released very fast due to VC high volatility. For this reason, the formation of inclusion complexes through the encapsulation of VC into beta-cyclodextrin (β-CD) and their incorporation in package materials is an alternative to maintain an antifungal atmosphere around the packaged fruits for longer times. In this context, the aim of this work was to develop inclusion complexes based in β-CD and VC (β-CD:VC) for further application in the antifungal food packaging materials development. β-CD:VC inclusion complexes were obtained with two different molar ratios 2:1 and 1:1, through co-precipitation method. The entrapment efficiency of β-CD:VC as well the release of antifungal compound from inclusion complexes exposed to different relative humidity (25, 50, and 97 %) to headspace were determined by gaseous chromatography (GC). Also, thermal and antimicrobial properties of β-CD:VC were determined through thermogravimetric analysis (TGA) and antifungal assays against Botrytis cinerea, respectively. GC results showed that β-CD:VC 2:1 had a higher entrapment efficiency than β-CD:VC 1:1, with values of 75.5 ± 3.71 % and 59.6 ± 1.51 %, respectively. It was probably because during the synthesis of β-CD:VC 1:1, there was less molecular space to the movement of VC molecules. Furthermore, the release of VC from β-CD:VC was directly related with the relative humidity. High amount of VC was released when the inclusion complexes were exposed to high humidity, possibly due to the interactions between the water molecules and the β-CD hydrophilic wall. On the other hand, a better thermal stability of VC in inclusion complexes allowed to verify its effective encapsulation into β-CD. Finally, antimicrobial assays showed that the inclusion complexes had a high antifungal activity at very low concentrations. Therefore, the results obtained in this work allow suggesting the β-CD:VC inclusion complexes as potential candidates to the development of fruit antifungal packaging materials, which activity is relative humidity dependent.

Keywords: Botrytis cinerea, fruit packaging, headspace release, volatile compounds

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Authors: Marta Malo, Carlota Soto, Carmen García-Rosales, Teresa Hernández

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SiC based composites are candidates for possible use as structural and functional materials in the future fusion reactors, the main role is intended for the blanket modules. In the blanket, the neutrons produced in the fusion reaction slow down and their energy is transformed into heat in order to finally generate electrical power. In the blanket design named Dual Coolant Lead Lithium (DCLL), a PbLi alloy for power conversion and tritium breeding circulates inside hollow channels called Flow Channel Inserts (FCIs). These FCI must protect the steel structures against the highly corrosive PbLi liquid and the high temperatures, but also provide electrical insulation in order to minimize magnetohydrodynamic interactions of the flowing liquid metal with the high magnetic field present in a magnetically confined fusion environment. Due to their nominally high temperature and radiation stability as well as corrosion resistance, SiC is the main choice for the flow channel inserts. The significantly lower manufacturing cost presents porous SiC (dense coating is required in order to assure protection against corrosion and as a tritium barrier) as a firm alternative to SiC/SiC composites for this purpose. This application requires the materials to be exposed to high radiation levels and extreme temperatures, conditions for which previous studies have shown noticeable changes in both the microstructure and the electrical properties of different types of silicon carbide. Both initial properties and radiation/temperature induced damage strongly depend on the crystal structure, polytype, impurities/additives that are determined by the fabrication process, so the development of a suitable material requires full control of these variables. For this work, several SiC samples with different percentage of porosity and sintering additives have been manufactured by the so-called sacrificial template method at the Ceit-IK4 Technology Center (San Sebastián, Spain), and characterized at Ciemat (Madrid, Spain). Electrical conductivity was measured as a function of temperature before and after irradiation with 1.8 MeV electrons in the Ciemat HVEC Van de Graaff accelerator up to 140 MGy (~ 2·10 -5 dpa). Radiation-induced conductivity (RIC) was also examined during irradiation at 550 ºC for different dose rates (from 0.5 to 5 kGy/s). Although no significant RIC was found in general for any of the samples, electrical conductivity increase with irradiation dose was observed to occur for some compositions with a linear tendency. However, first results indicate enhanced radiation resistance for coated samples. Preliminary thermogravimetric tests of selected samples, together with posterior XRD analysis allowed interpret radiation-induced modification of the electrical conductivity in terms of changes in the SiC crystalline structure. Further analysis is needed in order to confirm this.

Keywords: DCLL blanket, electrical conductivity, flow channel insert, porous SiC, radiation damage, thermal stability

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Authors: B. Makoudi, R. Ghanimi, A. Bargaz, M. Mouradi, M. Farissi, A. Kabbaj, J. J. Drevon, C. Ghoulam

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Legume species are able to establish a nitrogen fixing symbiosis with soil rhizobia that allows them, when it operates normally, to ensure their necessary nitrogen nutrition. This biological process needs high phosphorus (P) supply and consequently it is limited under low phosphorus availability. To overcome this constraint, legume-rhizobia symbiosis develops many mechanisms to increase P availability in the rhizosphere and also the efficiency of P fertilizers. The objectives of our research works are to understand the physiological and biochemical mechanisms implemented by legume-rhizobia symbiosis to increase its P use efficiency (PUE) in order to select legume genotypes-rhizobia strains combination more performing for BNF under P deficiency. Our studies were carried out on two grain legume species, common bean (Phaseolus vulgaris) and faba bean (Vicia faba) tested in farmers’ fields and in experimental station fewer than two soil phosphorus levels. Under field conditions, the P deficiency caused a significant decrease of Plant and nodule biomasses in all of the tested varieties with a difference between them. This P limitation increased the contents of available P in the rhizospheric soils that was positively correlated with the increase of phosphatases activities in the nodules and the rhizospheric soil. Some legume genotypes showed a significant increase of their P use efficiency under P deficiency. The P solubilization test showed that some rhizobia strains isolated from Haouz region presented an important capacity to grow on solid and liquid media with tricalcium phosphate as the only P source and their P solubilizing activity was confirmed by the assay of the released P in the liquid medium. Also, this P solubilizing activity was correlated with medium acidification and the excretion of acid phosphatases and phytases in the medium. Thus, we concluded that medium acidification and excretion of phosphatases in the rhizosphere are the prominent reactions for legume-rhizobia symbiosis to improve its P nutrition.

Keywords: legume, phosphorus deficiency, rhizobia, rhizospheric soil

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Authors: Zhanat Shomanova, Ruslan Safarov, Yuri Nosenko, Zheneta Tashmuchambetova, Alima Zharmagambetova

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An effective way of utilization of ferroalloy production wastes is preparing hydrocarbon refining catalysts from them. It is possible due to accordable transition metals containing in the wastes. In the work, we are presenting the results on elemental analysis of sludge samples from Aksu ferroalloy plant (Aksu, Kazakhstan), method of catalysts preparing, results of physical-chemical analysis of obtained catalysts (X-ray analysis, electron microscopy, the BET method etc.), results of using the catalysts in some hydrocarbons refining processes such as hydrocracking of rubber waste, cracking of gasoil, oxidation of cyclohexane. The main results of catalytic activity research are: a) In hydrocracking of rubber waste 64.9% of liquid products were fuel fractions; b) In cracking of gasoil conversion was 51% and selectivity by liquid products was 99%; c) In oxidation of cyclohexane the maximal product yield 87.9% and selectivity by cyclohexanol 93.0% were achieved.

Keywords: catalyst, cyclohexane oxidation, ferroalloy production waste, gasoil cracking

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Authors: Loganathan Kumaresan, Velusamy Chidambaram, Arumugam Velayutham Karthikeyani, Alex Cheru Pulikottil, Madhusudan Sau, Gurpreet Singh Kapur, Sankara Sri Venkata Ramakumar

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Environmentally driven regulations throughout the world stipulate dramatic improvements in the quality of transportation fuels and refining operations. The exhaust gases like CO, NOx, and SOx from stationary sources (e.g., refinery) and motor vehicles contribute to a large extent for air pollution. The refining industry is under constant environmental pressure to achieve more rigorous standards on sulphur content in the fuel used in the transportation sector and other off-gas emissions. Fluid catalytic cracking unit (FCCU) is a major secondary process in refinery for gasoline and diesel production. CO-combustion promoter additive and gasoline sulphur reduction (GSR) additive are catalytic systems used in FCCU to assist the combustion of CO to CO₂ in the regenerator and regulate sulphur in gasoline faction respectively along with main FCC catalyst. Effectiveness of these catalysts is governed by the active metal used, its dispersion, the type of base material employed, and retention characteristics of additive in FCCU such as attrition resistance and density. The challenge is to have a high-density microsphere catalyst support for its retention and high activity of the active metals as these catalyst additives are used in low concentration compare to the main FCC catalyst. The present paper discusses in the first part development of high dense microsphere of nanocrystalline alumina by hydro-thermal method for CO combustion promoter application. Performance evaluation of additive was conducted under simulated regenerator conditions and shows CO combustion efficiency above 90%. The second part discusses the efficacy of a co-precipitation method for the generation of the active crystalline spinels of Zn, Mg, and Cu with aluminium oxides as an additive. The characterization and micro activity test using heavy combined hydrocarbon feedstock at FCC unit conditions for evaluating gasoline sulphur reduction activity are studied. These additives were characterized by X-Ray Diffraction, NH₃-TPD & N₂ sorption analysis, TPR analysis to establish structure-activity relationship. The reaction of sulphur removal mechanisms involving hydrogen transfer reaction, aromatization and alkylation functionalities are established to rank GSR additives for their activity, selectivity, and gasoline sulphur removal efficiency. The sulphur shifting in other liquid products such as heavy naphtha, light cycle oil, and clarified oil were also studied. PIONA analysis of liquid product reveals 20-40% reduction of sulphur in gasoline without compromising research octane number (RON) of gasoline and olefins content.

Keywords: hydrothermal, nanocrystalline, spinel, sulphur reduction

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Authors: Igor Jerkovic

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Biodiversity of flora provides many different nectar sources for the bees. Unifloral honeys possess distinctive flavours, mainly derived from their nectar sources (characteristic volatile organic components (VOCs)). Specific or nonspecific VOCs (chemical markers) could be used for unifloral honey characterisation as addition to the melissopalynologycal analysis. The main honey volatiles belong, in general, to three principal categories: terpenes, norisoprenoids, and benzene derivatives. Some of these substances have been described as characteristics of the floral source, and other compounds, like several alcohols, branched aldehydes, and furan derivatives, may be related to the microbial purity of honey processing and storage conditions. Selection of the extraction method for the honey volatiles profiling should consider that heating of the honey produce different artefacts and therefore conventional methods of VOCs isolation (such as hydrodistillation) cannot be applied for the honey. Two-way approach for the isolation of the honey VOCs was applied using headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE). The extracts were analysed by gas chromatography and mass spectrometry (GC-MS). HS-SPME (with the fibers of different polarity such as polydimethylsiloxane/ divinylbenzene (PDMS/DVB) or divinylbenzene/carboxene/ polydimethylsiloxane (DVB/CAR/PDMS)) enabled isolation of high volatile headspace VOCs of the honey samples. Among them, some characteristic or specific compounds can be found such as 3,4-dihydro-3-oxoedulan (in Centaurea cyanus L. honey) or 1H-indole, methyl anthranilate, and cis-jasmone (in Citrus unshiu Marc. honey). USE with different solvents (mainly dichloromethane or the mixture pentane : diethyl ether 1 : 2 v/v) enabled isolation of less volatile and semi-volatile VOCs of the honey samples. Characteristic compounds from C. unshiu honey extracts were caffeine, 1H-indole, 1,3-dihydro-2H-indol-2-one, methyl anthranilate, and phenylacetonitrile. Sometimes, the selection of solvent sequence was useful for more complete profiling such as sequence I: pentane → diethyl ether or sequence II: pentane → pentane/diethyl ether (1:2, v/v) → dichloromethane). The extracts with diethyl ether contained hydroquinone and 4-hydroxybenzoic acid as the major compounds, while (E)-4-(r-1’,t-2’,c-4’-trihydroxy-2’,6’,6’-trimethylcyclo-hexyl)but-3-en-2-one predominated in dichloromethane extracts of Allium ursinum L. honey. With this two-way approach, it was possible to obtain a more detailed insight into the honey volatile and semi-volatile compounds and to minimize the risks of compound discrimination due to their partial extraction that is of significant importance for the complete honey profiling and identification of the chemical biomarkers that can complement the pollen analysis.

Keywords: honey chemical biomarkers, honey volatile compounds profiling, headspace solid-phase microextraction (HS-SPME), ultrasonic solvent extraction (USE)

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Authors: S. Rostampour Yasouri, M. Ghane

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Leptospirosis is one the most important common diseases between human and live stock occurred by different species of Leptospira. This disease has been construed as the native in the northern provinces of Iran and risk of the infection with pathogenic is high. One hundred fifteen samples of water (67), soil (36) and feces of rodents (12) were collected from the rice fields of the suburbs of Tonekabon Township situated in northern part of Iran in 2012. The samples, after passage from membranous filters, were cultured in the liquid and solid EMJH medium and incubated at 30°C for 1 month. Leptospira spp. were isolated using culture technique, and the plates were studied from viewpoint of colony formation, microscopic observations and then identified by phenotyping tests. Finally, the identification of Leptospira genus was verified by PCR technique and 16S rRNA gene sequencing. Of 115 samples totally, 55 samples (47.82%) became positive by use of the culture technique which the positive cases included 47 water samples (70.14%) and 8 soil samples (22.22%), while the isolation was not accomplished from the sample of the rodents feces. Overall, according to these data, Leptospira spp. exists with high frequency in North Iran. Hence, based on foregoing evidence environments in the north of Iran are vehicles of Leptospira spp.

Keywords: EMJH Medium, Leptospira, Northern of Iran, rice fields

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Authors: G. Blázquez, A. Gálvez-Pérez, M. Calero, I. Iáñez-Rodríguez, M. A. Martín-Lara, A. Pérez

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The production of olive oil is considered as one of the most important agri-food industries. However, some of the by-products generated in the process are potential pollutants and cause environmental problems. Consequently, the management of these by-products is currently considered as a challenge for the olive oil industry. In this context, several technologies have been developed and tested. In this sense, the autohydrolysis of these by-products could be considered as a promising technique. Therefore, this study focused on autohydrolysis treatments of a solid residue from the olive oil industry denominated olive cake. This one comes from the olive pomace extraction with hexane. Firstly, a water washing was carried out to eliminate the water soluble compounds. Then, an experimental design was developed for the autohydrolysis experiments carried out in the hydrothermal pressure reactor. The studied variables were temperature (30, 60 and 90 ºC) and time (30, 60, 90 min). On the other hand, aliquots of liquid obtained fractions were analysed by HPLC to determine the fructose and sucrose contents present in the liquid fraction. Finally, the obtained results of sugars contents and the yields of the different experiments were fitted to a neuro-fuzzy and to a polynomial model.

Keywords: ANFIS, olive cake, polyols, saccharides

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Authors: Mindaugas Liaudanskas, Darius Kviklys, Kristina Zymonė, Raimondas Raudonis, Jonas Viškelis, Norbertas Uselis, Pranas Viškelis, Valdimaras Janulis

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Apples are among the most commonly consumed fruits in the world. Based on data from the year 2014, approximately 84.63 million tons of apples are grown per annum. Apples are widely used in food industry to produce various products and drinks (juice, wine, and cider); they are also used unprocessed. Apples in human diet are an important source of different groups of biological active compounds that can positively contribute to the prevention of various diseases. They are a source of various biologically active substances – especially vitamins, organic acids, micro- and macro-elements, pectins, and phenolic, triterpenic, and other compounds. Triterpenic compounds, which are characterized by versatile biological activity, are the biologically active compounds found in apples that are among the most promising and most significant for human health. A specific analytical procedure including sample preparation and High Performance Liquid Chromatography (HPLC) analysis was developed, optimized, and validated for the detection of triterpenic compounds in the samples of different apples, their peels, and flesh from widespread apple cultivars 'Aldas', 'Auksis', 'Connel Red', 'Ligol', 'Lodel', and 'Rajka' grown in Lithuanian climatic conditions. The conditions for triterpenic compound extraction were optimized: the solvent of the extraction was 100% (v/v) acetone, and the extraction was performed in an ultrasound bath for 10 min. Isocratic elution (the eluents ratio being 88% (solvent A) and 12% (solvent B)) for a rapid separation of triterpenic compounds was performed. The validation of the methodology was performed on the basis of the ICH recommendations. The following characteristics of validation were evaluated: the selectivity of the method (specificity), precision, the detection and quantitation limits of the analytes, and linearity. The obtained parameters values confirm suitability of methodology to perform analysis of triterpenic compounds. Using the optimised and validated HPLC technique, four triterpenic compounds were separated and identified, and their specificity was confirmed. These compounds were corosolic acid, betulinic acid, oleanolic acid, and ursolic acid. Ursolic acid was the dominant compound in all the tested apple samples. The detected amount of betulinic acid was the lowest of all the identified triterpenic compounds. The greatest amounts of triterpenic compounds were detected in whole apple and apple peel samples of the 'Lodel' cultivar, and thus apples and apple extracts of this cultivar are potentially valuable for use in medical practice, for the prevention of various diseases, for adjunct therapy, for the isolation of individual compounds with a specific biological effect, and for the development and production of dietary supplements and functional food enriched in biologically active compounds. Acknowledgements. This work was supported by a grant from the Research Council of Lithuania, project No. MIP-17-8.

Keywords: apples, HPLC, triterpenic compounds, validation

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Authors: Andreia Garrido, Artur Conde, Ana Cunha, Ric De Vos

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Climate changes predictions point to increases in abiotic stress for crop plants in Portugal, like pronounced temperature variation and decreased precipitation, which will have negative impact on grapevine physiology and consequently, on grape berry and wine quality. Short-term mitigation strategies have, therefore, been implemented to alleviate the impacts caused by adverse climatic periods. These strategies include foliar application of kaolin, an inert mineral, which has radiation reflection proprieties that decreases stress from excessive heat/radiation absorbed by its leaves, as well as smart irrigation strategies to avoid water stress. However, little is known about the influence of these mitigation measures on grape berries, neither on the photosynthetic activity nor on the photosynthesis-related metabolic profiles of its various tissues. Moreover, the role of fruit photosynthesis on berry quality is poorly understood. The main objective of our work was to assess the effects of kaolin and irrigation treatments on the photosynthetic activity of grape berry tissues (exocarp and seeds) and on their global metabolic profile, also investigating their possible relationship. We therefore collected berries of field-grown plants of the white grape variety Alvarinho from two distinct microclimates, i.e. from clusters exposed to high light (HL, 150 µmol photons m⁻² s⁻¹) and low light (LL, 50 µmol photons m⁻² s⁻¹), from both kaolin and non-kaolin (control) treated plants at three fruit developmental stages (green, véraison and mature). Plant irrigation was applied after harvesting the green berries, which also enabled comparison of véraison and mature berries from irrigated and non-irrigated growth conditions. Photosynthesis was assessed by pulse amplitude modulated chlorophyll fluorescence imaging analysis, and the metabolite profile of both tissues was assessed by complementary metabolomics approaches. Foliar kaolin application resulted in, for instance, an increased photosynthetic activity of the exocarp of LL-grown berries at green developmental stage, as compared to the control non-kaolin treatment, with a concomitant increase in the levels of several lipid-soluble isoprenoids (chlorophylls, carotenoids, and tocopherols). The exocarp of mature berries grown at HL microclimate on kaolin-sprayed non-irrigated plants had higher total sugar levels content than all other treatments, suggesting that foliar application of this mineral results in an increased accumulation of photoassimilates in mature berries. Unbiased liquid chromatography-mass spectrometry-based profiling of semi-polar compounds followed by ASCA (ANOVA simultaneous component analysis) and ANOVA statistical analysis indicated that kaolin had no or inconsistent effect on the flavonoid and phenylpropanoid composition in both seed and exocarp at any developmental stage; in contrast, both microclimate and irrigation influenced the level of several of these compounds depending on berry ripening stage. Overall, our study provides more insight into the effects of mitigation strategies on berry tissue photosynthesis and phytochemistry, under contrasting conditions of cluster light microclimate. We hope that this may contribute to develop sustainable management in vineyards and to maintain grape berries and wines with high quality even at increasing abiotic stress challenges.

Keywords: climate change, grape berry tissues, metabolomics, mitigation strategies

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Authors: R. Ramesh, M. Y. M. Yunus, K. Ramesh

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The study conducted in this research are Viscosities, η, and Densities ,ρ, of 1, 4-dioxane with Bromobenzene at different mole fractions and various temperatures in the atmospheric pressure condition. From experimentations excess volumes, VE, and deviations in viscosities, Δη, of mixtures at infinite dilutions have been obtained. The measured systems exhibited positive values of VmE and negative values of Δη. The binary mixture 1, 4 dioxane + Bromobenzene show positive VE and negative Δη with increasing temperatures. The outcomes clearly indicate that weak interactions present in mixture. It is mainly because of number and position of methyl groups exist in these aromatic hydrocarbons. These measured data tailored to the nonlinear models to derive the binary coefficients. Standard deviations have been considered between the fitted outcomes and the calculated data is helpful deliberate mixing behavior of the binary mixtures. It can conclude that in our cases, the data found with the values correlated by the corresponding models very well. The molecular interactions existing between the components and comparison of liquid mixtures were also discussed.

Keywords: 1, 4 dioxane, bromobenzene, density, excess molar volume

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Authors: Mustafa Sertçelik, Hacali Necefoğlu, Turan Çalban, Soner Kuşlu

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In this study, Chevreul’s salt was dissolved in ammonium chloride solutions. All experiments were performed in a batch reactor. The obtained results were optimized. Parameters used in the experiments were the reaction temperature, the ammonium chloride concentration, the reaction time and the solid-to-liquid ratio. The optimum conditions were determined by 2⁴ factorial experimental design method. The best values of four parameters were determined as based on the experiment results. After the evaluation of experiment results, all parameters were found as effective in experiment conditions selected. The optimum conditions on the maximum Chevreul’s salt dissolution were the ammonium chloride concentration 4.5 M, the reaction time 13.2 min., the reaction temperature 25 ^oC, and the solid-to-liquid ratio 9/80 g.mL^-1. The best dissolution yield in these conditions was 96.20%.

Keywords: Chevreul's salt, factorial experimental design method, ammonium chloride, dissolution, optimization

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Authors: Luofu Liu, Fei Xiao Jr., Fei Xiao

Abstract:

Through the analysis technology of gas chromatography-mass spectrometry (GC-MS), the composition and distribution characteristics of aromatic hydrocarbons in the Chepaizi area of the Junggar Basin were analyzed in detail. Based on that, the biological input, maturity of crude oils and sedimentary environment of the corresponding source rocks were determined and the origin types of crude oils were divided. The results show that there are three types of crude oils in the study area including Type I, Type II and Type III oils. The crude oils from the 1st member of the Neogene Shawan Formation are the Type I oils; the crude oils from the 2nd member of the Neogene Shawan Formation are the Type II oils; the crude oils from the Cretaceous Qingshuihe and Jurassic Badaowan Formations are the Type III oils. For the Type I oils, they show a single model in the late retention time of the chromatogram of total aromatic hydrocarbons. The content of triaromatic steroid series is high, and the content of dibenzofuran is low. Maturity parameters related to alkyl naphthalene, methylphenanthrene and alkyl dibenzothiophene all indicate low maturity for the Type I oils. For the Type II oils, they have also a single model in the early retention time of the chromatogram of total aromatic hydrocarbons. The content of naphthalene and phenanthrene series is high, and the content of dibenzofuran is medium. The content of polycyclic aromatic hydrocarbon representing the terrestrial organic matter is high. The aromatic maturity parameters indicate high maturity for the Type II oils. For the Type III oils, they have a bi-model in the chromatogram of total aromatic hydrocarbons. The contents of naphthalene series, phenanthrene series, and dibenzofuran series are high. The aromatic maturity parameters indicate medium maturity for the Type III oils. The correlation results of triaromatic steroid series fingerprint show that the Type I and Type III oils have similar source and are both from the Permian Wuerhe source rocks. Because of the strong biodegradation and mixing from other source, the Type I oils are very different from the Type III oils in aromatic hydrocarbon characteristics. The Type II oils have the typical characteristics of terrestrial organic matter input under oxidative environment, and are the coal oil mainly generated by the mature Jurassic coal measure source rocks. However, the overprinting effect from the low maturity Cretaceous source rocks changed the original distribution characteristics of aromatic hydrocarbons to some degree.

Keywords: oil source, geochemistry, aromatic hydrocarbons, crude oils, chepaizi area, Junggar Basin

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Authors: A. Abdi, A. Barari, A. Hojatollah Nikbakht, Khosro Ebrahim

Abstract:

Aim: The purpose of the current study was to investigate the effect of a high intensity treadmill running training (8 weeks) with or without aqueous extraction of Crataegus pentagyna on heart and plasma LDH and CK. Design: Thirty-two Wistar male rats (4-6 weeks old, 125-135 gr weight) were used. Animals were randomly assigned into training (n = 16) and control (n = 16) groups and further divided into saline-control (SC, n = 8), saline-training (ST, n = 8), red Crataegus pentagyna extraction -control (CPEC, n = 8), and red Crataegus pentagyna extraction -training (CPET, n = 8) groups. Training groups have performed a high-intensity running program 34 m/min on 0% grade, 60 min/day, 5 days/week) on a motor-driven treadmill for 8 weeks. Animals were fed orally with Crataegus extraction and saline solution (500mg/kg body weight/or 10ml/kg body weight) for last six weeks. Seventy- two hours after the last training session, rats were sacrificed; plasma and heart were excised and immediately frozen in liquid nitrogen. LDH and CK levels were measured by colorimetric method. Statistical analysis was performed using a one way analysis of variance and Tukey test. Significance was accepted at P = 0.05. Results: Result showed that consumption crataegus lowers LDH and CK in heart and plasma. Also the heart LDH and CK were lower in the CPET compared to the ST, while plasma LDH and CK in CPET was higher than the ST. The results of ANOVA showed that the due high-intensity exercise and consumption crataegus, there are significant differences between levels of hearth LDH (P < 0/001), plasma (P < 0/006) and hearth (P < 0/001) CK. Conclusion: It appears that high-intensity exercise led to increased tissue damage and inflammatory factors in plasma. In other hand, consumption aqueous extraction of Red Crataegus maybe inhibits these factors and prevents muscle and heart damage.

Keywords: LDH, CK, crataegus, intensity

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Authors: L. Kolatorova, J. Vitku, K. Adamcova, M. Simkova, M. Hill, A. Parizek, M. Duskova

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Endocrine disruptors (EDs) are substances leaching from various industrial products, which are able to interfere with the endocrine system. Their harmful effects on human health are generally well-known, and exposure during fetal development may have lasting effects. Fetal exposure and transplacental transport of bisphenol A (BPA) have been recently studied; however, less is known about alternatives such as bisphenol S (BPS), bisphenol F (BPF) and bisphenol AF (BPAF), which have started to appear in consumer products. The human organism is usually exposed to the mixture of EDs, out of which parabens are otherwise known to transfer placenta. The usage of many cosmetic, pharmaceutical and consumer products during the pregnancy that may contain parabens and bisphenols has led to the need for investigation. The aim of the study was to investigate the transplacental transport of BPA, its alternatives, and parabens, and to study their relation to fetal steroidogenesis. BPA, BPS, BPF, BPAF, methylparaben, ethylparaben, propylparaben, butylparaben, benzylparaben and 15 steroids including estrogens, corticoids, androgens and immunomodulatory ones were determined in 27 maternal (37th week of gestation) and cord plasma samples using liquid chromatography - tandem mass spectrometry methods. The statistical evaluation of the results showed significantly higher levels of BPA (p=0.0455) in cord plasma compared to maternal plasma. The results from multiple regression models investigated that in cord plasma, methylparaben, propylparaben and the sum of all measured parabens were inversely associated with testosterone levels. To our best knowledge, this study is the first attempt to determine the levels of alternative bisphenols in the maternal and cord blood, and also the first study reporting the simultaneous detection of bisphenols, parabens, and steroids in these biological fluids. Our study confirmed the transplacental transport of BPA, with likely accumulation in the fetal compartment. The negative association of cord blood parabens and testosterone levels highlights their possible risks, especially for the development of male fetuses. Acknowledgements: This work was supported by the project MH CR 17-30528 A from the Czech Health Research Council, MH CZ - DRO (Institute of Endocrinology - EÚ, 00023761) and by the MEYS CR (OP RDE, Excellent research - ENDO.CZ).

Keywords: bisphenol, endocrine disruptor, paraben, pregnancy, steroid

Procedia PDF Downloads 178

Authors: G. V. Manzane, S. J. Modise

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Uterine fibroids, also known as leiomyomas or myomas, are non-cancerous growths that develop in the muscular wall of the uterus during the reproductive years. The cause of uterine fibroids includes hormonal, genetic, growth factors, and extracellular matrix factors. Common symptoms of uterine fibroids include heavy and prolonged menstrual bleeding which can lead to a high risk of anemia, lower abdominal pains, pelvic pressure, infertility, and pregnancy loss. The growth of this tumor is a concern because of its negative impact on women’s health and the increase in their economic burden. Traditional medicinal plants have long been used in Africa for their potential therapeutic effects against various ailments. In this study, we aimed to identify and characterize bioactive compounds from selected African medicinal plants with potential anti-fibrotic properties using Fourier-transform infrared spectroscopy (FTIR) and gas chromatography-mass spectrometry (GCMS) analysis. Two medicinal plant species known for their traditional use in fibrosis-related conditions were selected for investigation. Aqueous extracts were prepared from the plant materials, and FTIR analysis was conducted to determine the functional groups present in the extracts. GCMS analysis was performed to identify the chemical constituents of the extracts. The FTIR analysis revealed the presence of various functional groups, such as phenols, flavonoids, terpenoids, and alkaloids, known for their potential therapeutic activities. These functional groups are associated with antioxidant, anti-inflammatory, and anti-fibrotic properties. The GCMS analysis identified several bioactive compounds, including flavonoids, alkaloids, terpenoids, and phenolic compounds, which are known for their pharmacological activities. The discovery of bioactive compounds in African medicinal plants that exhibit anti-fibrotic effects, opens up promising avenues for further research and development of potential treatments for fibrosis. This suggests the potential of these plants as a valuable source of novel therapeutic agents for treating fibrosis-related conditions. In conclusion, our study identified and characterized bioactive compounds from selected African medicinal plants using FTIR and GCMS analysis. The presence of compounds with known antifibrotic properties suggests that these plants hold promise as a potential source of natural products for the development of novel anti-fibrotic therapies.

Keywords: uterine fibroids, african medicinal plants, bioactive compounds, identify and characterized

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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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Authors: Marisol Rodriguez-Duarte, Aide Saenz-Galindo, Carolina Flores-Gallegos, Raul Rodriguez-Herrera, Juan Ascacio-Valdes

Abstract:

The plant known as tarbush (Fluorensia cernua) is a plant originating in northern Mexico, mainly in the states of Coahuila, Durango, San Luis Potosí, Zacatecas and Chihuahua. It is a branched shrub that belongs to the family Asteraceae, has oval leaves of 6 to 11 cm in length and also has small yellow flowers. In Mexico, the tarbush is a very appreciated plant because it has been used as a traditional medicinal agent, for the treatment of gastrointestinal diseases, skin infections and as a healing agent. This plant has been used mainly as an infusion. Due to its traditional use, the content and type of phytochemicals present in the plant are currently unknown and are responsible for its biological properties, so its recovery and identification is very important because the compounds that it contains have relevant applications in the field of food, pharmaceuticals and medicine. The objective of this work was to determine the best extraction condition of phytochemical compounds (mainly polyphenolic compounds) from the leaf using ultrasound/microwave assisted extraction (U/M-AE). To reach the objective, U/M-AE extractions were performed evaluating three mass/volume ratios (1:8, 1:12, 1:16), three ethanol/water solvent concentrations (0%, 30% and 70%), ultrasound extraction time of 20 min and 5 min at 70°C of microwave treatment. All experiments were performed using a fractional factorial experimental design. Once the best extraction condition was defined, the compounds were recovered by liquid column chromatography using Amberlite XAD-16, the polyphenolic fraction was recovered with ethanol and then evaporated. The recovered polyphenolic compounds were quantified by spectrophotometric techniques and identified by HPLC/ESI/MS. The results obtained showed that the best extraction condition of the compounds was using a mass/volume ratio of 1:8 and solvent ethanol/water concentration of 70%. The concentration obtained from polyphenolic compounds using this condition was 22.74 mg/g and finally, 16 compounds of polyphenolic origin were identified. The results obtained in this work allow us to postulate the Mexican plant known as tarbush as a relevant source of bioactive polyphenolic compounds of food, pharmaceutical and medicinal interest.

Keywords: U/M-AE, tarbush, polyphenols, identification

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Authors: Babak Eslami

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Bimodal and trimodal AFM have provided additional capabilities to scanning probe microscopy characterization techniques. These capabilities have specifically enhanced material characterization of surfaces and provided subsurface imaging in addition to conventional topography images. Bimodal and trimodal AFM, being different techniques of multifrequency AFM, are based on exciting the cantilever’s fundamental eigenmode with second and third eigenmodes simultaneously. Although higher eigenmodes provide a higher number of observables that can provide additional information about the sample, they cause experimental challenges. In this work, different experimental approaches for enhancing AFM images in multifrequency for different characterization goals are provided. The trade-offs between eigenmodes including the advantages and disadvantages of using each mode for different samples (ranging from stiff to soft matter) in both air and liquid environments are provided. Additionally, the advantage of performing conventional single tapping mode AFM with higher eigenmodes of the cantilever in order to reduce sample indentation is discussed. These analyses are performed on widely used polymers such as polystyrene, polymethyl methacrylate and air nanobubbles on different surfaces in both air and liquid.

Keywords: multifrequency, sensitivity, soft matter, polymer

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Authors: Behzad Ali Khan, M. Zubair Akbar Qureshi

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The article analyzes the Darcy Forchheimer 2D Hybrid ferrofluid. The flow of a Hybrid ferrofluid is made due to an unsteady porous channel. The classical liquid water is treated as a based liquid. The flow in the permeable region is characterized by the Darcy-Forchheimer relation. Heat transfer phenomena are studied during the flow. The transformation of a partial differential set of equations into a strong ordinary differential frame is formed through appropriate variables. The numerical Shooting Method is executed for solving the simplified set of equations. In addition, a numerical analysis (ND-Solve) is utilized for the convergence of the applied technique. The influence of some flow model quantities like Pr (Prandtle number), r (porous medium parameter), F (Darcy-porous medium parameter), Re (Reynolds number), Pe (Peclet number) on velocity and temperature field are scrutinized and studied through sketches. Certain physical factors like f ''(η) (skin friction coefficient) and θ^'(η) (rate of heat transfer) are first derived and then presented through tables.

Keywords: darcy forcheimer, hybrid ferro fluid, porous medium, porous channel

Procedia PDF Downloads 174

Authors: Marinos Xagoraris, Elisavet Lazarou, Eleftherios Alissandrakis, Christos S. Pappas, Petros A. Tarantilis

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Strawberry tree (Arbutus unedo L.) and autumn heather (Erica manipuliflora Salisb.) are important beekeeping plants of Greece. Six monofloral honeys (four strawberry tree, two autumn heather) were analyzed by means of Solid Phase Micro-Extraction (SPME, 60 min, 60 oC) followed by Gas Chromatography coupled to Mass Spectrometry (GC-MS) for the purpose of assessing the botanical origin. A Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) fiber was employed, and benzophenone was used as internal standard. The volatile compounds with higher concentration (μg/ g of honey expressed as benzophenone) from strawberry tree honey samples, were α-isophorone (2.50-8.12); 3,4,5-trimethyl-phenol (0.20-4.62); 2-hydroxy-isophorone (0.06-0.53); 4-oxoisophorone (0.38-0.46); and β-isophorone (0.02-0.43). Regarding heather honey samples, the most abundant compounds were 1-methoxy-4-propyl-benzene (1.22-1.40); p-anisaldehyde (0.97-1.28); p-anisic acid (0.35-0.58); 2-furaldehyde (0.52-0.57); and benzaldehyde (0.41-0.56). Norisoprenoids are potent floral markers for strawberry-tree honey. β-isophorone is found exclusively in the volatile fraction of this type of honey, while also α-isophorone, 4-oxoisophorone and 2-hydroxy-isophorone could be considered as additional marker compounds. The analysis of autumn heather honey revealed that phenolic compounds are the most abundant and p-anisaldehyde; 1-methoxy-4-propyl-benzene; and p-anisic acid could serve as potent marker compounds. In conclusion, marker compounds for the determination of the botanical origin for these honeys could be identified as several norisoprenoids and phenolic components were found exclusively or in higher concentrations compared to common Greek honey varieties.

Keywords: SPME/GC-MS, volatile compounds, heather honey, strawberry tree honey

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Authors: Majid Javanmard

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Edible mushrooms are those agricultural products which contain high quantity of protein and can have special role in human diet. So search for methods to increase their shelf life is important. One of these strategies can be use of active packaging for absorb the ethylene which has been studied in present study. In this study, initially, production of impregnating zeolite with potassium permanganate has been studied with zeolite clinoptiolite available in iran. After that, these ethylene scavengers were placed in the package of edible mushrooms and then transferred to the refrigerator with temperature 4c for a period of 20 days. Each 5 days, several experiments accomplished on edible mushrooms such as weight loss, moisture content, color, texture, bacterial experiments and sensory evaluation. After production of impregnating zeolite with potassium permanganate (with a concentration of %2.5, %5, %7.5, %10 and %12.5) by zeolite type clinoptiolite (with mesh 35 and 60), samples have been analyzed with gas chromatography and titration with sodium oxalate. The results showed that zeolite by concentration of %5, %7.5 and %10 potassium permanganate and mesh 60 have a higher efficiency. Results from the experiments on edible mushrooms proved that impregnated zeolite with potassium permanganate have a meaningful influence in prevent the weight loss, decrease of moisture content and L-value, increase of a-value and overall color change (ΔE) and decrease of firmness texture of mushrooms. In addition, these absorbents can influence on decrease microbial load (mesophilic bacteria) rather than control. Generally, concluded that the impregnated zeolite with 10% permanganate potassium has a high efficiency on increase the shelf life of fresh edible mushrooms.

Keywords: active packaging, ethylene scavenger, zeolite clinoptiolite, permanganate potassium, shelf life

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Authors: Liliana Patricia Olivo Arias

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The present study focused on the hydrodynamic study in a three-phase fluidized bed reactor and the influence of important aspects, such as volume fractions (Hold up), velocity magnitude of gas, liquid and solid phases (hydrogen, gasoil, and gamma alumina), interactions of phases, through of drag models with the k-epsilon turbulence model. For this purpose was employed a Euler-Euler model and also considers the system is constituted of three phases, gaseous, liquid and solid, characterized by its physical and thermal properties, the transport processes that are developed within the transient regime. The proposed model of the three-phase fluidized bed reactor was solved numerically using the ANSYS-Fluent software with different mesh refinements on bed expansion zone in order to observe the influence of the hydrodynamic parameters and convergence criteria. With this model and the numerical simulations obtained for its resolution, it was possible to predict the results of the volume fractions (Hold ups) and the velocity magnitude for an unsteady system from the initial and boundaries conditions were established.

Keywords: three-phase fluidized bed system, CFD simulation, mesh dependency study, hydrodynamic study

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Authors: Patrícia T. Souza, Marina Ansolin, Eduardo A. C. Batista, Antonio J. A. Meirelles, Matthieu Tubino

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Lipid oxidation is a major cause of the deterioration of the quality of the biodiesel, because the waste generated damages the engines. Among the main undesirable effects are the increase of viscosity and acidity, leading to the formation of insoluble gums and sediments which cause the blockage of fuel filters. The auto-oxidation is defined as the spontaneous reaction of atmospheric oxygen with lipids. Unsaturated fatty acids are usually the components affected by such reactions. They are present as free fatty acids, fatty esters and glycerides. To determine the oxidative stability of biodiesels, through the induction period, IP, the Rancimat method is used, which allows continuous monitoring of the induced oxidation process of the samples. During the oxidation of the lipids, volatile organic acids are produced as byproducts, in addition, other byproducts, including alcohols and carbonyl compounds, may be further oxidized to carboxylic acids. By the methodology developed in this work using ion chromatography, IC, analyzing the water contained in the conductimetric vessel, were quantified organic anions of carboxylic acids in samples subjected to oxidation induced by Rancimat. The optimized chromatographic conditions were: eluent water:acetone (80:20 v/v) with 0.5 mM sulfuric acid; flow rate 0.4 mL min-1; injection volume 20 µL; eluent suppressor 20 mM LiCl; analytical curve from 1 to 400 ppm. The samples studied were methyl biodiesel from soybean oil and unsaturated fatty acids standards: oleic, linoleic and linolenic. The induced oxidation kinetics curves were constructed by analyzing the water contained in the conductimetric vessels which were removed, each one, from the Rancimat apparatus at prefixed intervals of time. About 3 g of sample were used under the conditions of 110 °C and air flow rate of 10 L h-1. The water of each conductimetric Rancimat measuring vessel, where the volatile compounds were collected, was filtered through a 0.45 µm filter and analyzed by IC. Through the kinetic data of the formation of the organic anions of carboxylic acids, the formation rates of the same were calculated. The observed order of the rates of formation of the anions was: formate >>> acetate > hexanoate > valerate for the oleic acid; formate > hexanoate > acetate > valerate for the linoleic acid; formate >>> valerate > acetate > propionate > butyrate for the linolenic acid. It is possible to suppose that propionate and butyrate are obtained mainly from linolenic acid and that hexanoate is originated from oleic and linoleic acid. For the methyl biodiesel the order of formation of anions was: formate >>> acetate > valerate > hexanoate > propionate. According to the total rate of formation these anions produced during the induced degradation of the fatty acids can be assigned the order of reactivity: linolenic acid > linoleic acid >>> oleic acid.

Keywords: anions of carboxylic acids, biodiesel, ion chromatography, oxidation

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Authors: Saheli Mitra, Ramesh Karri, Praveen K. Mylapalli, Arka. B. Dey, Gourav Bhattacharya, Gouriprasanna Roy, Syed M. Kamil, Surajit Dhara, Sunil K. Sinha, Sajal K. Ghosh

Abstract:

The most well-known structures of lyotropic liquid crystalline systems are the two dimensional hexagonal phase of cylindrical micelles with a positive interfacial curvature and the lamellar phase of flat bilayers with zero interfacial curvature. In aqueous solution of surfactants, the concentration dependent phase transitions have been investigated extensively. However, instead of changing the surfactant concentrations, the local curvature of an aggregate can be altered by tuning the electrostatic interactions among the constituent molecules. Intermediate phases with non-uniform interfacial curvature are still unexplored steps to understand the route of phase transition from hexagonal to lamellar. Understanding such structural evolution in lyotropic liquid crystalline systems is important as it decides the complex rheological behavior of the system, which is one of the main interests of the soft matter industry. Sodium dodecyl sulfate (SDS) is an anionic surfactant and can be considered as a unique system to tune the electrostatics by cationic additives. In present study, imidazolium-based ionic liquids (ILs) with different number of carbon atoms in their single hydrocarbon chain were used as the additive in the aqueous solution of SDS. At a fixed concentration of total non-aqueous components (SDS and IL), the molar ratio of these components was changed, which effectively altered the electrostatic interactions between the SDS molecules. As a result, the local curvature is observed to modify, and correspondingly, the structure of the hexagonal liquid crystalline phases are transformed into other phases. Polarizing optical microscopy of SDS and imidazole-based-IL systems have exhibited different textures of the liquid crystalline phases as a function of increasing concentration of the ILs. The small angle synchrotron x-ray diffraction (SAXD) study has indicated the hexagonal phase of direct cylindrical micelles to transform to a rectangular phase at the presence of short (two hydrocarbons) chain IL. However, the hexagonal phase is transformed to a lamellar phase at the presence of long (ten hydrocarbons) chain IL. Interestingly, at the presence of a medium (four hydrocarbons) chain IL, the hexagonal phase is transformed to another hexagonal phase of direct cylindrical micelles through the lamellar phase. To the best of our knowledge, such a phase sequence has not been reported earlier. Even though the small angle x-ray diffraction study has revealed the lattice parameters of these phases to be similar to each other, their rheological behavior has been distinctly different. These rheological studies have shed lights on how these phases differ in their viscoelastic behavior. Finally, the packing parameters, calculated for these phases based on the geometry of the aggregates, have explained the formation of the self-assembled aggregates.

Keywords: lyotropic liquid crystals, polarizing optical microscopy, rheology, surfactants, small angle x-ray diffraction

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