Search results for: Gel permeation chromatography

Authors: Mohammed Idaan Hassan Al-Majidi

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An analysis of twenty one assorted brands of vegetable oils in Babylon Iraq, reveals varying levels of cholesterol content. Cholesterol was found to be present in most of the oil brands sampled using three standard methods. Cholesterol was detected in seventeen of the vegetable oil brands with concentration of less than 1 mg/ml while seven of the oil brands had cholesterol concentrations ranging between 1-4 mg/ml. Low iodine values were obtained in four of the vegetable oil brands and three of them had high acid values. High performance liquid chromatography (HPLC) confirmed the presence of cholesterol at varying concentrations in all the oil brands and gave the lowest detectable cholesterol values in all the oil brands. The Laser brand made from rapeseed had the highest cholesterol concentration of 3.2 mg/ml while Grand brand made from groundnuts had the least concentration (0.12 mg/ml) of cholesterol using HPLC analysis. Leibermann-Burchard method showed that Gino brand from palm kernel had the least concentration of cholesterol (3.86 mg/ml ±0.032) and the highest concentration of 3.996 mg/ml ±0.0404 was obtained in Sesame seed oil brand. This report is important in view of health implications of cholesterol in our diets. Consequently, we have been able to show that there is no cholesterol free oil in the market as shown on the vegetable oil brand labels. Therefore, companies producing and marketing vegetable oils are enjoined to desist from misleading the public by labeling their products as “cholesterol free”. They should indicate the amount of cholesterol present in the vegetable oil, no matter how small the quantity may be.

Keywords: vegetable oils, heart diseases, leibermann-burchard, cholesterol

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Authors: Elgendy M. Eman, Sameeh Y. Manal

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Ginger (Zingiber officinale) is so important plant for its medicinal properties from ancient time and used as a spicy herb all over the world. This study was designed to examine the chemical composition of the essential oil and various crude extracts (n-hexane, chloroform and ethanol) of Zingiber officinale as well. GC–MS analyses of the essential oil resulted in the identification of 68 compounds,; 1,8-cineole (8.9%) and linalool (15.1%) were the main components in the essential oil .The crude extracts were analyzed with TLC plates and revealed several spots under UV light; however the hexane extract exhibited the highest number of spots compared to the other extracts. Hexane extract was selected for GC-MS profile, and the results revealed the presence of several volatile compounds and linalool was the major component with high percentage (11.4 %). Further investigation on the structure elucidation of the bioactive compound (linalool) using IR, GC-MS and NMR techniques compared to authenticated linalool then subjected to purification using preparative and column chromatography. Linalool has been epoxidized using m-chloroperbenzoicacid (mcpba) at room temperature in the presence of florescent lamps to give two cyclic oxygenated products (furan epoxide & pyran epoxide) as a stereospecific product.it is concluded that, oxidation process is enhanced by irradiation to form epoxide derivative, which acts as the precursor of important products.

Keywords: epoxide, ginger, irradiation, linalool

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Authors: Flávio A. F. da Ponte, Jackson Q. Malveira, José A. S. Ramos Filho, Monica C. G. Albuquerque

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The vegetable oils have many applications in industrial processes and due to this potential have constantly increased the demand for the use of low-quality oils, mainly in the production of biofuel. This work aims to the physicochemical evaluation of babassu oil (Orbinya speciosa) and coconut (Cocos nucifera) of low quality, as well the obtaining the free fatty acids 6 to 16 carbon atoms, with intention to be used as raw material for the biofuels production. The babassu oil and coconut low quality, as well the fatty acids obtained from these oils were characterized as their physicochemical properties and fatty acid composition (using gas chromatography coupled to mass). The NMR technique was used to assess the efficiency of fractional distillation under reduced pressure to obtain the intermediate carbonic chain fatty acids. The results showed that the bad quality in terms of physicochemical evaluation of babassu oils and coconut oils interfere directly in industrial application. However the fatty acids of intermediate carbonic chain (C6 to C16) may be used in cosmetic, pharmaceutical and particularly as the biokerosene fuel. The chromatographic analysis showed that the babassu oil and coconut oil have as major fatty acids are lauric acid (57.5 and 38.6%, respectively), whereas the top phase from distillation of coconut oil showed caprylic acid (39.1%) and major fatty acid.

Keywords: babassu oil (Orbinya speciosa), coconut oil (Cocos nucifera), fatty acids, biomass

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Authors: Natalina, Hwai Chyuan Onga, W. T. Chonga

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Oxidation stability of biodiesel is very important in fuel handling especially for remote location of biodiesel application. Variety of feedstocks and biodiesel production process resulted many variation of biodiesel oxidation stability. The current study relates to investigation of the impact of fatty acid composition that caused by natural and production process of calophyllum inophyllum palm oil methyl ester that correlated with improvement of biodiesel oxidation stability. Firstly, biodiesel was produced from crude oil of palm oil, calophyllum inophyllum and mixing of calophyllum inophyllum and palm oil. The production process of calophyllum inophyllum palm oil methyl ester (CIPOME) was divided by including washing process and without washing. Secondly, the oxidation stability was measured from the palm oil methyl ester (POME), calophyllum inophyllum methyl ester (CIME), CIPOME with washing process and CIPOME without washing process. Then, in order to find the differences of fatty acid compositions all of the biodiesels were measured by gas chromatography analysis. It was found that mixing calophyllum inophyllum into palm oil increased the oxidation stability. Washing process influenced the CIPOME fatty acid composition, and reduction of washing process during the production process gave significant oxidation stability number of CIPOME (38 h to 114 h).

Keywords: biodiesel, oxidation stability, calophyllum inophyllum, water content

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Authors: S. Techaoei, K. Jarmkom, P. Eakwaropas, W. Khobjai

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The objective of this research was focused on investigating in vitro antimicrobial activity of Phellinus linteus fruiting body extracts on Pseudomonas aeruginosa, Escherichia coli, Staphylococcus aureus and Methicillin-resistant Staphylococcus aureus. Phellinus linteus fruiting body was extracted with ethanol and ethyl acetate and was vaporized. The disc diffusion assay was used to assess antimicrobial activity against tested bacterial strains. Primary screening of chemical profile of crude extract was determined by using thin layer chromatography. The positive control and the negative control were used as erythromycin and dimethyl sulfoxide, respectively. Initial screening of Phellinus linteus crude extract with the disc diffusion assay demonstrated that only ethanol had greater antimicrobial activity against Pseudomonas aeruginosa, Escherichia coli, Staphylococcus aureus and Methicillin-resistant Staphylococcus aureus. The MIC assay showed that the lower MIC was observed with 0.5 mg/ml of Pseudomonas aeruginosa and Methicillin-resistant Staphylococcus aureus and 0.25 mg/ml. of Escherichia coli and Staphylococcus aureus, respectively. TLC chemical profile of extract was represented at R_f ≈ 0.71-0.76.

Keywords: Staphylococcus aureus, Escherichia coli, Phellinus linteus, Methicillin-resistant Staphylococcus aureus, antimicrobial activity

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Authors: Juergen Orasche, Vesta Kohlmeier, George C. Dragan, Gert Jakobi, Patricia Forbes, Ralf Zimmermann

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Underground mining poses a difficult environment for both man and machines. At more than 1000 meters underneath the surface of the earth, ores and other mineral resources are still gained by conventional and motorised mining. Adding to the hazards caused by blasting and stone-chipping, the working conditions are best described by the high temperatures of 35-40°C and high humidity, at low air exchange rates. Separate ventilation shafts lead fresh air into a mine and others lead expended air back to the surface. This is essential for humans and machines working deep underground. Nevertheless, mines are widely ramified. Thus the air flow rate at the far end of a tunnel is sensed to be close to zero. In recent years, conventional mining was supplemented by mining with heavy diesel machines. These very flat machines called Load Haul Dump (LHD) vehicles accelerate and ease work in areas favourable for heavy machines. On the other hand, they emit non-filtered diesel exhaust, which constitutes an occupational hazard for the miners. Combined with a low air exchange, high humidity and inorganic dust from the mining it leads to 'black smog' underneath the earth. This work focuses on the air quality in mines employing LHDs. Therefore we performed personal sampling (samplers worn by miners during their work), stationary sampling and aethalometer (Microaeth MA200, Aethlabs) measurements in a platinum mine in around 1000 meters under the earth’s surface. We compared areas of high diesel exhaust emission with areas of conventional mining where no diesel machines were operated. For a better assessment of health risks caused by air pollution we applied a separated gas-/particle-sampling tool (or system), with first denuder section collecting intermediate VOCs. These multi-channel silicone rubber denuders are able to trap IVOCs while allowing particles ranged from 10 nm to 1 µm in diameter to be transmitted with an efficiency of nearly 100%. The second section is represented by a quartz fibre filter collecting particles and adsorbed semi-volatile organic compounds (SVOC). The third part is a graphitized carbon black adsorber – collecting the SVOCs that evaporate from the filter. The compounds collected on these three sections were analyzed in our labs with different thermal desorption techniques coupled with gas chromatography and mass spectrometry (GC-MS). VOCs and IVOCs were measured with a Shimadzu Thermal Desorption Unit (TD20, Shimadzu, Japan) coupled to a GCMS-System QP 2010 Ultra with a quadrupole mass spectrometer (Shimadzu). The GC was equipped with a 30m, BP-20 wax column (0.25mm ID, 0.25µm film) from SGE (Australia). Filters were analyzed with In-situ derivatization thermal desorption gas chromatography time-of-flight-mass spectrometry (IDTD-GC-TOF-MS). The IDTD unit is a modified GL sciences Optic 3 system (GL Sciences, Netherlands). The results showed black carbon concentrations measured with the portable aethalometers up to several mg per m³. The organic chemistry was dominated by very high concentrations of alkanes. Typical diesel engine exhaust markers like alkylated polycyclic aromatic hydrocarbons were detected as well as typical lubrication oil markers like hopanes.

Keywords: diesel emission, personal sampling, aethalometer, mining

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Authors: Chahla Rahal, Philippe Refait

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Oleuropein-rich extract from olive leaf and acid hydrolysates, rich in hydroxytyrosol and elenolic acid was prepared under different experimental conditions. These phenolic compounds may be used as a corrosion inhibitor. The inhibitive action of these extracts and its major constituents on the corrosion of copper in 0.5 M NaCl solution has been evaluated by potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and weight loss measurements. The product of extraction was analyzed with high performance liquid chromatography (HPLC), whose analysis shows that olive leaf extract are greatly rich in phenolic compounds, mainly Oleuropeine (OLE), Hydroxytyrosol (HT) and elenolic acid (EA). After the acid hydrolysis and high temperature of extraction, an increase in hydroxytyrosol concentration was detected, coupled with relatively low oleuropeine content and high concentration of elenolic acid. The potentiodynamic measurements have shown that this extract acts as a mixed-type corrosion inhibitor, and good inhibition efficiency is observed with the increase in HT and EA concentration. These results suggest that the inhibitive effect of olive leaf extract might be due to the adsorption of the various phenolic compounds onto the copper surface.

Keywords: Olive leaf extract, Oleuropein, hydroxytyrosol, elenolic acid , Copper, Corrosion, HPLC/DAD, Polarisation, EIS

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Authors: Tanwarat Kajsongkram, Saowalux Rotamporn, Sirinat Limbunruang, Sirinan Thubthimthed.

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High-Performance Liquid Chromatography (HPLC) method was developed and validated for simultaneous estimation of 6-Gingerol(6G) and 6-Shogaol(6S) in joint pain relief gel containing ginger extract. The chromatographic separation was achieved by using C18 column, 150 x 4.6mm i.d., 5μ Luna, mobile phase containing acetonitrile and water (gradient elution). The flow rate was 1.0 ml/min and the absorbance was monitored at 282 nm. The proposed method was validated in terms of the analytical parameters such as specificity, accuracy, precision, linearity, range, limit of detection (LOD), limit of quantification (LOQ), and determined based on the International Conference on Harmonization (ICH) guidelines. The linearity ranges of 6G and 6S were obtained over 20-60 and 6-18 µg/ml respectively. Good linearity was observed over the above-mentioned range with linear regression equation Y= 11016x- 23778 for 6G and Y = 19276x-19604 for 6S (x is concentration of analytes in μg/ml and Y is peak area). The value of correlation coefficient was found to be 0.9994 for both markers. The limit of detection (LOD) and limit of quantification (LOQ) for 6G were 0.8567 and 2.8555 µg/ml and for 6S were 0.3672 and 1.2238 µg/ml respectively. The recovery range for 6G and 6S were found to be 91.57 to 102.36 % and 84.73 to 92.85 % for all three spiked levels. The RSD values from repeated extractions for 6G and 6S were 3.43 and 3.09% respectively. The validation of developed method on precision, accuracy, specificity, linearity, and range were also performed with well-accepted results.

Keywords: ginger, 6-gingerol, HPLC, 6-shogaol

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Authors: Najwa Othman, Norhidayah Suleiman, Gun Hean Chong

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Palm fatty acid distillate (PFAD) is a by-product of palm oil refineries which contains valuable compounds such as phytosterols, squalene, polycosanol, co-enzyme Q10 and vitamin E (tocopherols and tocotrienols). Approximately 0.7-1.0% of vitamin E accumulates in PFAD, and it functions as antioxidants and anti-inflammatory. The objective of this research is to evaluate the effect of manipulated variables in supercritical carbon dioxide towards the recovery of tocotrienols in PFAD. The vitamin E concentrate isolated varies depending on the pre-treatment of sample and extraction techniques. In this research, tocotrienols in PFAD was concentrated by removing the extraneous matters, especially free fatty acid (FFA) and acylglycerols. Pre-treatment method such as enzymatic hydrolysis by using lipase from Candida rugosa as an enzyme was used to remove FFA and improve recovery of vitamin E. After that, treated PFAD was extracted by using supercritical fluid extraction in co-current glass beads packed column (22 cm x 75 cm i.d) at different temperatures (40-60°C) and pressures (100-300 bar) for 5 hours. After the extraction, the sample was analyzed by using high-pressure liquid chromatography (HPLC) system to quantify the tocotrienols. The results indicated that a combined pressure (200 bar) and temperature (60°C) was predicted to provide highest tocotrienols yield and the extraction yield obtained was 106.45%.

Keywords: enzymatic hydrolysis, palm fatty acid distillate, supercritical fluid extraction, tocotrienols

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Authors: Bahdja Guerfi, N. Hadhoum, I. Azouz, M. Bendoumia, S. Bouafia, F. Z. Hadjadj Aoul

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Background: 'Penicillin V' is a narrow, bactericidal antibiotic of the beta-lactam family of the naturally occurring penicillin group. It is limited to infections due to the germs defined as sensitive. The objective of this work was to identify and to characterize Penicillin V acid and its related compounds by High-performance liquid chromatography (HPLC). Methods: Firstly phenoxymethylpenicillin was identified by an infrared absorption. The organoleptic characteristics, pH, and determination of water content were also studied. The dosage of Penicillin V acid active substance and the determination of its related compounds were carried on waters HPLC, equipped with a UV detector at 254 nm and Discovery HS C18 column (250 mm X 4.6 mm X 5 µm) which is maintained at room temperature. The flow rate was about 1 ml per min. A mixture of water, acetonitrile and acetic acid (65:35:01) was used as mobile phase for phenoxyacetic acid ‘impurity B' and a mixture of water, acetonitrile and acetic acid (650:150:5.75) for the assay and 4-hydroxypenicillin V 'impurity D'. Results: The identification of Penicillin V acid active substance and the evaluation of its chemical quality showed conformity with USP 35th edition. The Penicillin V acid content in the raw material is equal to 1692.22 UI/mg. The percentage content of phenoxyacetic acid and 4-hydroxypenicillin V was respectively: 0.035% and 0.323%. Conclusion: Through these results, we can conclude that the Penicillin V acid active substance tested is of good physicochemical quality.

Keywords: characterization, HPLC, Penicillin V acid, related substances

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Authors: Ikram Kamal, Mohamed Blaghen

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Petroleum hydrocarbons are serious problems and global pollutants in the environment due to their toxicity, carcinogenicity and persistent organic pollutant properties. One of the approaches to enhance biodegradation of petroleum hydrocarbons is to use biosurfactant. Biosurfactants are amphiphilic biomolecules produced as metabolic by-products from microorganisms they received considerable attention in the field of environmental remediation processes such as bioremediation. Biosurfactants have been considered as a desirable alternative to synthetic surfactants in various applications particularly in the environmental field. In comparison with their synthetic counterparts, biosurfactants have been reported to be less toxic, biodegradable and persistent. In this study we have investigated the potential of bacterial strains collected aseptically from the lagoon Marchika (water and soil) in Nador, Morocco; for the production of biosurfactants. This study also aimed to optimize the biosurfactant production process by changing the variables that influence the type and amount of biosurfactant produced by these microorganisms such as: carbon sources and also other physical and chemical parameters such as temperature and pH. Emulsification index, methylene blue test and thin layer chromatography (TLC) revealed the ability of strains used in this study to produce compounds that could emulsify gasoline. In addition, a HPLC/MS was used to separate and identify different biosurfactants purified.

Keywords: petroleum hydrocarbons, biosurfactants, biodegradation, lagoon marchika, emulsification index

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Authors: Ana Jurkeviciute, Larisa Grigorieva, Ksenia Moskvinа

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Oil shale alkylresorcinols are formed as a by-product in oil shale processing. They are unique raw material for chemical industry. Polycondensation resins obtaining is one of the worthwhile directions of oil shale alkylresorcinols use. These resins are widely applied in many branches of industry such as wood-working, metallurgic, tire, rubber products, construction etc. Possibility of resins obtaining using overall alkylresorcinols will allow to cheapen finished products on their base and to widen the range of resins offered on the market. Synthesis of polycondensation resins on the basis of alkylresorcinols was conducted by several methods in the process of investigations. In the formulations a part of resorcinol was replaced by fractions of oil shale alkylresorcinols containing different amount of 5-methylresorcinol (40-80 mass %). Some resins were modified by aromatic alkene at the stage of synthesis. Thermal stability and degradation behavior of resins were investigated by thermogravimetric analysis (TGA) method both in an inert nitrogen environment and in an oxidative environment of air. TGA integral curves were obtained and processed in dynamic mode for interval of temperatures from 25 to 830 °C. Rate of temperature rise was 5°C/min, gas flow rate - 50 ml/min. Resins power for carbonization was evaluated by carbon residue. Physical-chemical parameters of the resins were determined. Content of resorcinol and 5-methylresorcinol not reacted in the process of synthesis were determined by gas chromatography method.

Keywords: resorcinol, oil shale alkylresorcinols, aromatic alkene, polycondensation resins, modified resins

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Authors: Fatemeh Soltani, Simindokht Shirvani Arani, Ali Bahrami Samani, Mahdi Sadeghi, Kamal Yavari

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Cerium-141 [T1/2 = 32.501 days, Eβ (max) = 0.580 (29.8%) and 0.435(70.2%) MeV, Eγ=145.44 (48.2%) keV] possesses radionuclidic properties suitable for use in palliative therapy of bone metastases. 141Ce also has gamma energy of 145.44 keV, which resembles that of 99mTc. Therefore, the energy window is adjustable on the Tc-99m energy because of imaging studies. 141Ce can be produced through a relatively easy route that involves thermal neutron bombardment on natural CeO2 in medium flux research reactors (4–5×1013 neutrons/cm2•s). The requirement for an enriched target does not arise. Ethylenediamine tetramethylene phosphonic acid (EDTMP) was synthesized and radiolabeled with 141Ce. Complexation parameters were optimized to achieve maximum yields (>99%). The radiochemical purity of 141Ce-EDTMP was evaluated by radio-thin layer chromatography. The stability of the prepared formulation was monitored for one week at room temperature, and results showed that the preparation was stable during this period (>99%). Biodistribution studies of the complexes carried out in wild-type rats exhibited significant bone uptake with rapid clearance from blood. The properties of produced 141Ce-EDTMP suggest applying a new efficient bone pain palliative therapeutic agent to overcome metastatic bone pains.

Keywords: bone pain palliative, cerium-141, EDTMP, radiopharmaceutical

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Authors: Juzhong Tan, William Kerr

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Roasting is one critical procedure in chocolate processing, where special favors are developed, moisture content is decreased, and better processing properties are developed. Therefore, determination of roasting degree of cocoa bean is important for chocolate manufacturers to ensure the quality of chocolate products, and it also decides the commercial value of cocoa beans collected from cocoa farmers. The roasting degree of cocoa beans currently relies on human specialists, who sometimes are biased, and chemical analysis, which take long time and are inaccessible to many manufacturers and farmers. In this study, a self-made electronic nose system consists of gas sensors (TGS 800 and 2000 series) was used to detecting the gas generated by cocoa beans with a different roasting degree (0min, 20min, 30min, and 40min) and the signals collected by gas sensors were used to train a three-layers ANN. Chemical analysis of the graded beans was operated by traditional GC-MS system and the contents of volatile chemical compounds were used to train another ANN as a reference to electronic nosed signals trained ANN. Both trained ANN were used to predict cocoa beans with a different roasting degree for validation. The best accuracy of grading achieved by electronic nose signals trained ANN (using signals from TGS 813 826 820 880 830 2620 2602 2610) turned out to be 96.7%, however, the GC trained ANN got the accuracy of 83.8%.

Keywords: artificial neutron network, cocoa bean, electronic nose, roasting

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Authors: Luxy Grebers Swend Sinaga, Akhmaloka

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The global energy crisis, triggered by declining fossil The global energy crisis, triggered by declining fossil fuel reserves and exacerbated by population growth and increasing energy demand, was driven the development of renewable energy sources. One of the green energy alternatives being developed is biodiesel. Transesterification is at the core of biodiesel production, where fatty acids in oil are converted into methyl esters with the aid of a catalyst. Lipases exhibit high activity and stability during catalysis, especially under harsh conditions. Lipase (Lk1) isolated from organic waste compost at the Bandung Institute of Technology, Bandung, West Java, shows promising potential in this field. The thermostable lipase was purified using Ni-NTA affinity chromatography, followed by SDS-PAGE analysis for purity confirmation. Characterizing the transesterification activity of Lk1 is essential for assessing its effectiveness in converting oil into biodiesel, including methyl esters. The results of this study showed that Lk1 exhibited the highest activity on a methyl palmitate substrate, with an optimum temperature of 60°C, very stable activity in the non-polar solvent n-hexane, and was able to maintain its optimum activity for up to 1 hour. These characters make Lk1 highly suitable for biodiesel production, as it meets the main criteria for the transesterification process in producing renewable energy.

Keywords: biodiesel, lipase Lk1, transesterification, renewable energy, thermostability

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Authors: Kaustuvmani Patowary, Suresh Deka

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Oil pollution accidents, nowadays, have become a common phenomenon and have caused ecological and social disasters. Microorganisms with high oil-degrading performance are essential for bioremediation of petroleum hydrocarbon. In this investigation, an effective biosurfactant producer and hydrocarbon degrading bacterial strain, Pseudomonas sp.PG1 (identified by 16s rDNA sequencing) was isolated from hydrocarbon contaminated garage soil of Pathsala, Assam, India, using crude oil enrichment technique. The growth parameters such as pH and temperature were optimized for the strain and upto 81.8% degradation of total petroleum hydrocarbon (TPH) has been achieved after 5 weeks when grown in mineral salt media (MSM) containing 2% (w/v) crude oil as the carbon source. The biosurfactant production during the course of hydrocarbon degradation was monitored by surface tension measurement and emulsification activity. The produced biosurfactant had the ability to decrease the surface tension of MSM from 72 mN/m to 29.6 mN/m, with the critical micelle concentration (CMC)of 56 mg/L. The biosurfactant exhibited 100% emulsification activity on crude oil. FTIR spectroscopy and LCMS-MS analysis of the purified biosurfactant revealed that the biosurfactant is Rhamnolipidic in nature with several rhamnolipid congeners. Gas Chromatography-Mass spectroscopy (GC-MS) analysis clearly demonstrated that the strain PG1 efficiently degrade different hydrocarbon fractions of the crude oil. The study suggeststhat application of the biosurfactant producing strain PG1 as an appropriate candidate for bioremediation of crude oil contaminants.

Keywords: petroleum hydrocarbon, hydrocarbon contamination, bioremediation, biosurfactant, rhamnolipid

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Authors: Angelo Garofalo, Laura Donato, Maria Concetta Carnevale, Enrico Drioli, Omar Alharbi, Saad Aljlil, Alessandra Criscuoli, Catia Algieri

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Nowadays, water scarcity may be considered one of the most important and serious questions concerning our community: in fact, there is a remarkable mismatch between water supply and water demand. Exploitation of natural fresh water resources combined with higher water demand has led to an increased requirement for alternative water resources. In this context, desalination provides such an alternative source, offering water otherwise not accessible for irrigational, industrial and municipal use. Considering the various drawbacks of the polymeric membranes, zeolite membranes represent a potential device for water desalination owing to their high thermal and chemical stability. In this area wide attention was focused on the MFI (silicalite, ZSM-5) membranes, having a pore size lower (about 5.5 Å) than the major kinetic diameters of hydrated ions. In the present work, a scale-up for the preparation of supported silicalite membranes was performed. Therefore, tubular membranes 30 cm long were synthesized by using the secondary growth method coupled with the cross flow seeding procedure. The secondary growth presents two steps: seeding and growth of zeolite crystals on the support. This process, decoupling zeolite nucleation from crystals growth, permits to control the conditions of each step separately. The seeding procedure consists of a cross-flow filtration through a porous support coupled with the support rotation and tilting. The combination of these three different aspects allows a homogeneous and uniform coverage of the support with the zeolite seeds. After characterization by scanning electron microscope (SEM), X-ray diffractometry (XRD) and Energy-dispersive X-ray (EDX) analysis, the prepared membranes were tested by means of single gas permeation and then by Vacuum Membrane Distillation (VMD) using both deionized water and NaCl solutions. The experimental results evidenced the possibility to perform the scale up for the preparation of almost defect free silicalite membranes. VMD tests indicated the possibility to prepare membranes that exhibit interesting performance in terms of fluxes and salt rejections for concentrations from 0.2 M to 0.9 M. Furthermore, it was possible to restore the original performance of the membrane after an identified cleaning procedure. Acknowledgements: The authors gratefully acknowledge the support of the King Abdulaziz City for Science and Technology (KACST) for funding the research Project 895/33 entitled ‘Preparation and Characterization of Zeolite Membranes for Water Treatment’.

Keywords: desalination, MFI membranes, secondary growth, vacuum membrane distillation

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Authors: Leonce Dusengemungu

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Filamentous fungi indigenous to heavy metals (HMs) contaminated environments have a considerable biosorption potential yet are currently under-investigated in developing countries. In the work presented herein, the biosorption potential of three indigenous filamentous fungi (Aspergillus transmontanensis, Cladosporium cladosporioides, and Geotrichum candidum) isolated from copper and cobalt mining wasteland sites in Zambia's Copperbelt province was investigated. In Cu and Co tolerance tests, all the fungal isolates were shown to be tolerant, with mycelial growth at HMs concentrations of up to 7000 ppm. However, exposure to high Cu and Co concentrations hindered the growth of the three strains to varying degrees, resulting in reduced mycelial biomass (evidenced by loss of the infrared bands at 887 and 930 cm-1 of the 1,3-glucans backbone) as well as morphological alterations, sporulation, and pigment synthesis. In addition, gas chromatography-mass spectrometry characterization of the fungal biomass extracts allowed to detect changes in the chemical constituents upon exposure to HMs, with profiles poorer in maltol, 1,2-cyclopentadione, and n-hexadecanoic acid, and richer in furaldehydes. Biosorption tests showed that A. transmontanensis and G. candidum showed better performance as bioremediators than C. cladosporioides, with biosorption efficiencies of 1645, 1853 and 1253 ppm at pH 3, respectively, and may deserve further research in field conditions.

Keywords: bioremediation, fungi, biosorption, heavy metal

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Authors: Oktira Roka Aji, Maelita R. Moeis, Ihsanawati, Ernawati A. Giri-Rachman

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Globally, tuberculosis (TB) remains a leading cause of death. The emergence of multidrug-resistant strains and extensively drug-resistant strains have become a major public concern. One of the potential candidates for drug target is the cytoplasmic domain of PhoR Histidine Kinase, a part of the Two Component System (TCS) PhoR-PhoP in Mycobacterium tuberculosis (Mtb). TCS PhoR-PhoP relay extracellular signal to control the expression of 114 virulent associated genes in Mtb. The 3D structure of PhoR cytoplasmic domain is needed to screen novel drugs using structure based drug discovery. The PhoR cytoplasmic domain from Mtb H37Rv was overexpressed in E. coli BL21(DE3), then purified using IMAC Ni-NTA Agarose his-tag affinity column and DEAE-ion exchange column chromatography. The molecular weight of the purified protein was estimated to be 37 kDa after SDS-PAGE analysis. This sample was used for pre-crystallization screening by applying sitting drop vapor diffusion method using Natrix (HR2-116) 48 solutions crystal screen kit at 25ºC. Needle-like crystals were observed after the seventh day of incubation in test solution No.47 (0.1 M KCl, 0.01 M MgCl2.6H2O, 0.05 M Tris-Cl pH 8.5, 30% v/v PEG 4000). Further testing is required for confirming the crystal.

Keywords: tuberculosis, two component system, histidine kinase, needle-like crystals

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Authors: Bashar Al-Sabti, Jehad Harbali

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

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

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Authors: Yu Zhang, Il Kim

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Polypeptides with defined peptide sequences illustrate the power of remarkable applications in drug delivery, tissue engineering, sensing and catalysis. Especially the cyclic polypeptides, the distinctive topological architecture imparts many characteristic properties comparing to linear polypeptides. Here, a facile and highly efficient strategy for the synthesis of linear and cyclic polypeptides is reported using N-heterocyclic carbenes (NHCs)-mediated ring-opening polymerization (ROP) of α-amino acid N-carboxyanhydrides (NCA) in the presence or absence of primary amine initiator. The polymerization proceeds rapidly in a quasi-living manner, allowing access to linear and cyclic polypeptides of well-defined chain length and narrow polydispersity, as evidenced by nuclear magnetic resonance spectrum (1H NMR and 13C NMR spectra) and size exclusion chromatography (SEC) analysis. The cyclic architecture of the polypeptides was further verified by matrix-assisted laser desorption ionization-time of flight (MALDI-TOF) mass spectra (MALDI-TOF MS) and electrospray ionization (ESI) mass spectra, as well as viscosity studies. This approach can also simplify workup procedures and make bulk scale synthesis possible, which thereby opens avenues for practical uses in diverse areas, opening up the new generation of polypeptide synthesis.

Keywords: α-amino acid N-carboxyanhydrides, living polymerization, polypeptides, N-heterocyclic carbenes, ring-opening polymerization

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Authors: Salem Abdalla

Abstract:

Objective: Dipyrone is a widely used, well tolerated analgesic drug which, however, is compromised by agranulocytosis as an adverse effect. Subsequent to no enzymatic hydrolysis, the primary metabolic step is N-demethylation of 4-methylaminoantipyrine (4-MAA) to 4-aminoantipyrine (4-AA). The aim of the present study was to identify the cytochrome P-450 enzyme (CYP) mediating this reaction. Methods: We identified the relevant CYP using virus expressed isolated rat liver microsomes with chemical inhibition studies. The substrate of 4-methylaminantipyrine was employed at six different concentrations (25, 50, 100, 400, 800, and 1200 µmol/l) with varying concentrations of selective inhibitors of CYP1A2 (furafylline, fluvoxamine), CYP3A4 (ketoconazole), CYP2A6 (coumarin), CYP2D6 (quinidine), CYP2C19 (omeprazole, fluvoxamine, tranylcypromine), CYP2C9 (sulfaphenazole), and CYP1A1 (alpha-naphthoflavone). 4-MAA and 4-AA were analyzed by HPLC, and enzyme kinetic parameters (Km and Vmax) were determined by regression (Sigma plot 9.0). Results: The N-demethylation of 4-MAA by microsomes prepared from baculovirus-expressing human CYP was pronounced with CYP2C19. Intrinsic clearances of the most active enzymes were 0.092, 0.027, and 0.026 for the CYP enzymes 2C19, 2D6, and 1A2, respectively. Metabolism by rat liver microsomes was strongly inhibited by omeprazole (IC50 of 0.05). Conclusion: The enzyme CYP2C19 apparently has an important role in N-demethylation of 4-methylaminoantipyrine which should be further analyzed in clinical studies and which may also be interesting concerning the agranulocytosis.

Keywords: dipyrone, 4-methylaminoantipyrine (4-MAA), 4- aminoantipyrine (4-AA), metabolism, human CYP2C19

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Authors: Omasan Urhie Urhie, Adenipekun C. O, Eke W., Ogwu K., Erinle K. O

Abstract:

Polychlorinated Biphenyls (PCBs) are Persistent organic pollutants (POPs) that are very toxic; they possess ability to accumulate in soil and in human tissues hence resulting in health issues like birth defect, reproductive disorder and cancer. The air is polluted by PCBs through volatilization and dispersion; they also contaminate soil and sediments and are not easily degraded. Soil samples were collected from a depth of 0-15 cm from three substations (Warri, Ughelli and Ibadan) of Power Holding Company of Nigeria (PHCN) where old transformers were dumped in Nigeria. Extraction and cleanup of soil samples were conducted using Accelerated Solvent Extraction (ASE) with Pressurized Liquid extraction (PLE). The concentration of PCBs was determined using gsas chromatography/mass spectrometry (GC/MS). Mean total PCB concentrations in the soil samples increased in the order Ughelli ˂ Ibadan˂ Warri, 2.457757ppm Ughelli substation 4.198926ppm, for Ibadan substation and 14.05065ppm at Warri substation. In the Warri samples, PCB-167 was the most abundant at about 30% (4.28086ppm) followed by PCB-157 at about 20% (2.77871), of the total PCB concentrations (14.05065ppm). Of the total PCBs in the Ughelli and Ibadan samples, PCB-156 was the most abundant at about 44% and 40%, respectively. This study provides a baseline report on the presence of PCBs in the vicinity of abandoned electrical power facilities in different cities in Nigeria.

Keywords: polychlorintated biphenyls, persistent organic pollutants, soil, transformer

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Authors: Tripti Mishra, Shipra Shukla, Sanjeev Meena, , Ruchi Singh, Mahesh Pal, D. K. Upreti, Dipak Datta

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Roccella montagnei belongs to lichen family Roccelleceae growing luxuriantly along the coastal regions of India. As Roccella has been shown to be bioactive, we prepared methanolic extract and assessed its anticancer potential. The methanolic extract showed significant in vitro cytotoxic activity against four human cancer cell lines such as Colon (DLD-1, SW-620), Breast (MCF-7), Head and Neck (FaDu). This prompted us to isolate bioactive compounds through column chromatography. Two compounds Roccellic acid and Everninic acid have been isolated, out of which Everninic acid is reported for the first time. Both the compounds have been tested for in vitro cytotoxic activity in which Roccellic acid showed strong anticancer activity as compared to the Everninic acid. CDK-10 (Cyclin-dependent kinase) contributes to proliferation of cancer cells, and aberrant activity of these kinases has been reported in a wide variety of human cancers. These kinases, therefore, constitute biomarkers of proliferation and attractive pharmacological targets for the development of anticancer therapeutics. Therefore both the isolated compounds were tested for in silico molecular docking study against CDK-10 isomer enzyme to support the cytotoxic activity.

Keywords: cytotoxic activity, everninic acid, roccellic acid, R. montagnei

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Authors: S. Obregon-Cano, R. Moreno-Rojas, E. Cartea-Gonzalez, A. De Haro-Bailon

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The potential of near-infrared spectroscopy (NIRS) for screening the total glucosinolate (t-GSL) content, and also, the aliphatic glucosinolates gluconapin (GNA), progoitrin (PRO) and glucobrassicanapin (GBN) in turnip greens and turnip tops was assessed. This crop is grown for edible leaves and stems for human consumption. The reference values for glucosinolates, as they were obtained by high performance liquid chromatography on the vegetable samples, were regressed against different spectral transformations by modified partial least-squares (MPLS) regression (calibration set of samples n= 350). The resulting models were satisfactory, with calibration coefficient values from 0.72 (GBN) to 0.98 (tGSL). The predictive ability of the equations obtained was tested using a set of samples (n=70) independent of the calibration set. The determination coefficients and prediction errors (SEP) obtained in the external validation were: GNA=0.94 (SEP=3.49); PRO=0.41 (SEP=1.08); GBN=0.55 (SEP=0.60); tGSL=0.96 (SEP=3.28). These results show that the equations developed for total glucosinolates, as well as for gluconapin can be used for screening these compounds in the leaves and stems of this species. In addition, the progoitrin and glucobrassicanapin equations obtained can be used to identify those samples with high, medium and low contents. The calibration equations obtained were accurate enough for a fast, non-destructive and reliable analysis of the content in GNA and tGSL directly from NIR spectra. The equations for PRO and GBN can be employed to identify samples with high, medium and low contents.

Keywords: brassica rapa, glucosinolates, gluconapin, NIRS, turnip greens

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Authors: Gurleen Kour, Mowkshi Khullar, B. K. Chandan, Parvinder Pal Singh, Kushalava Reddy Yumpalla, Gurunadham Munagala, Ram A. Vishwakarma, Zabeer Ahmed

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New chemotherapeutic compounds against multidrug-resistant Mycobacterium tuberculosis (Mtb) are urgently needed to combat drug resistance in tuberculosis (TB). Apart from in-vitro potency against the target, physiochemical properties and pharmacokinetic properties play an imperative role in the process of drug discovery. We have identified novel nitroimidazole derivatives with potential activity against mycobacterium tuberculosis. One lead candidates, MCD-017, which showed potent activity against H37Rv strain (MIC=0.5µg/ml) and was further evaluated in the process of drug development. Methods: Basic physicochemical parameters like solubility and lipophilicity (LogP) were evaluated. Thermodynamic solubility was determined in PBS buffer (pH 7.4) using LC/MS-MS. The partition coefficient (Log P) of the compound was determined between octanol and phosphate buffered saline (PBS at pH 7.4) at 25°C by the microscale shake flask method. The compound followed Lipinski’s rule of five, which is predictive of good oral bioavailability and was further evaluated for metabolic stability. In-vitro metabolic stability was determined in rat liver microsomes. The hepatotoxicity of the compound was also determined in HepG2 cell line. In vivo pharmacokinetic profile of the compound after oral dosing was also obtained using balb/c mice. Results: The compound exhibited favorable solubility and lipophilicity. The physical and chemical properties of the compound were made use of as the first determination of drug-like properties. The compound obeyed Lipinski’s rule of five, with molecular weight < 500, number of hydrogen bond donors (HBD) < 5 and number of hydrogen bond acceptors(HBA) not more then 10. The log P of the compound was less than 5 and therefore the compound is predictive of exhibiting good absorption and permeation. Pooled rat liver microsomes were prepared from rat liver homogenate for measuring the metabolic stability. 99% of the compound was not metabolized and remained intact. The compound did not exhibit cytoxicity in hepG2 cells upto 40 µg/ml. The compound revealed good pharmacokinetic profile at a dose of 5mg/kg administered orally with a half life (t1/2) of 1.15 hours, Cmax of 642ng/ml, clearance of 4.84 ml/min/kg and a volume of distribution of 8.05 l/kg. Conclusion : The emergence of multi drug resistance (MDR) and extensively drug resistant (XDR) Tuberculosis emphasize the requirement of novel drugs active against tuberculosis. Thus, the need to evaluate physicochemical and pharmacokinetic properties in the early stages of drug discovery is required to reduce the attrition associated with poor drug exposure. In summary, it can be concluded that MCD-017 may be considered a good candidate for further preclinical and clinical evaluations.

Keywords: mycobacterium tuberculosis, pharmacokinetics, physicochemical properties, hepatotoxicity

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Authors: Ikram Kamal, Mohamed Blaghen

Abstract:

Biosurfactants are amphiphilic biological compounds consisting of hydrophobic and hydrophilic domains produced extracellularly or as part of the cell membrane by a variety of yeast, bacteria and filamentous fungi. Biosurfactant applications in the environmental industries are promising due to their biodegradability, low toxicity, and effectiveness in enhancing biodegradation and solubilization of low solubility compounds. Currently, the main application is for enhancement of oil recovery and hydrocarbon bioremediation due to their biodegradability and low critical micelle concentration (CMC). The use of biosurfactants has also been proposed for various industrial applications, such as in food additives, cosmetics, detergent formulations and in combinations with enzymes for wastewater treatment. In this study, we have investigated the potential of bacterial strains: Mannheimia haemolytica, Burkholderia cepacia and Serratia ficaria were collected aseptically from the lagoon Marchika (water and soil) in Nador, Morocco; for the production of biosurfactants. This study also aimed to optimize the biosurfactant production process by changing the variables that influence the type and amount of biosurfactant produced by these microorganisms such as: carbon sources and also other physical and chemical parameters such as temperature and pH. Emulsification index, methylene blue test, and thin layer chromatography (TLC) revealed the ability of strains used in this study to produce compounds that could emulsify gasoline. In addition, a GC/MS was used to separate and identify different biosurfactants purified.

Keywords: biosurfactants, Mannheimia haemolytica, biodegradability, Burkholderia cepacia, Serratia ficaria

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Authors: Sumbul Farhat, Pratyay Vaibhav, Sarah Jain, Kapinder Kumar, Archna Kumar

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The Diamondback Moth, Plutella xylostella (Linnaeus), is a major pest of cole crops that causes approximately 50% loss in global production. The utilization of inorganic pesticides is reflected in the development of resistance to this pest. Thus, there is a great need for an eco-friendly, sustainable strategy for the control of this pest. Although this pest, several natural enemies are reported worldwide, none of them can control it efficiently. Therefore, a proposed study is planned to understand the Volatile Organic Compounds (VOCs) mediated signaling interaction mechanism of the plant, pest, and natural enemy. For VOCs collection during different deployment stages of Cabbage POI, Green Ball, Pusa Cabbage, Cabbage Local, Snowball 16, Kanchan Plus, Pusa Meghna, Farm Sona Hybrid F1, and Samridhi F1 Hybrid, the Solid-phase microextraction (SPME) method was employed. Characterization of VOCs was conducted by Gas Chromatography-Mass Spectrometry (GC-MS). The impact of collected VOCs was assessed through Y-Tube Bioassays. The results indicate that the Cabbage variety Green Ball shows maximum repellency for P. xylostella (-100%). The cues present in this variety may be exploited for efficient management of P. xylostella in the cole crop ecosystem.

Keywords: Plutella xylostella, cole crops, volatile organic compounds, GC-MS, Green Ball

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Authors: O. Smara, H. Dendougui, B. Legseir

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Atriplex halimus L. is particularly well adapted to arid and salt-affected areas. In this species, salinity resistance is often attributed to the presence of vesiculated hairs covering leaf surface and containing a large amount of salt. Atriplex halimus L. (Chenopodiaceae) is a perennial shrub native to the Mediterranean basin with excellent tolerance to drought and salinity. The species is present in semiarid to subhumid areas of the north Mediterranean and in arid zones from North Africa and the eastern Mediterranean. The main aim of this study was to identify a medicinal plant used in the Ouargla (Est-southern Algeria) for the treatment of several human pathologies. This plant is an important source for livestock in nitrogenous matter, it is an effective and relatively inexpensive tool in the fight against erosion and desertification and rehabilitation of degraded lands. Phytochemical investigation is applied to the majority of extracts of the powder of the aerial parts of Atriplex halimus L. Different chromatographic methods after liquid-liquid extraction are used; it is the thin layer chromatography (TLC) and paper using multiple systems and chemical revelations. This study followed by an evaluation by the phenol assay the Folin-Ciocalteu method, using gallic acid as a reference for phenols and quercetin for flavonols. Some polar extracts showed an interesting result better than the less polar extracts.

Keywords: Atriples halimus L., chenopodiaceae, flavonoids, phenols

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Authors: Youn Young Shim, Ji Hye Kim, Jae Youl Cho, Martin JT Reaney

Abstract:

Flaxseed (Linumusitatissimum L.) is gaining popularity in the food industry as a superfood due to its health-promoting properties. Linusorbs (LOs, a.k.a. Cyclolinopeptide) are bioactive compounds present in flaxseed exhibiting potential health effects. The study focused on the effects of processing and storage on the stability of flaxseed-derived LOs added to various bakery products. The flaxseed meal fortified gluten-free (GF) bakery bread was prepared, and the changes of LOs during the bread-making process (meal, fortified flour, dough, and bread) and storage (0, 1, 2, and 4 weeks) at different temperatures (−18 °C, 4 °C, and 22−23 °C) were analyzed by high-performance liquid chromatography-diode array detection. The total oxidative LOs and LO1OB2 were almost kept stable in flaxseed meals at storage temperatures of 22−23 °C, −18 °C, and 4 °C for up to four weeks. Processing steps during GF-bread production resulted in the oxidation of LOs. Interestingly, no LOs were detected in the dough sample; however, LOs appeared when the dough was stored at −18 °C for one week, suggesting that freezing destroyed the sticky structure of the dough and resulted in the release of LOs. The final product, flaxseed meal fortified bread, could be stored for up to four weeks at −18 °C and 4 °C, and for one week at 22−23 °C. All these results suggested that LOs may change during processing and storage and that flaxseed flour-fortified bread should be stored at low temperatures to preserve effective LOs components.

Keywords: linum usitatissimum L., flaxseed, linusorb, stability, gluten-free, peptides, cyclolinopeptide

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