Search results for: Chromatography

Authors: S. Yodyingyong, C. Chaichana, C. Nuchsuk, S. Roytrakul, N. P. T-Thienprasert, S. Ratanapo

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Protein hydrolysates prepared from a number of medicinal plants are promising sources of various bioactive peptides. In this work, proteins from dried whole plant of Euphorbia hirta Linn. were extracted and digested with pepsin for 12h. The hydrolysates of lesser than 3 KDa were fractionated by a cut-off membrane. The peptide hydrolysate was then purified by an anion-exchange chromatography on DEAE-Sephacel™ column and reverse-phase chromatography on Sep-pak C₁₈ column, respectively. The cytotoxic effect of each peptide fraction against a gastric carcinoma cell line (KATO-III, ATCC No. HTB103) was investigated using colorimetric MTT viability assay. A human liver cell line (Chang Liver, CLS No. 300139) was used as a control normal cell line. Two purified peptide peaks, peak l and peak ll at 100µg peptides mL^-1 affected cell viability of the gastric cancer cell lines to 63.85±4.94 and 66.92±6.46%, respectively. Our result showed for the first time that the peptide fractions derived from protein hydrolysate of Euphorbia hirta Linn. have anti-gastric cancer activity, which offers a potential novel and natural anti-gastric cancer remedy.

Keywords: Cytotoxic, peptides, Euphorbia hirta Linn., gastric carcinoma.

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Authors: Sharareh Sharifi, Pargol Ghavam Mostafavi, Ali Mashinchian Moradi, Mohammad Hadi Givianrad, Hassan Niknejad

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Marine organisms such as soft coral, sponge, ascidians, and tunicate containing rich source of natural compound have been studied in last decades because of their special chemical compounds with anticancer properties. The aim of this study was to investigate anti-cancer property of ethyl acetate extracted from marine sea pen Virgularia gustaviana found from Persian Gulf coastal (Bandar Abbas). The extraction processes were carried out with ethyl acetate for five days. Thin layer chromatography (TLC) and high-performance liquid chromatography (HPLC) were used for qualitative identification of crude extract. The viability of HeLa and MDA-Mb-231 cancer cells was investigated using MTT assay at the concentration of 25, 50, and a 100 µl/ml of ethyl acetate is extracted. The crude extract of Virgularia gustaviana demonstrated ten fractions with different Retention factor (Rf) by TLC and Retention time (Rt) evaluated by HPLC. The crude extract dose-dependently decreased cancer cell viability compared to control group. According to the results, the ethyl acetate extracted from Virgularia gustaviana inhibits the growth of cancer cells, an effect which needs to be further investigated in the future studies.

Keywords: Virgularia gustaviana, Cembrane Diterpene, anti-cancer, HeLa cancer Cell, MDA-Md-231 Cancer cell.

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

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

Keywords: Alcohol dehydrogenases, DES, gas chromatography, RasADH.

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

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

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

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Authors: D. Selvi Gökkaya, M. Yüksel, M. Sağlam, T. Güngören Madenoğlu, N. Cengiz, T. Çokkuvvetli, L. Ballice

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In this study, production possibilities of hydrogen and/or methane via SCWG from black grape residues have been investigated. For this aim, grape residues which remain as a byproduct of the wine making process have been used. Since utilization from grape residues is limited due to the high moisture content, supercritical water gasification is the most convenient method. The effect of the gasification temperature and type of catalyst on supercritical water gasification have been investigated. Gasification experiments were performed in a batch autoclave at four different temperatures 300, 400, 500 and 600°C. K2CO3 and Trona (NaHCO3.Na2CO3·2H2O) were used as catalyst. Real biomass types of black grape residues have been successfully gasified and the product gas (hydrogen, methane, carbon dioxide, carbon monoxide and a small amount of ethane and ethylene) were identified by using gas chromatography. A TOC analyzer was used to determine total organic carbon (TOC) content of aqueous phase. The amounts of carboxylic acids, aldehydes, ketones, furfurals and phenols present in the aqueous solutions were analyzed by high performance liquid chromatography. When the temperature increased from 300°C to 600°C, mol% of H2 in gas products increased. The presence of catalysts improves the hydrogen yield. Trona showed gasification activity to be similar to that of K2CO3. It may be concluded that the use of Trona instead of commercially produced catalysts, can be preferably used in the gasification of biomass in supercritical water.

Keywords: Biomass, hydrogen, grape residues.

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

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

Keywords: Biomarkers, fingerprint profiling, gallic acid, HPTLC, Protorhus longifolia.

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

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

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

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Authors: Sarun Keithmaleesatti, Pakorn Varanusupakul, Wattasit Siriwong, Kumthorn Thirakhupt, Mark Robson, Noppadon Kitana

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Organochlorine pesticides (OCPs) are known to be persistent and bioaccumulative toxicants that may cause reproductive impairments in wildlife as well as human. The current study uses the snail-eating turtle Malayemys macrocephala, a long-lived animal commonly distribute in rice field habitat in central part of Thailand, as a sentinel to monitor OCP contamination in environment. The nest soil, complete clutch of eggs, and blood of the turtle were collected from agricultural areas in the Chao Phraya River Basin, Thailand during the nesting season of 2007-2008. The novel methods for tissue extraction by an accelerated solvent extractor (ASE, for egg) and liquid-liquid extraction (for blood) have been developed. The nineteen OCP residues were analyzed by gas chromatography with micro-electron captured detector (GC-μECD). The validated methods have met requirements of the AOAC standard. The results indicated that significant amounts of OCPs are still contaminated in nest soil and eggs of the turtle even though the OCPs had been banned in this area for many years. This suggested the potential risk to health of wildlife as well as human in the area.

Keywords: Gas chromatography, persistent organic pollutants, rice field, sentinel species.

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Authors: Dmitry Yu. Korulkin, Raissa A. Muzychkina

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In review the generalized data about different methods of extraction, separation and purification of natural and modify anthraquinones is presented. The basic regularity of an isolation process is analyzed. Action of temperature, pH, and polarity of extragent, catalysts and other factors on an isolation process is revealed.

Keywords: Anthraquinones, chromatography, extraction, phytopreparation, precipitation.

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Authors: Taruna Katyal Arora, Geeta Kumari, Hari Shankar, Neelima Mishra

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Substandard and counterfeit antimalarials is a major problem in malaria endemic areas. The availability of counterfeit/ substandard medicines is not only decreasing the efficacy in patients, but it is also one of the contributing factors for developing antimalarial drug resistance. Owing to this, a pilot study was conducted to survey quality of drugs collected from different malaria endemic areas of India. Artesunate+Sulphadoxine-Pyrimethamine (AS+SP), Artemether-Lumefantrine (AL), Chloroquine (CQ) tablets were randomly picked from public health facilities in selected states of India. The quality of antimalarial drugs from these areas was assessed by using Global Pharma Health Fund Minilab test kit. This includes physical/visual inspection and disintegration test. Thin-layer chromatography (TLC) was carried out for semi-quantitative assessment of active pharmaceutical ingredients. A total of 45 brands, out of which 21 were for CQ, 14 for AL and 10 for AS+SP were tested from Uttar Pradesh (U.P.), Mizoram, Meghalaya and Gujrat states. One out of 45 samples showed variable disintegration and retension factor. The variable disintegration and retention factor which would have been due to substandard quality or other factors including storage. However, HPLC analysis confirms standard active pharmaceutical ingredient, but may be due to humid temperature and moisture in storage may account for the observed result.

Keywords: Antimalarial medicines, counterfeit, substandard, thin layer chromatography.

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Authors: Patricia B. Cruz, Catrina Jean G. Valenzuela, Analyn N. Yumang

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Nearly a hundred per million of the Filipino population is diagnosed with Chronic Kidney Disease (CKD). The early stage of CKD has no symptoms and can only be discovered once the patient undergoes urinalysis. Over the years, different methods were discovered and used for the quantification of the urinary albumin such as the immunochemical assays where most of these methods require large machinery that has a high cost in maintenance and resources, and a dipstick test which is yet to be proven and is still debated as a reliable method in detecting early stages of microalbuminuria. This research study involves the use of the liquid chromatography concept in microfluidic instruments with biosensor as a means of separation and detection respectively, and linear regression to quantify human urinary albumin. The researchers’ main objective was to create a miniature system that quantifies and detect patients’ urinary albumin while reducing the amount of volume used per five test samples. For this study, 30 urine samples of unknown albumin concentrations were tested using VITROS Analyzer and the microfluidic system for comparison. Based on the data shared by both methods, the actual vs. predicted regression were able to create a positive linear relationship with an R² of 0.9995 and a linear equation of y = 1.09x + 0.07, indicating that the predicted values and actual values are approximately equal. Furthermore, the microfluidic instrument uses 75% less in total volume – sample and reagents combined, compared to the VITROS Analyzer per five test samples.

Keywords: Chronic kidney disease, microfluidics, linear regression, VITROS analyzer, urinary albumin.

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Authors: Marinos Xagoraris, Iliada K. Lappa, Charalambos Kanakis, Dimitra Daferera, Christina Papadopoulou, Georgios Sourounis, Charilaos Giotis, Pavlos Bouchagier, Christos S. Pappas, Petros A. Tarantilis, Efstathia Skotti

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The aim of this work was to recover phenolic compounds from grape skins produced in Greek varieties of the Ionian Islands in order to form the basis of calculations for their further utilization in the context of the circular economy. Isolation and further utilization of phenolic compounds is an important issue in winery by-products. For this purpose, 37 samples were collected, extracted, and analyzed in an attempt to provide the appropriate basis for their sustainable exploitation. Extraction of the bioactive compounds was held using an eco-friendly, non-toxic, and highly effective water-glycerol solvent system. Then, extracts were analyzed using UV-Vis, liquid chromatography-mass spectrometry (LC-MS), FTIR, and Raman spectroscopy. Also, total phenolic content and antioxidant activity were measured. LC-MS chromatography showed qualitative differences between different varieties. Peaks were attributed to monomeric 3-flavanols as well as monomeric, dimeric, and trimeric proanthocyanidins. The FT-IR and Raman spectra agreed with the chromatographic data and contributed to identifying phenolic compounds. Grape skins exhibited high total phenolic content (TPC), and it was proved that during vinification, a large number of polyphenols remained in the pomace. This study confirmed that grape skins from Ionian Islands are a promising source of bioactive compounds, suggesting their utilization under a bio-economic and environmental strategic framework.

Keywords: Antioxidant activity, grape skin, phenolic compounds, waste recovery.

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Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: Lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS.

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Authors: B. Y. Matmuratov, S. D. Madrakhimova. R. S. Esanov. A. D. Matchanov

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Supramolecular complexes of glycyrrhizic acid with kinetin in various molar ratios were obtained, physico-chemical parameters and spectral properties of the resulting complexes were studied (UV, IR, mass spectrometry.

Keywords: Monoammonium salt of glycyrrhizic acid, glycyrrhizic acid, supramolecular complex, isomolar series, IR spectroscopy.

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Authors: Gaurav Bhanjana, Ganga Ram Chaudhary, Sandeep Kumar, Neeraj Dilbaghi

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Main sources of endocrine disrupting compounds in the ecosystem are hormones, pesticides, phthalates, flame retardants, dioxins, personal-care products, coplanar polychlorinated biphenyls (PCBs), bisphenol A, and parabens. These endocrine disrupting compounds are responsible for learning disabilities, brain development problems, deformations of the body, cancer, reproductive abnormalities in females and decreased sperm count in human males. Although discharge of these chemical compounds into the environment cannot be stopped, yet their amount can be retarded through proper evaluation and detection techniques. The available techniques for determination of these endocrine disrupting compounds mainly include high performance liquid chromatography (HPLC), mass spectroscopy (MS) and gas chromatography-mass spectrometry (GC–MS). These techniques are accurate and reliable but have certain limitations like need of skilled personnel, time consuming, interference and requirement of pretreatment steps. Moreover, these techniques are laboratory bound and sample is required in large amount for analysis. In view of above facts, new methods for detection of endocrine disrupting compounds should be devised that promise high specificity, ultra sensitivity, cost effective, efficient and easy-to-operate procedure. Nowadays, electrochemical sensors/biosensors modified with nanomaterials are gaining high attention among researchers. Bioelement present in this system makes the developed sensors selective towards analyte of interest. Nanomaterials provide large surface area, high electron communication feature, enhanced catalytic activity and possibilities of chemical modifications. In most of the cases, nanomaterials also serve as an electron mediator or electrocatalyst for some analytes.

Keywords: Sensors, endocrine disruptors, nanoparticles, electrochemical, microscopy.

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Authors: Deepak K. Semwal, Ruchi B. Semwal, Aijaz Ahmad, Guy P. Kamatou, Alvaro M. Viljoen

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Kigelia africana (Lam.) Benth. (Bignoniaceae) is a reputed traditional remedy for various human ailments such as skin diseases, microbial infections, melanoma, stomach troubles, metabolic disorders, malaria and general pains. In spite of the fruit being widely used for purposes related to its antibacterial and antifungal properties, the chemical constituents associated with the activity have not been fully identified. To elucidate the active principles, we evaluated the antimicrobial activity of fruit extracts and purified fractions against Staphylococcus aureus, Enterococcus faecalis, Moraxella catarrhalis, Escherichia coli, Candida albicans and Candida tropicalis. Shade-dried fruits were powdered and extracted with hydroalcoholic (1:1) mixture by soaking at room temperature for 72 h. The crude extract was further fractionated by column chromatography, with successive elution using hexane, dichloromethane, ethyl acetate, acetone and methanol. The dichloromethane and ethyl acetate fractions were combined and subjected to column chromatography to furnish a wax and oil from the eluates of 20% and 40% ethyl acetate in hexane, respectively. The GC-MS and GC×GC-MS results revealed that linoleic acid, linolenic acid, palmitic acid, arachidic acid and stearic acid were the major constituents in both oil and wax. The crude hydroalcoholic extract exhibited the strongest activity with MICs of 0.125-0.5 mg/mL, followed by the ethyl acetate (MICs = 0.125-1.0 mg/mL), dichloromethane (MICs = 0.250-2.0 mg/mL), hexane (MICs = 0.25- 2.0 mg/mL), acetone (MICs = 0.5-2.0 mg/mL) and methanol (MICs = 1.0-2.0 mg/mL), whereas the wax (MICs = 2.0-4.0 mg/mL) and oil (MICs = 4.0-8.0 mg/mL) showed poor activity. The study concludes that synergistic interactions of chemical constituents could be responsible for the antimicrobial activity of K. africana fruits, which needs a more holistic approach to understand the mechanism of its antimicrobial activity.

Keywords: Kigelia Africana, traditional medicine, antimicrobial activity, Candida albicans, palmitic acid, synergistic interaction.

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Authors: M. P. Casiraghi, C. M. Quintella, P. Almeida

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Paraffinic oils were submitted to microbial action. The microorganisms consisted of bacteria of the genera Pseudomonas sp. and Bacillus lincheniforms. The alterations in interfacial tension were determined using a tensometer and applying the hanging drop technique at room temperature (299 K ±275 K). The alteration in the constitution of the paraffins was evaluated by means of gas chromatography. The microbial activity was observed to reduce interfacial tension by 54 to 78%, as well as consuming the paraffins C19 to C29 and producing paraffins C36 to C44. The LIFirr technique made it possible to determine the microbial action quickly.

Keywords: Paraffins, biosurfactants, LIFirr.

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Authors: A. Aljohani, M. Orif

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The concentration of polycyclic aromatic hydrocarbons (PAH) in clams (A. glabrata) was examined in samples collected from Alseef Beach, 30 km south of Jeddah city. Gas chromatography-mass spectrometry (GC-MS) was used to analyze the 14 PAHs. The concentration of total PAHs was found to range from 11.521 to 40.149 ng/gdw with a mean concentration of 21.857 ng/gdw, which is lower compared to similar studies. The lower molecular weight PAHs with three rings comprised 18.14% of the total PAH concentrations in the clams, while the high molecular weight PAHs with four rings, five rings, and six rings account for 81.86%. Diagnostic ratios for PAH source distinction suggested pyrogenic or anthropogenic sources.

Keywords: Bivalves, biomonitoring, hydrocarbons, PAHs.

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Authors: Anelise Leal Vieira Cubas, Marina de Medeiros Machado, Marília de Medeiros Machado

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The volatile organic compounds - BTEX (Benzene, Toluene, Ethylbenzene, and Xylene) petroleum derivatives, have high rates of toxicity, which may carry consequences for human health, biota and environment. In this directon, this paper proposes a method of treatment of these compounds by using corona discharge plasma technology. The efficiency of the method was tested by analyzing samples of BTEX after going through a plasma reactor by gas chromatography method. The results show that the optimal residence time of the sample in the reactor was 8 minutes.

Keywords: BTEX, Degradation, Cold plasma.

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Authors: Frantisek Bozek, Lenka Jesonkova, Jiri Dvorak

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Trihalogenmethanes are the most significant byproducts of the reaction of disinfection agent with organic precursors naturally present in ground and surface waters.Their incidence negatively affects the quality of drinking water in relation to their nephrotoxic, hepatotoxic and genotoxic effects on human health. Taking into consideration the considerable volatility of monitored contaminants it could be assumed that their incidence in drinking water would depend on the distance of sampling from the area of disinfection. Based on the concentration of trihalogenmethanes determined with the help of gas chromatography with mass detector and the analysis of variance (ANOVA) such dependence has been proved as statistically significant. The acquired outcomes will be used for assessing the non-carcinogenic and genotoxic risks to consumers.

Keywords: disinfection byproducts, drinking water, trihalogenmethanes

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Authors: A. M. Tarola, R. Preti, A. M. Girelli, P. Campana

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Safeguarding, studying and enhancing biodiversity play an important and indispensable role in re-launching agriculture. The ancient local varieties are therefore a precious resource for genetic and health improvement. In order to protect biodiversity through the recovery and valorization of autochthonous varieties, in this study we analyzed 12 samples of four ancient apple cultivars representative of Friuli Venezia Giulia, selected by local farmers who work on a project for the recovery of ancient apple cultivars. The aim of this study is to evaluate the polyphenolic profile and the antioxidant capacity that characterize the organoleptic and functional qualities of this fruit species, besides having beneficial properties for health. In particular, for each variety, the following compounds were analyzed, both in the skins and in the pulp: gallic acid, catechin, chlorogenic acid, epicatechin, caffeic acid, coumaric acid, ferulic acid, rutin, phlorizin, phloretin and quercetin to highlight any differences in the edible parts of the apple. The analysis of individual phenolic compounds was performed by High Performance Liquid Chromatography (HPLC) coupled with a diode array UV detector (DAD), the antioxidant capacity was estimated using an in vitro essay based on a Free Radical Scavenging Method and the total phenolic compounds was determined using the Folin-Ciocalteau method. From the results, it is evident that the catechins are the most present polyphenols, reaching a value of 140-200 μg/g in the pulp and of 400-500 μg/g in the skin, with the prevalence of epicatechin. Catechins and phlorizin, a dihydrohalcone typical of apples, are always contained in larger quantities in the peel. Total phenolic compounds content was positively correlated with antioxidant activity in apple pulp (r² = 0,850) and peel (r² = 0,820). Comparing the results, differences between the varieties analyzed and between the edible parts (pulp and peel) of the apple were highlighted. In particular, apple peel is richer in polyphenolic compounds than pulp and flavonols are exclusively present in the peel. In conclusion, polyphenols, being antioxidant substances, have confirmed the benefits of fruit in the diet, especially as a prevention and treatment for degenerative diseases. They demonstrated to be also a good marker for the characterization of different apple cultivars. The importance of protecting biodiversity in agriculture was also highlighted through the exploitation of native products and ancient varieties of apples now forgotten.

Keywords: Apple, biodiversity, polyphenols, antioxidant activity, HPLC-DAD, characterization.

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Authors: A. de Folly d’Auris, R. Bagatin, P. Filtri

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This paper discusses the importance of having a good initial characterization of soil samples when thermal desorption has to be applied to polluted soils for the removal of contaminants. Particular attention has to be devoted on the desorption kinetics of the samples to identify the gases evolved during the heating, and contaminant degradation pathways. In this study, two samples coming from different points of the same contaminated site were considered. The samples are much different from each other. Moreover, the presence of high initial quantity of heavy hydrocarbons strongly affected the performance of thermal desorption, resulting in formation of dangerous intermediates. Analytical techniques such TGA (Thermogravimetric Analysis), DSC (Differential Scanning Calorimetry) and GC-MS (Gas Chromatography-Mass) provided a good support to give correct indication for field application.

Keywords: Desorption kinetics, hydrocarbons, thermal desorption, thermogravimetric measurements.

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Authors: Pitcha Wongskeo, Pramoch Rangsunvigit, Sumaeth Chavadej

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The possibility of using cassava residue containing 49.66% starch, 21.47% cellulose, 12.97% hemicellulose, and 21.86% lignin as a raw material to produce glucose using enzymatic hydrolysis was investigated. In the experiment, each reactor contained the cassava residue, bacteria cells, and production medium. The effects of particles size (40 mesh and 60 mesh) and strains of bacteria (A002 and M015) isolated from Thai higher termites, Microcerotermes sp., on the glucose concentration at 37°C were focused. High performance liquid chromatography (HPLC) with a refractive index detector was used to determine the quantity of glucose. The maximum glucose concentration obtained at 37°C using strain A002 and 60 mesh of the cassava residue was 1.51 g/L at 10 h.

Keywords: Hydrolysis, termites, glucose, cassava

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Authors: Suboohi Shervani, Jingjing Ling, Jiabin Liu, Tahir Husain

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Offshore oil-spill has become the most emerging problem in the world. In the current paper, a graphene/ZnO/polymer nanocomposite thin film is coated on stainless steel mesh via layer by layer deposition method. The structural characterization of materials is determined by Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). The total petroleum hydrocarbons (TPHs) and separation efficiency have been measured via gas chromatography – flame ionization detector (GC-FID). TPHs are reduced to 2 ppm and separation efficiency of the nanocomposite coated mesh is reached ≥ 99% for the final sample. The nanocomposite coated mesh acts as a promising candidate for the separation of oil- water mixture.

Keywords: Oil-spill, graphene, oil-water separation, nanocomposite.

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Authors: I. F. Fiţigău, F. Peter, C. G. Boeriu

Abstract:

Five lignin samples were fractionated with Acetone/Water mixtures and the obtained fractions were subjected to extensive structural characterization, including Fourier Transform Infrared (FT-IR), Gel permeation Chromatography (GPC) and Phosphorus-31 NMR spectroscopy (31P-NMR). The results showed that for all studied lignins the solubility increases with the increment of the acetone concentration. Wheat straw lignin has the highest solubility in 90/10 (v/v) Acetone/Water mixture, 400 mg lignin being dissolved in 1 mL mixture. The weight average molecular weight of the obtained fractions increased with the increment of acetone concentration and thus with solubility. 31P-NMR analysis based on lignin modification by reactive phospholane into phosphitylated compounds was used to differentiate and quantify the different types of OH groups (aromatic, aliphatic, and carboxylic) found in the fractions obtained with 70/30 (v/v) Acetone/Water mixture.

Keywords: Lignin, fractionation, FT-IR, GPC, 31P-NMR.

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Authors: Congmin Z. Xie, Terry Healy, Peter Robinson, Kevin Stewart

Abstract:

An HPLC-UV analytical method was developed to determine ethylenediaminetetraacetic acid (EDTA) in dairy wastewater and surface water. The optimizing separation was achieved by reversed–phase ion-pair liquid chromatography on a C18 column using methanol as mobile phase solvent, tetrabutylammonium bromide as the ion-pair reagent in pH 3.3 formate buffer solution at a flow rate of 0.9 mL min-1 with a UV detector at 265 nm. No interference of Ca, Mg or NO3 - was detected. Method performance was evaluated in terms of linearity, repeatability and reproducibility. The method detection limit was 5 μg L-1. The contents of EDTA in dairy effluents were 72 ~ 261 μg L-1 at a large dairy site. A change of EDTA concentration was observed downstream of the dairy effluent discharge, but this was well under the predicted no effect concentration for aquatic ecosystem.

Keywords: Dairy wastewater, EDTA, HPLC, surface water.

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Authors: Y. L. Yung, Kong Mun Lo

Abstract:

In this study, solid phase micro-extraction (SPME) was optimized to improve the sensitivity and accuracy in formaldehyde determination for plywood panels. Further work has been carried out to compare the newly developed technique with existing method which reacts formaldehyde collected in desiccators with acetyl acetone reagent (DC-AA). In SPME, formaldehyde was first derivatized with O-(2,3,4,5,6 pentafluorobenzyl)-hydroxylamine hydrochloride (PFBHA) and analysis was then performed by gas chromatography in combination with mass spectrometry (GC-MS). SPME data subjected to various wood species gave satisfactory results, with relative standard deviations (RSDs) obtained in the range of 3.1-10.3%. It was also well correlated with DC values, giving a correlation coefficient, RSQ, of 0.959. The quantitative analysis of formaldehyde by SPME was an alternative in wood industry with great potential

Keywords: Formaldehyde, GCMS, Plywood and SPME

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Authors: Mustafa Erat

Abstract:

Glutathione S-transferase was purified from human erythrocytes and effects of some polyphenols were investigated on the enzyme activity. The purification procedure was performed on Glutathione-Agarose affinity chromatography after preparation of erythrocytes hemolysate with a yield of 81%. The purified enzyme showed a single band on the SDS-PAGE. The effects of some poliphenolic compounds such as catechin, dopa, dopamine, progallol and catechol were examined on the in vitro GST activity. Catechin was determined to be inhibitor for the enzyme, but others were not effective on the enzyme as inhibitors or activators. IC50 value -the concentration of inhibitor which reduces enzyme activity by 50%- was estimated to be 10 mM. Ki constants were also calculated as 6.38 ± 0,70 mM with GSH substrate, and 3.86 ± 0,78 mM with CDNB substrate using the equations of graphs for the inhibitor, and its inhibition type was determined as non-competitive.

Keywords: Drug resistance, Glutathione S-transferase, Inhibition.

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Authors: C. Nobre, C. C. Castro, A.-L. Hantson, J. A. Teixeira, L. R. Rodrigues, G. De Weireld

Abstract:

Fructo-oligosaccharides (FOS) are produced from sucrose by Aureobasidium pullulans in yields between 40-60% (w/w). To increase the amount of FOS it is necessary to remove the small, non-prebiotic sugars, present. Two methods for producing high-purity FOS have been developed: the use of microorganisms able to consume small saccharides; and the use of continuous chromatography to separate sugars: simulated moving bed (SMB). It is herein proposed the combination of both methods. The aim of this study is to optimize the composition of the fermentative broth (in terms of salts and sugars) that will be further purified by SMB. A yield of 0.63 gFOS.gSucrose^-1 was obtained with A. pullulans using low amounts of salts in the initial fermentative broth. By removing the small sugars, Saccharomyces cerevisiae and Zymomonas mobilis increased the percentage of FOS from around 56.0% to 83% (w/w) in average, losing only 10% (w/w) of FOS during the recovery process.

Keywords: Fructo-oligosaccharides, microbial treatment, Saccharomyces cerevisiae, Zymomonas mobilis.

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Authors: Jhalique Jane R. Fojas, Rizalinda L. De Leon, Lucille V. Abad

Abstract:

The characterization of κ-carrageenan could provide a better understanding of its functions in biological, medical and industrial applications. Chemical and physical analyses of carrageenan from seaweeds, Euchema cottonii L., were done to offer information on its properties and the effects of Co-60 γ-irradiation on its thermochemical characteristics. The structural and morphological characteristics of κ-carrageenan were determined using scanning electron microscopy (SEM) while the composition, molecular weight and thermal properties were determined using attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), gel permeation chromatography (GPC), thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). Further chemical analysis was done using hydrogen-1 nuclear magnetic resonance (1H NMR) and functional characteristics in terms of biocompatibility were evaluated using cytotoxicity test.

Keywords: Biocompatibility, carrageenan, DSC, FTIR, GPC, irradiation, NMR, physicochemical, SEM, TGA.

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