Search results for: inductively coupled mass spectrometry

Authors: El Kolli Meriem, Laouer Hocine, Sahli Farida, Akkal Salah, El Kolli Hayet

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The aerial parts of Daucus gracilis (Apiaceae) were subjected to hydrodistillation by a Clevenger apparatus to obtain the essential oil (EO) which has been analyzed by Gas Chromatography (GC) and GC coupled with mass spectrometry. The antioxidant properties of this EO and D. gracilis methanolic extract were studied by both of the free diphenyl-1-picrylhydrazyl (DPPH) radical scavenging and the reducing power techniques. The dominant constituents of the EO were the elemicin (35.3 %) and the geranyl acetate (26.8 %). Both of EO and methanolic extract showed important antioxidant properties with respectively IC50 of 0,002 mg/ml and 0.06 mg/ml. They showed also a reducing power dose-dependent.

Keywords: daucus gracilis, apiaceae, essential oil, antioxidant activity

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Authors: Illyas Md Isa, Mohamad Idris Saidin, Mustaffa Ahmad, Norhayati Hashim

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A highly selective and sensitive carbon paste electrode modified with multiwall carbon nanotubes and 2,6–diacetylpyridine-di-(1R)–(-)–fenchone diazine tetracarbonylmolybdenum(0) complex was used for determination of trace amounts of Cu(II) using square wave anodic stripping voltammetry (SWASV). The influences of experimental variables on the proposed electrode such as pH, supporting electrolyte, preconcentration potential and time, and square wave parameters were investigated. Under optimal conditions, the proposed electrode showed a linear relationship with concentration in the range of 1.0 × 10–10 to 1.0 × 10– 6 M Cu(II) with a limit of detection 8.0 × 10–11 M. The relative standard deviation (n = 5) for a solution containing 1.0 × 10– 6 M of Cu(II) was 0.036. The presence of various cations (in 10 and 100-folds concentration) did not interfere. Electrochemical impedance spectroscopy (EIS) showed that the charge transfer at the electrode-solution interface was favourable. The proposed electrode was applied for the determination of Cu(II) in several water samples. Results agreed very well with those obtained by inductively coupled plasma-optical emission spectrometry. The modified electrode was then proposed as an alternative for determination of Cu(II).

Keywords: chemically modified electrode, Cu(II), square wave anodic stripping voltammetry, tetracarbonylmolybdenum(0)

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Authors: Fangyan Li, Lin Min Lee, Hui Zhu Peh, Shoet Harn Chan

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Advantame, a derivative of aspartame, is the latest addition to a family of low caloric and high potent dipeptide sweeteners which include aspartame, neotame and alitame. The use of advantame as a high-intensity sweetener in food was first accepted by Food Standards Australia New Zealand in 2011 and subsequently by US and EU food authorities in 2014, with the results from toxicity and exposure studies showing advantame poses no safety concern to the public at regulated levels. To our knowledge, currently there is barely any detailed information on the analytical method of advantame in food matrix, except for one report published in Japanese, stating a high performance liquid chromatography (HPLC) and liquid chromatography/ mass spectrometry (LC-MS) method with a detection limit at ppm level. However, the use of acid in sample preparation and instrumental analysis in the report raised doubt over the reliability of the method, as there is indication that stability of advantame is compromised under acidic conditions. Besides, the method may not be suitable for analyzing food matrices containing advantame at low ppm or sub-ppm level. In this presentation, a simple, specific and sensitive method for the determination of advantame in food is described. The method involved extraction with water and clean-up via solid phase extraction (SPE) followed by detection using liquid chromatography tandem mass spectrometry (LC-MS/MS) in negative electrospray ionization mode. No acid was used in the entire procedure. Single laboratory validation of the method was performed in terms of linearity, precision and accuracy. A low detection limit at ppb level was achieved. Satisfactory recoveries were obtained using spiked samples at three different concentration levels. This validated method could be used in the routine inspection of the advantame level in food.

Keywords: advantame, food, LC-MS/MS, sweetener

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Authors: R. Mickiene, A. Friese, U. Rosler, A. Maruska, O. Ragazinskiene

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This research focuses on phytochemistry and antimicrobial activities of compounds isolated and identified from three species of Eryngium. The antimicrobial activity of extracts from Eryngiumplanum L., Eryngium maritimum L., Eryngium campestre L. grown in Lithuania, were tested by the method of series dilutions, against different bacteria species: Escherichia coli, Proteus vulgaris and Staphylococcus aureus with and without antibiotic resistances, originating from livestock. The antimicrobial activity of extracts was described by determination of the minimal inhibitory concentration. Preliminary results show that the minimal inhibitory concentration range between 8.0 % and 17.0 % for the different Eryngium extracts and bacterial species.The total amounts ofphenolic compounds and total amounts of flavonoids were tested in the methanolic extracts of the plants. Identification and evaluation of the phenolic compounds were performed by liquid chromatography. The essential oils were analyzed by gas chromatography mass spectrometry.

Keywords: antimicrobial activities, Eryngium L. species, essential oils, gas chromatography mass spectrometry

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

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

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

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Authors: Yehya Elsayed, Sarah Dalibalta, Fareedah Alqtaishat, Ioline Gomes, Nagelle Fernandes

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Bakhour or Arabian incense is traditionally used to perfume houses, shops and clothing as part of cultural or religious practices in several Middle Eastern countries. Conventionally, Bakhour consists of a mixture of natural ingredients such as chips of agarwood (oud), musk and sandalwoods that are soaked in scented oil. Bakhour is usually burned by charcoal or by using gas or electric burners to produce the scented smoke. It is necessary to evaluate the impact of such practice on human health and environment especially that the burning of Bakhour is usually done on a regular basis and in closed areas without proper ventilation. Although significant amount of research has been reported in scientific literature on the chemical analysis of various types of incense smoke, unfortunately only very few of them focused specifically on the health impacts of Bakhour. Raw Bakhour samples, their smoke emissions and the ash residue were analyzed to assess the existence of toxic ingredients and their possible influence on health and the environment. Three brands of Bakhour samples were analyzed for the presence of harmful heavy metals and organic compounds. Thermal Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to identify organic compounds while Inductively Coupled Plasma (ICP) and Scanning Electron Microscope-Energy Dispersive X-Ray Spectrometer (SEM-EDS) were used to analyze the presence of toxic and heavy metals. Organic compounds from the smoke were collected on specific tenax and activated carbon adsorption tubes. More than 850 chemical compounds were identified. The presence of 19 carcinogens, 23 toxins and 173 irritants were confirmed. Additionally, heavy metals were detected in amounts similar to those present in cigarettes. However, it was noticed that many of the detected compounds in the smoke lacked clinical studies on their health effects which shows the need for further clinical studies to be devoted to this area of study.

Keywords: Bakhour, incense smoke, pollution, indoor environment, health risk, chemical analysis

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Authors: Yehya Elsayed, Sarah Dalibalta, Fareedah Alqtaishat, Ioline Gomes, Nagelle Fernandes

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Bakhour, or Arabian incense, is traditionally used to perfume houses, shops and clothing as part of cultural or religious practices in several Middle Eastern countries. Conventionally, Bakhour consists of a mixture of natural ingredients such as chips of agarwood (oud), musk and sandalwoods that are soaked in scented oil. Bakhour is usually burned by charcoal or by using gas or electric burners to produce the scented smoke. It is necessary to evaluate the impact of such practice on human health and environment especially that the burning of Bakhour is usually done on a regular basis and in closed areas without proper ventilation. Although significant amount of research has been reported in scientific literature on the chemical analysis of various types of incense smoke, unfortunately, only very few of them focused specifically on the health impacts of Bakhour. Raw Bakhour samples, their smoke emissions and the ash residue were analyzed to assess the existence of toxic ingredients and their possible influence on health and the environment. Three brands of Bakhour samples were analyzed for the presence of harmful heavy metals and organic compounds. Thermal Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to identify organic compounds while Inductively Coupled Plasma (ICP) and Scanning Electron Microscope-Energy Dispersive X-Ray Spectrometer (SEM-EDS) were used to analyze the presence of toxic and heavy metals.. Organic compounds from the smoke were collected on specific tenax and activated carbon adsorption tubes. More than 850 chemical compounds were identified. The presence of 19 carcinogens, 23 toxins, and 173 irritants were confirmed. Additionally, heavy metals were detected in amounts similar to those present in cigarettes. However, it was noticed that many of the detected compounds in the smoke lacked clinical studies on their health effects which shows the need for further clinical studies to be devoted to this area of study.

Keywords: bakhour, incense smoke, pollution, indoor environment, health risk, chemical analysis

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Authors: Louise H. Gracioso, Marcela P.G. Baltazar, Ingrid R. Avanzi, Bruno Karolski, Luciana J. Gimenes, Claudio O. Nascimento, Elen A. Perpetuo

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Introduction: Higher copper concentrations promote a selection pressure on organisms such as plants, fungi and bacteria, which allows surviving only the resistant organisms to the contaminated site. This selective pressure keeps only the organisms most resistant to a specific condition and subsequently increases their bioremediation potential. Despite the bacteria importance for biosphere maintenance, it is estimated that only a small fraction living microbial species has been described and characterized. Due to the molecular biology development, tools based on analysis 16S ribosomal RNA or another specific gene are making a new scenario for the characterization studies and identification of microorganisms in the environment. News identification of microorganisms methods have also emerged like Biotyper (MALDI / TOF), this method mass spectrometry is subject to the recognition of spectroscopic patterns of conserved and features proteins for different microbial species. In view of this, this study aimed to isolate bacteria resistant to copper present in a Copper Processing Area (Sossego Mine, Canaan, PA) and identifies them in two different methods: Recent (spectrometry mass) and conventional. This work aimed to use them for a future bioremediation of this Mining. Material and Methods: Samples were collected at fifteen different sites of five periods of times. Microorganisms were isolated from mining wastes by culture enrichment technique; this procedure was repeated 4 times. The isolates were inoculated into MJS medium containing different concentrations of chloride copper (1mM, 2.5mM, 5mM, 7.5mM and 10 mM) and incubated in plates for 72 h at 28 ºC. These isolates were subjected to mass spectrometry identification methods (Biotyper – MALDI/TOF) and 16S gene sequencing. Results: A total of 105 strains were isolated in this area, bacterial identification by mass spectrometry method (MALDI/TOF) achieved 74% agreement with the conventional identification method (16S), 31% have been unsuccessful in MALDI-TOF and 2% did not obtain identification sequence the 16S. These results show that Biotyper can be a very useful tool in the identification of bacteria isolated from environmental samples, since it has a better value for money (cheap and simple sample preparation and MALDI plates are reusable). Furthermore, this technique is more rentable because it saves time and has a high performance (the mass spectra are compared to the database and it takes less than 2 minutes per sample).

Keywords: copper mining area, bioremediation, microorganisms, identification, MALDI/TOF, RNA 16S

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Authors: Lowanika Victor Tibane, David Mamba

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Human body, animals, and plants depend on certain essential metals in permissible quantities for their survival. Excessive metal concentration may cause severe malfunctioning of the organisms and even fatal in extreme cases. Because of gold mining in the Witwatersrand basin in South Africa, enormous untreated mine dumps comprise elevated concentration of essential trace elements. Elevated quantities of trace metal have direct negative impact on the quality of soil for different land use types, reduce soil efficiency for plant growth, and affect the health human and animals. A total of 21 subsoil samples were examined using inductively coupled plasma optical emission spectrometry and X-ray fluorescence methods and the results elevated men concentration of Fe (36,433.39) > S (5,071.83) > Cu (1,717,28) > Mn (612.81) > Cr (74.52) > Zn (68.67) > Ni (40.44) > Co (9.63) > P (3.49) > Mo > (2.74), reported in mg/kg. Using various contamination indices, it was discovered that the sites surveyed are on average moderately contaminated with Co, Cr, Cu, Mn, Ni, S, and Zn. The ecological risk assessment revealed a low ecological risk for Cr, Ni and Zn, whereas Cu poses a very high ecological risk.

Keywords: essential trace elements, soil contamination, contamination indices, toxicity, descriptive statistics, ecological risk evaluation

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Authors: M. S. M. Yusof, R. Ramli, S. K. C. Soh, N. Ismail, N. Ngah

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This study presents the synthesis of a series of methoxybenzoylthiourea amino acid derivatives. The compounds were obtained from the reactions between 2/3/4-methoxybenzoyl isothiocyanate with threonine. All of the compounds were characterized via mass spectrometry, ¹H and ¹³C NMR spectrometry, UV-Vis spectrophotometer and FT-IR spectroscopy. Mass spectra for all of the compounds showed the presence of molecular ion [M]⁺ peaks at m/z 312, which are in agreement to the calculated molecular weight. For ¹H NMR spectra, the presence of OCH₃, C=S-NH and C=O-NH protons were observed within range of δ_H 3.8-4.0 ppm, 11.1-11.5 ppm and 10.0-11.5 ppm, respectively. ¹³C NMR spectra in all compounds displayed the presence of OCH₃, C=O-NH, C=O-OH and C=S carbon resonances within range of δ_C 55.0-57.0 ppm, 165.0-168.0 ppm, 170.0-171.0 ppm and 180.0-182.0 ppm, respectively. In UV spectra, two absorption bands have been observed and both were assigned to the n-π* and π-π* transitions. Six vibrational modes of v(N-H), v(O-H), v(C=O-OH), v(C=O-NH), v(C=C) aromatic and v(C=S) appeared in the FT-IR spectra within the range of 3241-3467 cm^-1, 2976-3302 cm^-1, 1720-1768 cm^-1, 1655-1672 cm^-1, 1519-1525 cm^-1 and 754-763 cm^-1, respectively. The antibacterial activity for all of the compounds was screened against Staphylococcus aureus, Staphylococcus epidermidis, Salmonella typhimurium and Escherichia coli. However, no activity was observed.

Keywords: methoxybenzoyl isothiocyanate, amino acid, threonine, antibacterial

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Authors: Kanlaya Kong-Ngern, Chutima Homwonk, Sittiruk Roytrakul

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In this research, we compared the proteomic profile of two rice leaf sheaths under salt stress, Thai moderately salt tolerant rice (Leaung Anan), and high salt tolerant rice (Pokkali). Seeds were grown in hydroponic culture for 21 days before NaCl was introduced initially at the level of 12 dS m⁻¹ for 10 days. Then the leaf sheath proteomes were analyzed by 1D-SDS-PAGE and NanoLC-MS/MS. In this study, 873 proteins were detected. Among these proteins, 219 proteins were known proteins and the other proteins were unnamed and unknown proteins. By using Mev software, we found that only 31 proteins in treated plants of both rice cultivars significantly expressed, 21 proteins were up-regulated and 10 proteins were down-regulated. Interestingly, the intensity of the 3 proteins in the Leaung Anan more expressed than in the Pokkali. The results indicate that the up-regulated proteins were more expressed in less tolerant rice may play an important role in helping rice to survive under salt stress.

Keywords: mass spectrometry, proteomics, rice leaf sheaths, salt stress

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Authors: Yanghui Xu, Qin Ou, Xintu Wang, Feng Hou, Peng Li, Jan Peter van der Hoek, Gang Liu

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The level and removal of microplastics (MPs) in wastewater treatment plants (WWTPs) has been well evaluated by the particle number, while the mass concentration of MPs and especially nanoplastics (NPs) remains unclear. In this study, microfiltration, ultrafiltration and hydrogen peroxide digestion were used to extract MPs and NPs with different size ranges (0.01−1, 1−50, and 50−1000 μm) across the whole treatment schemes in two WWTPs. By identifying specific pyrolysis products, pyrolysis gas chromatography−mass spectrometry were used to quantify their mass concentrations of selected six types of polymers (i.e., polymethyl methacrylate (PMMA), polypropylene (PP), polystyrene (PS), polyethylene (PE), polyethylene terephthalate (PET), and polyamide (PA)). The mass concentrations of total MPs and NPs decreased from 26.23 and 11.28 μg/L in the influent to 1.75 and 0.71 μg/L in the effluent, with removal rates of 93.3 and 93.7% in plants A and B, respectively. Among them, PP, PET and PE were the dominant polymer types in wastewater, while PMMA, PS and PA only accounted for a small part. The mass concentrations of NPs (0.01−1 μm) were much lower than those of MPs (>1 μm), accounting for 12.0−17.9 and 5.6− 19.5% of the total MPs and NPs, respectively. Notably, the removal efficiency differed with the polymer type and size range. The low-density MPs (e.g., PP and PE) had lower removal efficiency than high-density PET in both plants. Since particles with smaller size could pass the tertiary sand filter or membrane filter more easily, the removal efficiency of NPs was lower than that of MPs with larger particle size. Based on annual wastewater effluent discharge, it is estimated that about 0.321 and 0.052 tons of MPs and NPs were released into the river each year. Overall, this study investigated the mass concentration of MPs and NPs with a wide size range of 0.01−1000 μm in wastewater, which provided valuable information regarding the pollution level and distribution characteristics of MPs, especially NPs, in WWTPs. However, there are limitations and uncertainties in the current study, especially regarding the sample collection and MP/NP detection. The used plastic items (e.g., sampling buckets, ultrafiltration membranes, centrifugal tubes, and pipette tips) may introduce potential contamination. Additionally, the proposed method caused loss of MPs, especially NPs, which can lead to underestimation of MPs/NPs. Further studies are recommended to address these challenges about MPs/NPs in wastewater.

Keywords: microplastics, nanoplastics, mass concentration, WWTPs, Py-GC/MS

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Authors: Aubrey Langeland, Richard Neitzel, Kowit Nambunmee

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Electronic waste, ‘e-waste’, refers generally to discarded electronics and electrical equipment, including products from cell phones and laptops to wires, batteries and appliances. While e-waste represents a transformative source of income in low- and middle-income countries, informal e-waste workers use rudimentary methods to recover materials, simultaneously releasing harmful chemicals into the environment and creating a health hazard for themselves and surrounding communities. Valuable materials such as precious metals, copper, aluminum, ferrous metals, plastic and components are recycled from e-waste. However, persistent organic pollutants such as polychlorinated biphenyls (PCBs) and some polybrominated diphenyl ethers (PBDEs), and heavy metals are toxicants contained within e-waste and are of great concern to human and environmental health. The current study seeks to evaluate the environmental contamination resulting from informal e-waste recycling in a predominantly agricultural community in northeastern Thailand. To accomplish this objective, five types of environmental samples were collected and analyzed for concentrations of eight metals commonly associated with e-waste recycling during the period of July 2016 through July 2017. Rice samples from the community were collected after harvest and analyzed using inductively coupled plasma mass spectrometry (ICP-MS) and gas furnace atomic spectroscopy (GF-AS). Soil samples were collected and analyzed using methods similar to those used in analyzing the rice samples. Surface water samples were collected and analyzed using absorption colorimetry for three heavy metals. Environmental air samples were collected using a sampling pump and matched-weight PVC filters, then analyzed using Inductively Coupled Argon Plasma-Atomic Emission Spectroscopy (ICAP-AES). Finally, surface wipe samples were collected from surfaces in homes where e-waste recycling activities occur and were analyzed using ICAP-AES. Preliminary1 results indicate that some rice samples have concentrations of lead and cadmium significantly higher than limits set by the United States Department of Agriculture (USDA) and the World Health Organization (WHO). Similarly, some soil samples show levels of copper, lead and cadmium more than twice the maximum permissible level set by the USDA and WHO, and significantly higher than other areas of Thailand. Surface water samples indicate that areas near e-waste recycling activities, particularly the burning of e-waste products, result in increased levels of cadmium, lead and copper in surface waters. This is of particular concern given that many of the surface waters tested are used in irrigation of crops. Surface wipe samples measured concentrations of metals commonly associated with e-waste, suggesting a danger of ingestion of metals during cooking and other activities. Of particular concern is the relevance of surface contamination of metals to child health. Finally, air sampling showed that the burning of e-waste presents a serious health hazard to workers and the environment through inhalation and deposition2. Our research suggests a need for improved methods of e-waste recycling that allows workers to continue this valuable revenue stream in a sustainable fashion that protects both human and environmental health. 1Statistical analysis to be finished in October 2017 due to follow-up field studies occurring in July and August 2017. 2Still awaiting complete analytic results.

Keywords: e-waste, environmental contamination, informal recycling, metals

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Authors: J. Chandrasekhar Rao, B. G. Naidu, G. J. Naga Raju, P. Sarita

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Particle Induced X-ray Emission (PIXE) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) techniques have been employed in this work to determine the elements present in the root of Cyperus rotundus medicinal plant used in the treatment of rheumatoid arthritis. The elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, and Sr were commonly identified and quantified by both PIXE and ICP-MS whereas the elements Li, Be, Al, As, Se, Ag, Cd, Ba, Tl, Pb and U were determined by ICP-MS and Cl, K, Ca, Ti and Br were determined by PIXE. The regional variation of elemental content has also been studied by analyzing the same plant collected from different geographical locations. Information on the elemental content of the medicinal plant would be helpful in correlating its ability in the treatment of rheumatoid arthritis and also in deciding the dosage of this herbal medicine from the metal toxicity point of view. Principal component analysis and cluster analysis were also applied to the data matrix to understand the correlation among the elements.

Keywords: PIXE, CP-MS, elements, Cyperus rotundus, rheumatoid arthritis

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Authors: A. Md. Bayejid Hosen, B. M Zakir Hossain Howlader, C. Yearul Kabir

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Contamination of soil and agricultural products by heavy metals resulting from rapid industrial development has caused major concern. Dietary exposure to heavy metals has been associated with toxic and adverse health effects. The main threats to human health from heavy metals are associated with exposure to Pb, Cd and Hg. The aim of this study was to monitor the presence of heavy metals in cereals collected from different wholesale markets of Dhaka City. One hundred and sixty cereal samples were collected and analyzed for determination of heavy metals. Heavy metals were analyzed by inductively coupled plasma mass spectrometry (ICP-MS). A total of six heavy metals– lead, chromium, cadmium, mercury, arsenic and antimony were estimated. The average concentrations of heavy metals in cereals fall within the safe limit established by regulatory organizations except for Pb (152.4 μg/100g) and Hg (15.13 μg/100g) which exceeded the safe limits. BARI gom-26 was the highest source of Pb (304.1 μg/100g) whereas Haski-29 rice variety contained the highest amount of Hg (60.85 μg/100g). Though all the cereal varieties contained approximately same amount of Cr the naizer sail varieties contained huge amount of Cr (171.8 μg/100g). Among all the cereal samples miniket rice varieties contained the least amount of heavy metals. The concentration of Cr (63.24 μg/100g), Cd (5.54 μg/100g) and As (3.26 μg/100g) in all cereals were below the safe limits. The daily intake of heavy metals was determined using the total weight of cereals consumed each day multiplied by the concentrations of heavy metals in cereals. The daily intake was compared with provisional maximum tolerable daily intake set by different regulatory organizations. The daily intake of Cd (23.0 μg), Hg (63.0 μg) and as (13.6 μg) through cereals were below the risk level except for Pb (634.0 μg) and Cr (263.1 μg). As the main meal of average Bangladeshi people is boiled rice served with some sorts of vegetables, our findings indicate that the residents of Dhaka City are at risk from Pb and Cr contamination. Potential health risks from exposure to heavy metals in self-planted cereals need more attention.

Keywords: contamination, dietary exposure, heavy metals, human health, ICP-MS

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Authors: Till Fehlauer, Blanche Collin, Bernard Angeletti, Andrea Somogyi, Claire Lallemand, Perrine Chaurand, Cédric Dentant, Clement Levard, Jerome Rose

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Over the last decades, yttrium (Y) has gained importance in high-tech applications. It is an essential part of alloys and compounds used for lasers, displays, or cell phones, for example. Due to its chemical similarities with the lanthanides, Y is often considered a rare earth element (REE). Despite their increased usage, the environmental behavior of REEs remains poorly understood. Especially regarding their interactions with plants, many uncertainties exist. On the one hand, Y is known to have a negative effect on root development and germination, but on the other hand, it appears to promote plant growth at low concentrations. In order to understand these phenomena, a precise knowledge is necessary about how Y is absorbed by the plant and how it is handled once inside the organism. Contradictory studies exist, stating that due to a similar ionic radius, Y and the other REEs might be absorbed through Ca²⁺-channels, while others suspect that Y has a shared pathway with Al³⁺. In this study, laser ablation coupled ICP-MS, and synchrotron-based micro-X-ray fluorescence (µXRF, beamline Nanoscopium, SOLEIL, France) have been used in order to localize Y within the plant tissue and identify associated elements. The plant used in this study is Saxifraga paniculata, a rugged alpine plant that has shown an affinity for Y in previous studies (in prep.). Furthermore, Saxifraga paniculata performs guttation, which means that it possesses phloem sap secreting openings on the leaf surface that serve to regulate root pressure. These so-called hydathodes could provide special insights in elemental transport in plants. The plants have been grown on Y doped soil (500mg/kg DW) for four months. The results showed that Y was mainly concentrated in the roots of Saxifraga paniculata (260 ± 85mg/kg), and only a small amount was translocated to the leaves (10 ± 7.8mg/kg). µXRF analysis indicated that within the root transects, the majority of Y remained in the epidermis and hardly penetrated the stele. Laser ablation coupled ICP-MS confirmed this finding and showed a positive correlation in the roots between Y, Fe, Al, and to a lesser extent Ca. In the stem transect, Y was mainly detected in a hotspot of approximately 40µm in diameter situated in the endodermis area. Within the stem and especially in the hotspot, Y was highly colocalized with Al and Fe. Similar-sized Y hotspots have been detected in/on the leaves. All of them were strongly colocalized with Al and Fe, except for those situated within the hydathodes, which showed no colocalization with any of the measured elements. Accordingly, a relation between Y and Ca during root uptake remains possible, whereas a correlation to Fe and Al appears to be dominant in the aerial parts, suggesting common storage compartments, the formation of complexes, or a shared pathway during translocation.

Keywords: laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), Phytoaccumulation, Rare earth elements, Saxifraga paniculata, Synchrotron-based micro-X-ray fluorescence, Yttrium

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Authors: Louise Jones, Rafael De Andrade Moral, John C. Stephens

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Background: Minerals are an essential component of correct nutrition. Conserved hay/haylage is an important component of many horse's diets. Variations in the mineral content of conserved forage should be considered when assessing dietary intake. Objectives: This study describes the levels and differences in 15 commonly analysed minerals in conserved forage fed to horses in the United Kingdom (UK), Ireland (IRL), and France (FRA). Methods: Hay (FRA n=92, IRL n=168, UK n=152) and haylage samples (UK n=287, IRL n=49) were collected during 2017-2020. Mineral analysis was undertaken using inductively coupled plasma-mass spectrometry (ICP-MS). Statistical analysis was performed using beta regression, Gaussian, or gamma models, depending on the nature of the response variable. Results: There are significant differences in the mineral content of the UK, IRL, and FRA conserved forage samples. FRA hay samples had a significantly higher (p < 0.05) levels of Sulphur (0.16 ± 0.0051 %), Calcium (0.56 ± 0.0342%), Magnesium (0.16 ± 0.0069 mg/ kg DM), Iron (194 ± 23.0 mg/kg DM), Cobalt (0.21 ± 0.0244 mg/kg DM) and Copper (4.94 ± 0.196 mg/kg DM) content compared to hay from the other two countries. UK hay samples had significantly less (p < 0.05) Selenium (0.07 ± 0.0084 mg/kg DM), whilst IRL hay samples were significantly (p < 0.05) higher in Chloride (0.9 ± 0.026mg/kg DM) compared to hay from the other two countries. IRL haylage samples were significantly (p < 0.05) higher in Phosphorus (0.26 ± 0.0102 %), Sulphur (0.17 ± 0.0052 %), Chloride (1.01 ± 0.0519 %), Calcium (0.54 ± 0.0257 %), Selenium (0.17 ± 0.0322 mg/kg DM) and Molybdenum (1.47 ± 0.137 mg/kg DM) compared to haylage from the UK. Main Limitations: Forage samples were obtained from professional yards and may not be reflective of forages fed by most horse owners. Information regarding soil type, species of grass, fertiliser treatment, harvest, or storage conditions were not included in this study. Conclusions: At a DM intake of 2% body weight, conserved forage as sampled in this study will be insufficient to meet Zinc, Iodine, and Copper NRC maintenance requirements, and Se intake will also be insufficient for horses fed the UK conserved forage. Many horses receive hay/haylage as the main component of their diet; this study highlights the need to consider forage analysis when making dietary recommendations.

Keywords: conserved forage, hay, haylage, minerals

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Authors: Bakhtishod Matmuratov, Sakhiba Madraximova, Rakhmat Esanov, Alimjan Matchanov

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Studies have been performed to obtain complexes of glycyrrhizic acid and kinetins in a 2:1 ratio. The complex of glycyrrhizic acid and kinetins in a 2:1 ratio was considered evidence of the formation of a molecular complex by determining the molecular masses using chromato-mass spectroscopy and analyzing the IR spectra.

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

Procedia PDF Downloads 141

Authors: W. Walke, J. Przondziono, K. Nowińska

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The study comprises evaluation of suitability of passive layer created on the surface of AISI 316L stainless steel for products that are intended to have contact with blood. For that purpose, prior to and after chemical passivation, samples were subject to 7 day exposure in artificial plasma at the temperature of T=37°C. Next, tests of metallic ions infiltration from the surface to the solution were performed. The tests were performed with application of spectrometer JY 2000, by Yobin – Yvon, employing Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). In order to characterize physical and chemical features of electrochemical processes taking place during exposure of samples to artificial plasma, tests with application of electrochemical impedance spectroscopy were suggested. The tests were performed with application of measuring unit equipped with potentiostat PGSTAT 302n with an attachment for impedance tests FRA2. Measurements were made in the environment simulating human blood at the temperature of T=37°C. Performed tests proved that application of chemical passivation process for AISI 316L stainless steel used for production of goods intended to have contact with blood is well-grounded and useful in order to improve safety of their usage.

Keywords: AISI 316L stainless steel, chemical passivation, artificial plasma, ions infiltration, EIS

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Authors: Rafid Doulab

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Elemental Impurities in the Pharmaceuticals industryis are indispensable to ensure pharmaceuticalssafety for 24 elements. Although atomic absorption and inductively coupled plasma are used in the U.S Pharmacopeia and the European Pharmacopoeia, FESEM with energy dispersive spectrometers can be applied as an alternative analysis method for quantitative and qualitative results for a variety of elements without chemical pretreatment, unlike other techniques. This technique characterizes by shortest time, with more less contamination, no reagent consumption, and generation of minimal residue or waste, as well as sample preparations time limiting, with minimal analysis error. Simple dilution for powder or direct analysis for liquid, we analyzed the usefulness of EDS method in testing with field emission scanning electron microscopy (FESEM, SUPRA 55 Carl Zeiss Germany) with an X-ray energy dispersion (XFlash6l10 Bruker Germany). The samples analyzed directly without coating by applied 5µ of known concentrated diluted sample on carbon stub with accelerated voltage according to sample thickness, the result for this spot was in atomic percentage, and by Avogadro converted factor, the final result will be in microgram. Conclusion and recommendation: The conclusion of this study is application of FESEM-EDS in US pharmacopeia and ICH /Q3D guideline to reach a high-precision and accurate method in element impurities analysis of drugs or bulk materials to determine the permitted daily exposure PDE in liquid or solid specimens, and to obtain better results than other techniques, by the way it does not require complex methods or chemicals for digestion, which interfere with the final results with the possibility of to keep the sample at any time for re analysis. The recommendation is to use this technique in pharmacopeia as standard methods like inductively coupled plasma both ICP-AES, ICP-OES, and ICP-MS.

Keywords: pharmacopoeia, FESEM-EDS, element impurities, atomic concentration

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Authors: Rahmat Purwoko, Bambang Riyanto Trilaksono

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This paper gives comparison of INS/GNSS architecture namely Loosely Coupled and Tightly Coupled using Hardware in the Loop Simulation in Guided Missile RKX-200 rocket model. INS/GNSS Tightly Coupled architecture requires pseudo-range, pseudo-range rate, and position and velocity of each satellite in constellation from GPS (Global Positioning System) measurement. The Loosely Coupled architecture use estimated position and velocity from GNSS receiver. INS/GNSS architecture also requires angular rate and specific force measurement from IMU (Inertial Measurement Unit). Loosely Coupled arhitecture designed using 15 states Kalman Filter and Tightly Coupled designed using 17 states Kalman Filter. Integration algorithm calculation using ECEF frame. Navigation System implemented Zedboard All Programmable SoC.

Keywords: kalman filter, loosely coupled, navigation system, tightly coupled

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Authors: H. Aljabiry, L. Bailey, S. Young

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Qatar is a desert with an average temperature 37⁰C, reaching over 40⁰C during summer. Precipitation is uncommon and mostly in winter. Qatar depends on desalination for drinking water and on groundwater and recycled water for irrigation. Water consumption and network leakage per capita in Qatar are amongst the highest in the world; re-use of treated wastewater is extremely limited with only 14% of treated wastewater being used for irrigation. This has led to the country disposing of unwanted water from various sources in lagoons situated around the country, causing concern over the possibility of environmental pollution. Accordingly, our hypothesis underpinning this research is that the quality and quantity of water in lagoons is having an impact on the groundwater reservoirs in Qatar. Lagoons (n = 14) and wells (n = 55) were sampled for both summer and winter in 2018 (summer and winter). Water, adjoining soil and plant samples were analysed for multiple elements by Inductively Coupled Plasma Mass Spectrometry. Organic and inorganic carbon were measured (CN analyser) and the major anions were determined by ion chromatography. Salinization in both the lagoon and the wells was seen with good correlations between Cl⁻, Na⁺, Li, SO₄, S, Sr, Ca, Ti (p-value < 0.05). Association of heavy metals was observed of Ni, Cu, Ag, and V, Cr, Mo, Cd which is due to contamination from anthropological activities such as wastewater disposal or spread of contaminated dust. However, looking at each elements none of them exceeds the Qatari regulation. Moreover, gypsum saturation in the system was observed in both the lagoon and wells water samples. Lagoons and the water of the well are found to be of a saline type as well as Ca²⁺, Cl⁻, SO₄²⁻ type evidencing both gypsum dissolution and salinization in the system. Moreover, Maps produced by Inverse distance weighting showed an increasing level of Nitrate in the groundwater in winter, and decrease chloride and sulphate level, indicating recharge effect after winter rain events. While E. coli and faecal bacteria were found in most of the lagoons, biological analysis for wells needs to be conducted to understand the biological contamination from lagoon water infiltration. As a conclusion, while both the lagoon and the well showed the same results, more sampling is needed to understand the impact of the lagoons on the groundwater.

Keywords: groundwater quality, lagoon, treated wastewater, water management, wastewater treatment, wetlands

Procedia PDF Downloads 107

Authors: Mutiara Effendi

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Nunukan Island is located on North Kalimantan of Indonesia. The region is one of Indonesia’s cross-border with Malaysia. In conjunction with its strategic geographic location, its potential as the new oil and gas resources has brought many researchers to do their studies here. The research area consists of claystone which criss-crossed with quarts sandstone. There are also rocks claystone-grained which are the weathering product of basaltic volcanic rocks. In some places, there are argillic clays which are the hydrothermal-altered product of Sei Apok ancient volcano. Geochemical study was established to learn the origin of the claystones, whether it came from weathering, hydrothermal alteration, or both. The samples used in this research are fresh rock, weathering rocks, hydrothermally-altered rock, and claystones. Chemical compositions of each sample were determined and their relations was studied. The studies encompass major and minor elements analysis using X-Ray Fluoresence (XRF) method and trace elements analysis, specifically rare earth elements, using Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) method. The results were plotted on certain graphics to learn about the trend and the relations of each sample and element. Any changes in chemical compositions, like increase and decrease of elements or species, was analysed to learn about geological phenomenon that happens during the formation of claystones. The result of this study shows that claystones of Nunukan Island have relation with volcanic rocks of its surrounding area. Its chemical composition profile corresponds to weathering product of volcanic rocks rather than hydrothermally-altered product. The general profile also resembles claystone minerals of illite or montmorillonite, especially in the existence of aluminum, iron, potassium, and magnesium. Both minerals are formed in basic condition and commonly happen to shales. It is consistent with the fact that claystone was found mixing with shales and silt to clay grained mudstones in field exploration. Even though the general profile is much alike, the amount of each elements is not precisely the same as theoretically claystone mineral compositions because the mineral have not formed completely yet.

Keywords: claystone, geochemistry, ICP-MS, XRF

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Authors: Ammar Amsyar Abdul Haddi, Mohd Hasni Jaafar

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Heavy metals are elements naturally presented in the environment that can cause adverse effect to health. But not much literature was found on effects toward lung function, where impairment of lung function may lead to various lung diseases. The objective of the study is to explore the lung function impairment, urinary heavy metal level, and its associated factors among the community in Klang valley, Malaysia. Sampling was done in Kuala Lumpur suburb public and housing areas during community events throughout March 2019 till October 2019. respondents who gave the consent were given a questionnaire to answer and was proceeded with a lung function test. Urine samples were obtained at the end of the session and sent for Inductively coupled plasma mass spectrometry (ICP-MS) analysis for heavy metal cadmium (Cd) and lead (Pb) concentration. A total of 200 samples were analysed, and of all, 52% of respondents were male, Age ranging from 18 years old to 74 years old with a mean age of 38.44. Urinary samples show that 12% of the respondent (n=22) has Cd level above than average, and 1.5 % of the respondent (n=3) has urinary Pb at an above normal level. Bivariate analysis show that there was a positive correlation between urinary Cd and urinary Pb (r= 0.309; p<0.001). Furthermore, there was a negative correlation between urinary Cd level and full vital capacity (FVC) (r=-0.202, p=0.004), Force expiratory volume at 1 second (FEV1) (r = -0.225, p=0.001), and also with Force expiratory flow between 25-75% FVC (FEF25%-75%) (r= -0.187, p=0.008). however, urinary Pb did not show any association with FVC, FEV1, FEV1/FVC, or FEF25%-75%. Multiple linear regression analysis shows that urinary Cd remained significant and negatively affect FVC% (p=0.025) and FEV1% (p=0.004) achieved from the predicted value. On top of that, other factors such as education level (p=0.013) and duration of smoking(p=0.003) may influencing both urinary Cd and performance in lung function as well, suggesting Cd as a potential mediating factor between smoking and impairment of lung function. however, there was no interaction detected between heavy metal or other influencing factor in this study. In short, there is a negative linear relationship detected between urinary Cd and lung function, and urinary Cd is likely to affects lung function in a restrictive pattern. Since smoking is also an influencing factor for urinary Cd and lung function impairment, it is highly suggested that smokers should be screened for lung function and urinary Cd level in the future for early disease prevention.

Keywords: lung function, heavy metals, community

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Authors: Rezala Houria, Valverde Jose Luis, Romero Amaya, Molinari Alessandra, Maldotti Andrea

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The escalation of oil prices in 1973 confronted the oil industry with the problem of how to maximize the processing of crude oil, especially the heavy fractions, to give gasoline components. Strong impetus was thus given to the development of catalysts with relatively large pore sizes, which were able to deal with larger molecules than the existing molecular sieves, and with good thermal and hydrothermal stability. The oil embargo in 1973 therefore acted as a stimulus for the investigation and development of pillared clays. Iron doped titania-pillared montmorillonite clays was prepared using bentonite from deposits of Maghnia in western-Algeria. The preparation method consists of differents steps (purification of the raw bentonite, preparation of a pillaring agent solution and exchange of the cations located between the clay layers with the previously formed iron/titanium solution). The characterization of this material was carried out by X-ray fluorescence spectrometry, X-ray diffraction, textural measures by BET method, inductively coupled plasma atomic emission spectroscopy, diffuse reflectance UV visible spectroscopy, temperature- programmed desorption of ammonia and atomic absorption.This new material was investigated as photocatalyst for selective oxygenation of the liquid alkylaromatics such as: toluene, paraxylene and orthoxylene and the photocatalytic properties of it were compared with those of the titanium-pillared clays.

Keywords: iron doping, montmorillonite clays, pillared clays, oil industry

Procedia PDF Downloads 285

Authors: Doroteya K. Staykova, Dirk J. Lefeber, Sabine A. Fuchs, Judith J. M. Jans

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Cholestasis is characterized by the accumulation of toxic bile salts and lipids in the organism. The variety in causes (genetic, immunologic, environmental) and nature (benign, transient, chronic, progressive) combined with the need for early diagnosis and rapid clinical decisions emphasizes the need for good diagnostic strategies to improve patient outcomes. In a current diagnostic analysis of cholestasis, mass-spectrometry metabolomics is a widely adopted tool to enhance clinical decisions at point-of-care, thanks to a short turnaround in measurement times while performing comprehensive molecular profiling of patient material. However, this comes at the cost of difficult-to-identify yet actionable knowledge, often buried within large and heterogenous omics data. Here, we demonstrate how topological data analysis can overcome this challenge in large metabolomics datasets of patients with twenty categories of Metabolic Disorders and overlapping clinical manifestations. To elucidate the complexity of disease progression in three cholestasis patients, we applied topological data analysis to direct-infusion mass spectrometry data collected from 190 plasma samples, including 67 controls, at the University Medical Center in Utrecht, Netherlands. Using the Mapper algorithm and filter function defined as a two-component projection based on Principal Component Analysis, we constructed a topological graph of connected patients, termed a Patient Connectivity Network (PCN). With incorporated clinical and molecular information, PCN revealed the topological shape of causes and severity of cholestasis and transitions in patients’ conditions. In conclusion, topology based PCN provides a holistic view of cholestasis state dynamics that has the potential to support and expedite clinical decisions.

Keywords: mass spectrometry-based metabolomics, patient connectivity network, topological data analysis, unmet clinical needs in Cholestasis

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Authors: Mokhtar Labiod, Nabil Ikhlef, Keltoum Bouherine, Olivier Leroy

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A numerical model for the radio-frequency (RF) Argon discharge chamber is developed to simulate the low pressure low temperature inductively coupled plasma. This model will be of fundamental importance in the design of the plasma magnetic control system. Electric and magnetic fields inside the discharge chamber are evaluated by solving a magnetic vector potential equation. To start with, the equations of the ideal magnetohydrodynamics theory will be presented describing the basic behaviour of magnetically confined plasma and equations are discretized with finite element method in cylindrical coordinates. The discharge chamber is assumed to be axially symmetric and the plasma is treated as a compressible gas. Plasma generation due to ionization is added to the continuity equation. Magnetic vector potential equation is solved for the electromagnetic fields. A strong dependence of the plasma properties on the discharge conditions and the gas temperature is obtained.

Keywords: direct-coupled model, magnetohydrodynamic, modelling, plasma torch simulation

Procedia PDF Downloads 405

Authors: Wed Albalawi, Ebtihaj Jambi, Maha Albazi, Shareefa AlGhamdi

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Heavy metal pollution has become a hard threat to marine ecosystems alongside extremely industrialized and urban (urbanized) zones because of their toxicity, resolution, and non-biodegradable nature. Great interest has been given to a new technique -biosorption- which exploits the cell envelopes of organisms to remove metals from water solutions. The main objective of the present study is to explore the potential of marine algae from the Red Sea for the removal of heavy metals from an aqueous medium. The subsequent objective is to study the effect of pH and agitation time on the adsorption capacity of marine algae. Randomly chosen algae from the Red Sea (Jeddah) with known altitude and depth were collected. Analysis of heavy metal ion concentration was measured by ICP-OES (Inductively coupled plasma - optical emission spectrometry) using air argon gas. A standard solution of heavy metal ions was prepared by diluting the original standard solution with ultrapure water. Types of seaweed were used to study the effect of pH on the biosorption of different heavy metals. The biosorption capacity of Cr is significantly lower in Padina Pavonica (P.P) compared to the biosorption capacity in Sargassum Muticum (S.M). The S.M exhibited significantly higher in Cr removal than the P.P at pH 2 and pH 7. However, the P.P exhibited significantly higher in Cr removal than the S.M at pH 3, pH 4, pH 5, pH 6, and pH 8. In conclusion, the dried cells of algae can be used as an effective tool for the removal of heavy metals.

Keywords: biosorption, heavy metal, pollution, pH value, brown algae

Procedia PDF Downloads 43

Authors: Renata Adriana Labanca, Gabriela Rezende Costa, Nilton de Oliveira Couto e Silva, José Marcos Gontijo Mandarino, Rodrigo Santos Leite, Nilson César Castanheira Guimarães, Roberto Gonçalves Junqueira

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The objective of this study was to evaluate the differences in composition between six brands of conventional soybean and six genetically modified cultivars (GM), all of them from Minas Gerais State, Brazil. We focused on the isoflavones profile and mineral content questioning the substantial equivalence between conventional and GM organisms. The statement of compliance label for conventional grains was verified for the presence of genetic modified genes by real time polymerase chain reaction (PCR). We did not detect the presence of the 35S promoter in commercial samples, indicating the absence of transgene insertion. For mineral analysis, we used the method of inductively coupled plasma-optical emission spectrometry (ICP-OES). Isoflavones quantification was performed by high performance liquid chromatography (HPLC). The results showed no statistical difference between the conventional and transgenic soybean groups concerning isoflavone content and mineral composition. The concentration of potassium, the main mineral component of soy, was the highest in conventional soybeans compared to that in GM soy, while GM samples presented the highest concentrations of iron.

Keywords: glycine max, genetically modified organism, bioactive compounds, ICP-OES, HPLC

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Authors: Tara Miller, Tariq Ganief, Jonathan Blackburn

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Millions of babies are still born to HIV-infected mothers each year despite the ramped-up HAART use. However, these infants are HIV uninfected but exposed, which is now a growing population that has weakened immune systems and poorer outcomes. Due to HIV exposure and possible ARV exposure during pregnancy and breastfeeding, these infants are believed to have altered immune responses and microbiomes when compared to their healthy counterparts. The gut microbiome roles an important role in infant development, specifically in the immune system. Research has shown these HIV-exposed, uninfected infants have weaker immune responses to their neonate vaccines, and in developing countries, this leaves them vulnerable to opportunistic disease. By gaining a deeper understanding of the gut microbiome and the products of the microbes via metaproteomic analysis, we can hopefully understand and improve the immune system and health of these infants. To investigate the metaproteome of the infants’ guts, mass spectrometry will be used, followed by data analysis using DIA-NN. The hypothesized results are that the HIV-exposed, uninfected infants have an altered microbiome compared to their healthy counterparts. Additionally, the differences found are hypothesized to be involved with inflammation which would contribute to the poor health of the infants.

Keywords: HIV, mass spectrometry, metaproteomics, microbiome

Procedia PDF Downloads 57