Search results for: capillary electrophoresis-mass spectrometry

Authors: Bernadett Henn, Katalin Tálos, Éva Kováss Széles

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During the last 50 years, the worldwide permeation of the nuclear techniques induces several new problems in the environmental and in the human life. Nowadays, due to the increasing of the risk of terrorism worldwide, the potential occurrence of terrorist attacks using also weapon of mass destruction containing radioactive or nuclear materials as e.g. dirty bombs, is a real threat. For instance, the uranium pellets are one of the potential nuclear materials which are suitable for making special weapons. The nuclear forensics mainly focuses on the determination of the origin of the confiscated or found nuclear and other radioactive materials, which could be used for making any radioactive dispersive device. One of the most important signatures in nuclear forensics to find the origin of the material is the determination of the rare earth element patterns (REE) in the seized or found radioactive or nuclear samples. The concentration and the normalized pattern of the REE can be used as an evidence of uranium origin. The REE are the fourteen Lanthanides in addition scandium and yttrium what are mostly found together and really low concentration in uranium pellets. The problems of the REE determination using ICP-MS technique are the uranium matrix (high concentration of uranium) and the interferences among Lanthanides. In this work, our aim was to develop an effective chemical sample preparation process using extraction chromatography for separation the uranium matrix and the rare earth elements from each other following some publications can be found in the literature and modified them. Secondly, our purpose was the optimization of the ICP-MS measuring process for REE concentration. During method development, in the first step, a REE model solution was used in two different types of extraction chromatographic resins (LN® and TRU®) and different acidic media for environmental testing the Lanthanides separation. Uranium matrix was added to the model solution and was proved in the same conditions. Methods were tested and validated using REE UOC (uranium ore concentrate) reference materials. Samples were analyzed by sector field mass spectrometer (ICP-SFMS).

Keywords: extraction chromatography, nuclear forensics, rare earth elements, uranium

Procedia PDF Downloads 277

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: Mohit Kumar

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Natural fractures are classified in two broad categories of joints and faults on the basis of shear movement in the deposited strata. Natural fracture always has high structural relationship with extensional or non-extensional tectonics and sometimes the result is seen in the form of micro cracks. Geological evidences suggest that both large and small-scale fractures help in to analyze the seismic anisotropy which essentially contribute into characterization of petro physical properties behavior associated with directional migration of fluid. We generally question why basement study is much needed as historically it is being treated as non-productive and geoscientist had no interest in exploration of these basement rocks. Basement rock goes under high pressure and temperature, and seems to be highly fractured because of the tectonic stresses that are applied to the formation along with the other geological factors such as depositional trend, internal stress of the rock body, rock rheology, pore fluid and capillary pressure. Sometimes carbonate rocks also plays the role of basement and igneous body e.g basalt deposited over the carbonate rocks and fluid migrate from carbonate to igneous rock due to buoyancy force and adequate permeability generated by fracturing. So in order to analyze the complete petroleum system, FMC (Fluid Migration Characterization) is necessary through fractured media including fracture intensity, orientation and distribution both in basement rock and county rock. Thus good understanding of fractures can lead to project the correct wellbore trajectory or path which passes through potential permeable zone generated through intensified P-T and tectonic stress condition. This paper deals with the analysis of these fracture property such as intensity, orientation and distribution in basement rock as large scale fracture can be interpreted on seismic section, however, small scale fractures show ambiguity in interpretation because fracture in basement rock lies below the seismic wavelength and hence shows erroneous result in identification. Seismic attribute technique also helps us to delineate the seismic fracture and subtle changes in fracture zone and these can be inferred from azimuthal anisotropy in velocity and amplitude and spectral decomposition. Seismic azimuthal anisotropy derives fracture intensity and orientation from compressional wave and converted wave data and based on variation of amplitude or velocity with azimuth. Still detailed analysis of fractured basement required full isotropic and anisotropic analysis of fracture matrix and surrounding rock matrix in order to characterize the spatial variability of basement fracture which support the migration of fluid from basement to overlying rock.

Keywords: basement rock, natural fracture, reservoir characterization, seismic attribute

Procedia PDF Downloads 171

Authors: Anna Stepien

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The paper presents the results of research on modifications of sand-lime bricks, especially using glass additives (glass fiber and glass sand) and other additives (e.g.:basalt&barite aggregate, lithium silicate and microsilica) as well. The main goal of this paper is to answer the question ‘How to use glass additives in the sand-lime mass and get a better bricks?’ The article contains information on modification of sand-lime bricks using glass fiber, glass sand, microsilica (different structure of silica). It also presents the results of the conducted compression tests, which were focused on compressive strength, water absorption, bulk density, and their microstructure. The Scanning Electron Microscope, spectrum EDS, X-ray diffractometry and DTA analysis helped to define the microstructural changes of modified products. The interpretation of the products structure revealed the existence of diversified phases i.e.the C-S-H and tobermorite. CaO-SiO2-H2O system is the object of intensive research due to its meaning in chemistry and technologies of mineral binding materials. Because the blocks are the autoclaving materials, the temperature of hydrothermal treatment of the products is around 200°C, the pressure - 1,6-1,8 MPa and the time - up to 8hours (it means: 1h heating + 6h autoclaving + 1h cooling). The microstructure of the products consists mostly of hydrated calcium silicates with a different level of structural arrangement. The X-ray diffraction indicated that the type of used sand is an important factor in the manufacturing of sand-lime elements. Quartz sand of a high hardness is also a substrate hardly reacting with other possible modifiers, which may cause deterioration of certain physical and mechanical properties. TG and DTA curves show the changes in the weight loss of the sand-lime bricks specimen against time as well as the endo- and exothermic reactions that took place. The endothermic effect with the maximum at T=573°C is related to isomorphic transformation of quartz. This effect is not accompanied by a change of the specimen weight. The next endothermic effect with the maximum at T=730-760°C is related to the decomposition of the calcium carbonates. The bulk density of the brick it is 1,73kg/dm3, the presence of xonotlite in the microstructure and significant weight loss during DTA and TG tests (around 0,6% after 70 minutes) have been noticed. Silicate elements were assessed on the basis of their compressive property. Orthogonal compositional plan type 3k (with k=2), i.e.full two-factor experiment was applied in order to carry out the experiments both, in the compression strength test and bulk density test. Some modification (e.g.products with barite and basalt aggregate) have improved the compressive strength around 41.3 MPa and water absorption due to capillary raising have been limited to 12%. The next modification was adding glass fiber to sand-lime mass, then glass sand. The results show that the compressive strength was higher than in the case of traditional bricks, while modified bricks were lighter.

Keywords: bricks, fiber, glass, microstructure

Procedia PDF Downloads 327

Authors: Binyam Teferi

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Numerical and theoretical analysis of mixed convection flow of magneto- hydrodynamics micropolar fluid with stretching capillary in the presence of thermal radiation, chemical reaction, viscous dissipation, and heat generation/ absorption have been studied. The non-linear partial differential equations of momentum, angular velocity, energy, and concentration are converted into ordinary differential equations using similarity transformations which can be solved numerically. The dimensionless governing equations are solved by using Runge Kutta fourth and fifth order along with the shooting method. The effect of physical parameters viz., micropolar parameter, unsteadiness parameter, thermal buoyancy parameter, concentration buoyancy parameter, Hartmann number, spin gradient viscosity parameter, microinertial density parameter, thermal radiation parameter, Prandtl number, Eckert number, heat generation or absorption parameter, Schmidt number and chemical reaction parameter on flow variables viz., the velocity of the micropolar fluid, microrotation, temperature, and concentration has been analyzed and discussed graphically. MATLAB code is used to analyze numerical and theoretical facts. From the simulation study, it can be concluded that an increment of micropolar parameter, Hartmann number, unsteadiness parameter, thermal and concentration buoyancy parameter results in decrement of velocity flow of micropolar fluid; microrotation of micropolar fluid decreases with an increment of micropolar parameter, unsteadiness parameter, microinertial density parameter, and spin gradient viscosity parameter; temperature profile of micropolar fluid decreases with an increment of thermal radiation parameter, Prandtl number, micropolar parameter, unsteadiness parameter, heat absorption, and viscous dissipation parameter; concentration of micropolar fluid decreases as unsteadiness parameter, Schmidt number and chemical reaction parameter increases. Furthermore, computational values of local skin friction coefficient, local wall coupled coefficient, local Nusselt number, and local Sherwood number for different values of parameters have been investigated. In this paper, the following important results are obtained; An increment of micropolar parameter and Hartmann number results in a decrement of velocity flow of micropolar fluid. Microrotation decreases with an increment of the microinertial density parameter. Temperature decreases with an increasing value of the thermal radiation parameter and viscous dissipation parameter. Concentration decreases as the values of Schmidt number and chemical reaction parameter increases. The coefficient of local skin friction is enhanced with an increase in values of both the unsteadiness parameter and micropolar parameter. Increasing values of unsteadiness parameter and micropolar parameter results in an increment of the local couple stress. An increment of values of unsteadiness parameter and thermal radiation parameter results in an increment of the rate of heat transfer. As the values of Schmidt number and unsteadiness parameter increases, Sherwood number decreases.

Keywords: thermal radiation, chemical reaction, viscous dissipation, heat absorption/ generation, similarity transformation

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Authors: M. A. Ferhat, M. N. Boukhatem, F. Chemat

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Eucalyptus essential oil is extracted from Eucalyptus globulus of the Myrtaceae family and is also known as Tasmanian blue gum or blue gum. Despite the reputation earned by aromatic and medicinal plants of Algeria. The objectives of this study were: (i) the extraction of the essential oil from the leaves of Eucalyptus globulus Labill., Myrtaceae grown in Algeria, and the quantification of the yield thereof, (ii) the identification and quantification of the compounds in the essential oil obtained, and (iii) the determination of physical and chemical properties of EGEO. The chemical constituents of Eucalyptus globulus essential oil (EGEO) of Blida origin has not previously been investigated. Thus, the present study has been conducted for the determination of chemical constituents and different physico-chemical properties of the EGEO. Chemical composition of the EGEO, grown in Algeria, was analysed by Gas Chromatography-Mass Spectrometry. The chemical components were identified on the basis of Retention Time and comparing with mass spectral database of standard compounds. Relative amounts of detected compounds were calculated on the basis of GC peak areas. Fresh leaves of E. globulus on steam distillation yielded 0.96% (v/w) of essential oil whereas the analysis resulted in the identification of a total of 11 constituents, 1.8 cineole (85.8%), α-pinene (7.2%), and β-myrcene (1.5%) being the main components. Other notable compounds identified in the oil were β-pinene, limonene, α-phellandrene, γ-terpinene, linalool, pinocarveol, terpinen-4-ol, and α-terpineol. The physical properties such as specific gravity, refractive index and optical rotation and the chemical properties such as saponification value, acid number and iodine number of the EGEO were examined. The oil extracted has been analyzed to have 1.4602-1.4623 refractive index value, 0.918-0.919 specific gravity (sp.gr.), +9 - +10 optical rotation that satisfy the standards stipulated by European Pharmacopeia. All the physical and chemical parameters were in the range indicated by the ISO standards. Our findings will help to access the quality of the Eucalyptus oil which is important in the production of high value essential oils that will help to improve the economic condition of the community as well as the nation.

Keywords: chemical composition, essential oil, eucalyptol, gas chromatography

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Authors: Ahmed El-Fiqi, Hae-Won Kim

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Incorporation of therapeutic elements such as Sr, Cu and Co into bioglass structure and their release as ions is considered as one of the promising approaches to enhance cellular responses, e.g., osteogenesis and angiogenesis. Here, cobalt as angiogenesis promoter has been incorporated (at 0, 1 and 4 mol%) into sol-gel derived calcium silicate mesoporous bioglass nanoparticles. The composition and structure of cobalt-free (CFN) and cobalt-doped (CDN) mesoporous bioglass nanoparticles have been analyzed by X-ray fluorescence (XRF), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Fourier-Transform Infra-red spectroscopy (FT-IR). The physicochemical properties of CFN and CDN have been investigated using high-resolution transmission electron microscopy (HR-TEM), Selected area electron diffraction (SAED), and Energy-dispersive X-ray (EDX). Furthermore, the textural properties, including specific surface area, pore-volume, and pore size, have been analyzed from N²⁻sorption analyses. Surface charges of CFN and CDN were also determined from surface zeta potential measurements. The release of ions, including Co²⁺, Ca²⁺, and SiO₄⁴⁻ has been analyzed using inductively coupled plasma atomic emission spectrometry (ICP-AES). Loading and release of diclofenac as an anti-inflammatory drug model were explored in vitro using Ultraviolet-visible spectroscopy (UV-Vis). XRD results ensured the amorphous state of CFN and CDN whereas, XRF further confirmed that their chemical compositions are very close to the designed compositions. HR-TEM analyses unveiled nanoparticles with spherical morphologies, highly mesoporous textures, and sizes in the range of 90 - 100 nm. Moreover, N²⁻ sorption analyses revealed that the nanoparticles have pores with sizes of 3.2 - 2.6 nm, pore volumes of 0.41 - 0.35 cc/g and highly surface areas in the range of 716 - 830 m²/g. High-resolution XPS analysis of Co 2p core level provided structural information about Co atomic environment and it confirmed the electronic state of Co in the glass matrix. ICP-AES analysis showed the release of therapeutic doses of Co²⁺ ions from 4% CDN up to 100 ppm within 14 days. Finally, diclofenac loading and release have ensured the drug/ion co-delivery capability of 4% CDN.

Keywords: mesoporous bioactive glass, nanoparticles, cobalt ions, release

Procedia PDF Downloads 85

Authors: Luciana P. Mazur, Tatiana A. Pozdniakova, Rui A. R. Boaventura, Vitor J. P. Vilar

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The principal mechanism of metal ions sequestration by brown algae involves the formation of complexes between the metal ion and functional groups present on the cell wall of the biological material. To understand the role of functional groups on copper(II) uptake by Ascophyllum nodosum, some functional groups were chemically modified. The esterification of carboxylic groups was carried out by suspending the biomass in a methanol/HCl solution under stirring for 48 h and the blocking of the sulfonic groups was performed by repeating the same procedure for 4 cycles of 48 h. The methylation of amines was conducted by suspending the biomass in a formaldehyde/formic acid solution under shaking for 6 h and the chemical modification of sulfhydryl groups on the biomass surface was achieved using dithiodipyridine for 1 h. Equilibrium sorption studies for Cu2+ using the raw and esterified algae were performed at pH 2.0 and 4.0. The experiments were performed using an initial copper concentration of 300 mg/L and algae dose of 1.0 g/L. After reaching the equilibrium, the metal in solution was quantified by atomic absorption spectrometry. The biological material was analyzed by Fourier Transform Infrared Spectroscopy and Potentiometric Titration techniques for functional groups identification and quantification, respectively. The results using unmodified algae showed that the maximum copper uptake capacity at pH 4.0 and 2.0 was 1.17 and 0.52 mmol/g, respectively. At acidic pH values most carboxyl groups are protonated and copper sorption suffered a significant reduction of 56%. Blocking the carboxylic, sulfonic, amines and sulfhydryl functional groups, copper uptake decreased by 24/26%, 69/81%, 1/23% and 40/27% at pH 2.0/4.0, respectively, when compared to the unmodified biomass. It was possible to conclude that the carboxylic and sulfonic groups are the main functional groups responsible for copper binding (>80%). This result is supported by the fact that the adsorption capacity is directly related to the presence of carboxylic groups of the alginate polymer, and the second most abundant acidic functional group in brown algae is the sulfonic acid of fucoidan that contributes, to a lower extent, to heavy metal binding, particularly at low pH.

Keywords: biosorption, brown marine macroalgae, copper, ion-exchange

Procedia PDF Downloads 297

Authors: Saurabh B. Ganorkar, Atul A. Shirkhedkar

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The need for investigations protecting against toxic impurities though seems to be a primary requirement; the impurities which may prove non - toxic can be explored for their therapeutic potential if any to assist advanced drug discovery. The essential role of pharmaceutical analysis can thus be extended effectively to achieve it. The present study successfully achieved these objectives with characterization of major degradation products as impurities for Zileuton which has been used for to treat asthma since years. The forced degradation studies were performed to identify the potential degradation products using Ultra-fine Liquid-chromatography. Liquid-chromatography-Mass spectrometry (Time of Flight) and Proton Nuclear Magnetic Resonance Studies were utilized effectively to characterize the drug along with five major oxidative and hydrolytic degradation products (DP’s). The mass fragments were identified for Zileuton and path for the degradation was investigated. The characterized DP’s were subjected to In-Silico studies as XP Molecular Docking to compare the gain or loss in binding affinity with 5-Lipooxygenase enzyme. One of the impurity of was found to have the binding affinity more than the drug itself indicating for its potential to be more bioactive as better Antiasthmatic. The close structural resemblance has the ability to potentiate or reduce bioactivity and or toxicity. The chances of being active biologically at other sites cannot be denied and the same is achieved to some extent by predictions for probability of being active with Prediction of Activity Spectrum for Substances (PASS) The impurities found to be bio-active as Antineoplastic, Antiallergic, and inhibitors of Complement Factor D. The toxicological abilities as Ames-Mutagenicity, Carcinogenicity, Developmental Toxicity and Skin Irritancy were evaluated using Toxicity Prediction by Komputer Assisted Technology (TOPKAT). Two of the impurities were found to be non-toxic as compared to original drug Zileuton. As the drugs are purposed and repurposed effectively the impurities can also be; as they can have more binding affinity; less toxicity and better ability to be bio-active at other biological targets.

Keywords: UFLC, LC-MS-TOF, NMR, Zileuton, impurities, toxicity, bio-activity

Procedia PDF Downloads 171

Authors: M. Soleimani, D. Cree, C. Chafe, L. Bates

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The accidental release of petroleum products into the environment could have harmful consequences to our ecosystem. Different techniques such as mechanical separation, membrane filtration, incineration, treatment processes using enzymes and dispersants, bioremediation, and sorption process using sorbents have been applied for oil spill remediation. Most of the techniques investigated are too costly or do not have high enough efficiency. This study was conducted to determine the sorption performance of hemp byproducts (cellulosic materials) in terms of sorption capacity and kinetics for hydrophobic and hydrophilic fluids. In this study, heavy oil, light oil, diesel fuel, and water/water vapor were used as sorbate fluids. Hemp stalk in different forms, including loose material (hammer milled (HM) and shredded (Sh) with low bulk densities) and densified forms (pellet form (P) and crumbled pellets (CP)) with high bulk densities, were used as sorbents. The sorption/retention tests were conducted according to ASTM 726 standard. For a quick-purpose application of the sorbents, the sorption tests were conducted for 15 min, and for an ideal sorption capacity of the materials, the tests were carried out for 24 h. During the test, the sorbent material was exposed to the fluid by immersion, followed by filtration through a stainless-steel wire screen. Water vapor adsorption was carried out in a controlled environment chamber with the capability of controlling relative humidity (RH) and temperature. To determine the kinetics of sorption for each fluid and sorbent, the retention capacity also was determined intervalley for up to 24 h. To analyze the kinetics of sorption, pseudo-first-order, pseudo-second order and intraparticle diffusion models were employed with the objective of minimal deviation of the experimental results from the models. The results indicated that HM and Sh materials had the highest sorption capacity for the hydrophobic fluids with approximately 6 times compared to P and CP materials. For example, average retention values of heavy oil on HM and Sh was 560% and 470% of the mass of the sorbents, respectively. Whereas, the retention of heavy oil on P and CP was up to 85% of the mass of the sorbents. This lower sorption capacity for P and CP can be due to the less exposed surface area of these materials and compacted voids or capillary tubes in the structures. For water uptake application, HM and Sh resulted in at least 40% higher sorption capacity compared to those obtained for P and CP. On average, the performance of sorbate uptake from high to low was as follows: water, heavy oil, light oil, diesel fuel. The kinetic analysis indicated that the second-pseudo order model can describe the sorption process of the oil and diesel better than other models. However, the kinetics of water absorption was better described by the pseudo-first-order model. Acetylation of HM materials could improve its oil and diesel sorption to some extent. Water vapor adsorption of hemp fiber was a function of temperature and RH, and among the models studied, the modified Oswin model was the best model in describing this phenomenon.

Keywords: environment, fiber, petroleum, sorption

Procedia PDF Downloads 106

Authors: Eman Abdullah Morsi, Hend Okasha, Heba Abdel Hady, Mortada El-Sayed, Mohamed Abbas Shemis

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Context: Linum usitatissimum (Linn), known as Flaxseed, is one of the most important medicinal plants traditionally used for various health as nutritional purposes. Objective: Estimation of total phenolic and flavonoid contents as well as evaluate the antioxidant using α, α-diphenyl-β-picrylhydrazyl (DPPH), 2-2'azinobis (3-ethylbenzthiazoline-6-sulphonic acid (ABTS) and total antioxidant capacity (TAC) assay and investigation of anti-inflammatory by Bovine serum albumin (BSA) and anticancer activities of hepatocellular carcinoma cell line (HepG2) and breast cancer cell line (MCF7) have been applied on hexane, ethyl acetate, n-butanol and methanol extracts and also, fractions of methonal extract (hexane, ethyl acetate and n-butanol). Materials and Methods: Phenolic and flavonoid contents were detected using spectrophotometric and colorimetric assays. Antioxidant and anti-inflammatory activities were estimated in-vitro. Anticancer activity of extracts and fractions of methanolic extract were tested on (HepG2) and (MCF7). Results: Methanolic extract and its ethyl acetate fraction contain higher contents of total phenols and flavonoids. In addition, methanolic extract had higher antioxidant activity. Butanolic and ethyl acetate fractions yielded higher percent of inhibition of protein denaturation. Meanwhile, ethyl acetate fraction and methanolic extract had anticancer activity against HepG2 and MCF7 (IC50=60 ± 0.24 and 29.4 ± 0.12µg.mL⁻¹) and (IC50=94.7 ± 0.21 and 227 ± 0.48µg.mL⁻¹), respectively. In Gas chromatography-mass spectrometry (GC-MS) analysis, methanolic extract has 32 compounds, whereas; ethyl acetate and butanol fractions contain 40 and 36 compounds, respectively. Conclusion: Flaxseed contains totally different biologically active compounds that have been found to possess good variable activities, which can protect human body against several diseases.

Keywords: phenolic content, flavonoid content, HepG2, MCF7, hemolysis-assay, flaxseed

Procedia PDF Downloads 101

Authors: Chanchal Biswas, Anrin Bhattacharyya, Gopes Chandra Das, Mahua Ghosh Chaudhuri, Rajib Dey

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Boiler coals with low fixed carbon and higher ash content have always challenged the metallurgists to develop a suitable method for their utilization. In the present study, an attempt is made to establish an energy effective method for the reduction of iron ore fines in the form of nuggets by using ‘Syngas’. By devolatisation (expulsion of volatile matter by applying heat) of boiler coal, gaseous product (enriched with reducing agents like CO, CO2, H2, and CH4 gases) is generated. Iron ore nuggets are reduced by this syngas. For that reason, there is no direct contact between iron ore nuggets and coal ash. It helps to control the minimization of the sulphur intake of the reduced nuggets. A laboratory scale devolatisation furnace designed with reduction facility is evaluated after in-depth studies and exhaustive experimentations including thermo-gravimetric (TG-DTA) analysis to find out the volatile fraction present in boiler grade coal, gas chromatography (GC) to find out syngas composition in different temperature and furnace temperature gradient measurements to minimize the furnace cost by applying one heating coil. The nuggets are reduced in the devolatisation furnace at three different temperatures and three different times. The pre-reduced nuggets are subjected to analytical weight loss calculations to evaluate the extent of reduction. The phase and surface morphology analysis of pre-reduced samples are characterized using X-ray diffractometry (XRD), energy dispersive x-ray spectrometry (EDX), scanning electron microscopy (SEM), carbon sulphur analyzer and chemical analysis method. Degree of metallization of the reduced nuggets is 78.9% by using boiler grade coal. The pre-reduced nuggets with lesser sulphur content could be used in the blast furnace as raw materials or coolant which would reduce the high quality of coke rate of the furnace due to its pre-reduced character. These can be used in Basic Oxygen Furnace (BOF) as coolant also.

Keywords: alternative ironmaking, coal gasification, extent of reduction, nugget making, syngas based DRI, solid state reduction

Procedia PDF Downloads 242

Authors: Amanina Iymia Jeffree, Reena Thriumani, Mohammad Iqbal Omar, Ammar Zakaria, Yumi Zuhanis Has-Yun Hashim, Ali Yeon Md Shakaff

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Metabolite profiling is a strategy to be approached in the pattern recognition method focused on three types of cancer cell line that driving the most to death specifically lung, breast, and colon cancer. The purpose of this study was to discriminate the VOCs pattern among cancerous and control group based on metabolite profiling. The sampling was executed utilizing the cell culture technique. All culture flasks were incubated till 72 hours and data collection started after 24 hours. Every running sample took 24 minutes to be completed accordingly. The comparative metabolite patterns were identified by the implementation of headspace-solid phase micro-extraction (HS-SPME) sampling coupled with gas chromatography-mass spectrometry (GCMS). The optimizations of the main experimental variables such as oven temperature and time were evaluated by response surface methodology (RSM) to get the optimal condition. Volatiles were acknowledged through the National Institute of Standards and Technology (NIST) mass spectral database and retention time libraries. To improve the reliability of significance, it is of crucial importance to eliminate background noise which data from 3rd minutes to 17th minutes were selected for statistical analysis. Targeted metabolites, of which were annotated as known compounds with the peak area greater than 0.5 percent were highlighted and subsequently treated statistically. Volatiles produced contain hundreds to thousands of compounds; therefore, it will be optimized by chemometric analysis, such as principal component analysis (PCA) as a preliminary analysis before subjected to a pattern classifier for identification of VOC samples. The volatile organic compound profiling has shown to be significantly distinguished among cancerous and control group based on metabolite profiling.

Keywords: in vitro cancer cell line, metabolite profiling, pattern recognition, volatile organic compounds

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Authors: Mengsha Yin

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Extractable organic matter (EOM) from thirty-six biogenic gas source rocks from the Sanhu Depression in Qaidam Basin in northwestern China were obtained via Soxhlet extraction. Twenty-nine of them were conducted SARA (Saturates, Aromatics, Resins and Asphaltenes) separation for bulk composition analysis. Saturated and aromatic fractions of all the extractions were analyzed by Gas Chromatography-Mass Spectrometry (GC-MS) to investigate the compound compositions. More abundant n-alkanes, naphthalene, phenanthrene, dibenzothiophene and their alkylated products occur in samples in shallower depths. From 2000m downward, concentrations of these compounds increase sharply, and concentration ratios of more-over-less biodegradation susceptible compounds coincidently decrease dramatically. ∑iC15-16, 18-20/∑nC15-16, 18-20 and hopanoids/∑n-alkanes concentration ratios and mono- and tri-aromatic sterane concentrations and concentration ratios frequently fluctuate with depth rather than trend with it, reflecting effects from organic input and paleoenvironments other than biodegradation. Saturated and aromatic compound distributions on the saturates and aromatics total ion chromatogram (TIC) traces of samples display different degrees of biodegradation. Dramatic and simultaneous variations in compound concentrations and their ratios at 2000m and their changes with depth underneath cooperatively justified the crucial control of burial depth on organic matter biodegradation scales in source rocks and prompted the proposition that 2000m is the bottom depth boundary for active microbial activities in this study. The study helps to better curb the conditions where effective source rocks occur in terms of depth in the Sanhu biogenic gas fields and calls for additional attention to source rock pore size estimation during biogenic gas source rock appraisals.

Keywords: pore space, Sanhu depression, saturated and aromatic hydrocarbon compound concentration, source rock organic matter biodegradation, total ion chromatogram

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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

Procedia PDF Downloads 193

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

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

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

Procedia PDF Downloads 150

Authors: Fariba Tadayon, Elmira Hassanlou, Hasan Bagheri, Mostafa Jafarian

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Heavy metals are released into water, plants, soil, and food by natural and human activities. Lead has toxic roles in the human body and may cause serious problems even in low concentrations, since it may have several adverse effects on human. Therefore, determination of lead in different samples is an important procedure in the studies of environmental pollution. In this work, an ultrasonic assisted-ionic liquid based-liquid-liquid microextraction (UA-IL-DLLME) procedure for the determination of lead in zucchini, pomegranate, and lettuce has been established and developed by using flame atomic absorption spectrometer (FAAS). For UA-IL-DLLME procedure, 10 mL of the sample solution containing Pb2+ was adjusted to pH=5 in a glass test tube with a conical bottom; then, 120 μL of 1-Hexyl-3-methylimidazolium hexafluoro phosphate (CMIM)(PF6) was rapidly injected into the sample solution with a microsyringe. After that, the resulting cloudy mixture was treated by ultrasonic for 5 min, then the separation of two phases was obtained by centrifugation for 5 min at 3000 rpm and IL-phase diluted with 1 cc ethanol, and the analytes were determined by FAAS. The effect of different experimental parameters in the extraction step including: ionic liquid volume, sonication time and pH was studied and optimized simultaneously by using Response Surface Methodology (RSM) employing a central composite design (CCD). The optimal conditions were determined to be an ionic liquid volume of 120 μL, sonication time of 5 min, and pH=5. The linear ranges of the calibration curve for the determination by FAAS of lead were 0.1-4 ppm with R2=0.992. Under optimized conditions, the limit of detection (LOD) for lead was 0.062 μg.mL-1, the enrichment factor (EF) was 93, and the relative standard deviation (RSD) for lead was calculated as 2.29%. The levels of lead for pomegranate, zucchini, and lettuce were calculated as 2.88 μg.g-1, 1.54 μg.g-1, 2.18 μg.g-1, respectively. Therefore, this method has been successfully applied for the analysis of the content of lead in different food samples by FAAS.

Keywords: Dispersive liquid-liquid microextraction, Central composite design, Food samples, Flame atomic absorption spectrometry.

Procedia PDF Downloads 257

Authors: Laribi-Habchi Hasiba, Bouanane-Darenfed Amel, Drouiche Nadjib, Pausse André, Mameri Nabil

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Chitin, a linear 1, 4-linked N-acetyl-d-glucosamine (GlcNAc) polysaccharide is the major structural component of fungal cell walls, insect exoskeletons and shells of crustaceans. It is one of the most abundant naturally occurring polysaccharides and has attracted tremendous attention in the fields of agriculture, pharmacology and biotechnology. Each year, a vast amount of chitin waste is released from the aquatic food industry, where crustaceans (prawn, crab, Shrimp and lobster) constitute one of the main agricultural products. This creates a serious environmental problem. This linear polymer can be hydrolyzed by bases, acids or enzymes such as chitinase. In this context an extracellular chitinase (ChiA-65) was produced and purified from a newly isolated LHH100. Pure protein was obtained after heat treatment and ammonium sulphate precipitation followed by Sephacryl S-200 chromatography. Based on matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF/MS) analysis, the purified enzyme is a monomer with a molecular mass of 65,195.13 Da. The sequence of the 27 N-terminal residues of the mature ChiA-65 showed high homology with family-18 chitinases. Optimal activity was achieved at pH 4 and 75◦C. Among the inhibitors and metals tested p-chloromercuribenzoic acid, N-ethylmaleimide, Hg2+ and Hg + completelyinhibited enzyme activity. Chitinase activity was high on colloidal chitin, glycol chitin, glycol chitosane, chitotriose and chitooligosaccharide. Chitinase activity towards synthetic substrates in the order of p-NP-(GlcNAc) n (n = 2–4) was p-NP-(GlcNAc)2> p-NP-(GlcNAc)4> p-NP-(GlcNAc)3. Our results suggest that ChiA-65 preferentially hydrolyzed the second glycosidic link from the non-reducing end of (GlcNAc) n. ChiA-65 obeyed Michaelis Menten kinetics the Km and kcat values being 0.385 mg, colloidal chitin/ml and5000 s−1, respectively. ChiA-65 exhibited remarkable biochemical properties suggesting that this enzyme is suitable for bioconversion of chitin waste.

Keywords: Bacillus licheniformis LHH100, characterization, extracellular chitinase, purification

Procedia PDF Downloads 416

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 109

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

Procedia PDF Downloads 212

Authors: Hanaa A. Al-Gaoudi, Hassan Ebeid

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The research investigates the materials and processes used in the manufacturing of an Egyptian polychrome cartonnage mummy mask with the aim of dating this object and establishing trade patterns of certain materials that were used and available at the time of ancient Egypt. This anonymous-source object was held in the basement storage of the Egyptian Museum in Cairo (EMC) and has never been on display. Furthermore, there is no information available regarding its owner, provenance, date, and even the time of its possession by the museum. Moreover, the object is in a very poor condition where almost two-thirds of the mask was bent and has never received any previous conservation treatment. This research has utilized well-established multi-analytical methods to identify the considerable diversity of materials that have been used in the manufacturing of this object. These methods include Computed Tomography Scan (CT scan) to acquire detailed pictures of the inside physical structure and condition of the bended layers. Dino-Lite portable digital microscope, scanning electron microscopy with energy dispersive X-ray spectrometer (SEM-EDX), and the non-invasive imaging technique of multispectral imaging (MSI) to obtain information about the physical characteristics and condition of the painted layers and to examine the microstructure of the materials. Portable XRF Spectrometer (PXRF) and X-Ray powder diffraction (XRD) to identify mineral phases and the bulk element composition in the gilded layer, ground, and pigments; Fourier-transform infrared (FTIR) to identify organic compounds and their molecular characterization; accelerator mass spectrometry (AMS 14C) to date the object. Preliminary results suggest that there are no human remains inside the object, and the textile support is linen fibres with tabby weave 1/1 and these fibres are in a very bad condition. Several pigments have been identified, such as Egyptian blue, Magnetite, Egyptian green frit, Hematite, Calcite, and Cinnabar; moreover, the gilded layers are pure gold and the binding media in the pigments is Arabic gum and animal glue in the textile support layer.

Keywords: analytical methods, Egyptian museum, mummy mask, pigments, textile

Procedia PDF Downloads 98

Authors: Navpreet Kaur, Himkusha Thakur, Nirmal Prabhakar

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The most controversial issue in crop production is the use of Organophosphate insecticides. This is evident in many reports that Organophosphate (OP) insecticides, among the broad range of pesticides are mainly involved in acute and chronic poisoning cases. OPs detection is of crucial importance for health protection, food and environmental safety. In our study, a nanocomposite of poly (3,4 ethylenedioxythiophene) (PEDOT) and multi-walled carbon nanotubes (MWCNTs) has been deposited electrochemically onto the surface of fluorine doped tin oxide sheets (FTO) for the analysis of malathion OP. The -COOH functionalization of MWCNTs has been done for the covalent binding with amino groups of AChE enzyme. The use of PEDOT-MWCNT films exhibited an excellent conductivity, enables fast transfer kinetics and provided a favourable biocompatible microenvironment for AChE, for the significant malathion OP detection. The prepared biosensors were characterized by Fourier transform infrared spectrometry (FTIR), Field emission-scanning electron microscopy (FE-SEM) and electrochemical studies. Various optimization studies were done for different parameters including pH (7.5), AChE concentration (50 mU), substrate concentration (0.3 mM) and inhibition time (10 min). Substrate kinetics has been performed and studied for the determination of Michaelis Menten constant. The detection limit for malathion OP was calculated to be 1 fM within the linear range 1 fM to 1 µM. The activity of inhibited AChE enzyme was restored to 98% of its original value by 2-pyridine aldoxime methiodide (2-PAM) (5 mM) treatment for 11 min. The oxime 2-PAM is able to remove malathion from the active site of AChE by means of trans-esterification reaction. The storage stability and reusability of the prepared biosensor is observed to be 30 days and seven times, respectively. The application of the developed biosensor has also been evaluated for spiked lettuce sample. Recoveries of malathion from the spiked lettuce sample ranged between 96-98%. The low detection limit obtained by the developed biosensor made them reliable, sensitive and a low cost process.

Keywords: PEDOT-MWCNT, malathion, organophosphates, acetylcholinesterase, biosensor, oxime (2-PAM)

Procedia PDF Downloads 425

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

Procedia PDF Downloads 132

Authors: Mathodzi Nditsheni, Olawole Emmanuel Aina, Joshua Oluwole Olowoyo

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The ever-increasing world population is putting extreme pressure on the already limited agricultural resources for food production. Different soil enhancers were introduced by famers to meet the need of the ever-increasing population demand for food. One of the soil enhancers is the municipal waste sludge. This research investigated the differences in the concentrations of trace metals and levels of phytochemicals in four different tomato varieties cultivated on soil treated with municipal waste sludge in Pretoria, South Africa. Fruits were harvested at maturity and analyzed for trace metals and phytochemicals contents using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and a High-Performance Liquid Chromatography (HPLC) respectively. A one-way analysis of variance (ANOVA) was used to determine the differences in the concentrations of trace metals and phytochemical from different tomato varieties were significant. From the study, Rodade tomato bioaccumulated the highest concentrations of Mn, Cr, Cu and Ni, Roma bioaccumulated the highest concentrations of, Cd, Fe and Pb while Heinz bioaccumulated the highest concentrations of As and Zn. Cherry tomato on the other hand, recorded the lowest concentrations for most metals, Cd, Cr, Cu, Mn, Ni, Pb and Zn. The results of the study further showed that phenolic and flavonoids content were higher in the Solanum lycopersicum fruit grown in soils treated with municipal waste sludge. The study also showed that there was an inverse relationship between the levels of trace metals and phytochemicals. The calculated contamination factor values of trace metals like Cr, Cu, Pb and Zn were above the safe value of 1 which indicated that the tomato fruits may be unsafe for human consumption. However, the contamination factor values for the remaining trace metals were well below the safe value of 1. From the results obtained either for the control group or the treatment, the tomato varieties used in the study, bioaccumulated the toxic trace metals in their fruits and some of the values obtained were higher than the acceptable limit, which may then imply that the varieties of tomato used in this study bio accumulated the toxic trace metals from the soil, hence care should be taken when these tomato varieties are either cultivated or harvested from polluted areas

Keywords: trace metals, flavonoids, phenolics, waste sludge, tomato, contamination factors

Procedia PDF Downloads 52

Authors: K. Tesfamariam, S. Gebreyesus, C. Lachat, P. Kolsteren, S. De Saeger, M. De Boevre, A. Argaw

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Aflatoxins are toxic secondary metabolites produced by Aspergillus fungi, which are ubiquitously present in the food supplies of low- and middle-income countries. Studies of maternal aflatoxin exposure and fetal outcomes are mainly focused on size at birth and the effect on intrauterine fetal growth has not been assessed using repeated longitudinal fetal biometry across gestation. Therefore, this study intends to assess the association between chronic aflatoxin exposure during pregnancy and fetal growth trajectories in a rural Ethiopian setting. In a prospective cohort study, we enrolled 492 pregnant women. A phlebotomist collected 5 mL of a venous blood sample from eligible women before 28 completed weeks of gestation and aflatoxin B1-lysine concentration was determined using liquid chromatography-tandem mass spectrometry. The mean (±SD) gestational age was 19.1 (3.71) weeks at enrollment, and 28.5 (3.51) and 34.5 (2.44) weeks of gestation at the second and third rounds of ultrasound measurements, respectively. Estimated fetal weight was expressed in centiles using the INTERGROWTH-21st reference. We fitted a multivariable linear mixed-effects model to estimate the rate of fetal growth between aflatoxin-exposed (i.e., aflatoxin B1-lysine concentration above or equal to the limit of detection) and non-exposed mothers in the study. Mothers had a mean (±SD) age of 26.0 (4.58) years. The median (P25, P75) serum AFB1-lysine concentration was 12.6 (0.93, 96.9) pg/mg albumin, and aflatoxin exposure was observed in 86.6% of maternal blood samples. Eighty-five percent of the women enrolled provided at least two ultrasound measurements for analysis. On average, the aflatoxin-exposed group had a significantly lower change over time in fetal weight-for-gestational age centile than the unexposed group (ß = -1.01 centiles/week, 95% CI: -1.87, -0.15, p = 0.02). Chronic maternal AF exposure is associated with lower fetal weight gain over time. Our findings emphasize the importance of nutrition-sensitive strategies to mitigate dietary aflatoxin exposure as well as adopting food safety measures in low-income settings, particularly during the fetal period of development.

Keywords: aflatoxin, fetal growth, low-income setting, mycotoxins

Procedia PDF Downloads 107

Authors: Iwona Cieślik, Władysław Migdał, Kinga Topolska, Ewa Cieślik

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The consumption of fish is recommended as a means of preventing serious diseases, especially cardiovascular problems. Fish is known to be a valuable source of protein (rich in essential amino acids), unsaturated fatty acids, fat-soluble vitamins, macro- and microelements. However, it can also contain several contaminants (e.g. pesticides, heavy metals) that may pose considerable risks for humans. Among others, pesticide are of special concern. Their widespread use has resulted in the contamination of environmental compartments, including water. The occurrence of pesticides in the environment is a serious problem, due to their potential toxicity. Therefore, a systematic monitoring is needed. The aim of the study was to determine the organochlorine and organophosphate pesticide residues in fish muscle tissues of the pike (Esox lucius, L.) and the rainbow trout (Oncorhynchus mykkis, Walbaum) by a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method, using Gas Chromatography Quadrupole Mass Spectrometry (GC/Q-MS), working in selected-ion monitoring (SIM) mode. The analysis of α-HCH, β-HCH, lindane, diazinon, disulfoton, δ-HCH, methyl parathion, heptachlor, malathion, aldrin, parathion, heptachlor epoxide, γ-chlordane, endosulfan, α-chlordane, o,p'-DDE, dieldrin, endrin, 4,4'-DDD, ethion, endrin aldehyde, endosulfan sulfate, 4,4'-DDT, and metoxychlor was performed in the samples collected in the Carp Valley (Malopolska region, Poland). The age of the pike (n=6) was 3 years and its weight was 2-3 kg, while the age of the rainbow trout (n=6) was 0.5 year and its weight was 0.5-1.0 kg. Detectable pesticide (HCH isomers, endosulfan isomers, DDT and its metabolites as well as metoxychlor) residues were present in fish samples. However, all these compounds were below the limit of quantification (LOQ). The other examined pesticide residues were below the limit of detection (LOD). Therefore, the levels of contamination were - in all cases - below the default Maximum Residue Levels (MRLs), established by Regulation (EC) No 396/2005 of the European Parliament and of the Council. The monitoring of pesticide residues content in fish is required to minimize potential adverse effects on the environment and human exposure to these contaminants.

Keywords: contaminants, fish, pesticides residues, QuEChERS method

Procedia PDF Downloads 191

Authors: Mustapha A. Tijjani, Fanna I. Abdulrahman, Irfan Z. Khan, Umar K. Sandabe, Cong Li

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Air dried sample V. doniana after collection and identification was extracted with ethanol and further partition with chloroform, ethyl acetate and n-butanol. Ethanolic extract (11.9g) was fractionated on a silica gel accelerated column chromatography using solvents such as n-hexane, ethyl acetate and methanol. Each eluent fractions (150ml aliquots) were collected and monitored with thin layer chromatography. Fractions with similar Rf values from same solvents system were pooled together. Phytochemical test of all the fractions were performed using standard procedure. Complete elution yielded 48 fractions (150ml/fraction) which were pooled to 24 fractions base on the Rf values. It was further recombined and 12 fractions were obtained on the basis on Rf values and coded Vd1 to Vd12 fractions. Vd8 was further eluted with ethylacetate and methanol and gave fourteen sub fractions Vd8-a, -Vd8-m. Fraction Vd8-a (56mg) gave a white crystal compound coded V1. It was further checked on TLC and observed under ultraviolet lamp and was found to give a single spot. The Rf values were calculated to be 0.433. The melting point was determined using Gallenkamp capillary melting point apparatus and found to be 241-243°C uncorrected. Characterization of the isolated compound coded V1 was done using FT-infra-red spectroscopy, HNMR, 13CNMR(1and 2D) and HRESI-MS. The IR spectrum of compound V1 shows prominent peaks that corresponds to OHstr (3365cm-1) and C=0 (1652cm-1) etc. This spectrum suggests that among the functional moiety in compound V1 are the carbonyl and hydroxyl group. The 1H NMR (400 MHz) spectrum of compound V1 in DMSO-d6 displayed five singlet signals at δ 0.72 (3H, s, H-18), 0.79 (3H, s, H-19), 1.03 (3H, s, H-21), 1.04 (3H, s, H-26), 1.06 (3H, s, H-27) each integrating for three protons indicating the five methyl functional groups present in the compound. It further showed a broad singlet at δ 5.58 integrated for 1 H due to an olefinic H-atom adjacent to the carbonyl carbon atom. Three signals at δ 3.10 (d, J = 9.0 Hz, H-22), 3.59 (m, 1H, 2H-a) and 3.72 (m, 1H, 3H-e), each integrating for one proton is due to oxymethine protons indicating that three oxymethine H-atoms are present in the compound. These all signals are characteristic to the ecdysteroid skeletons. The 13C-NMR spectrum showed the presence of 27 carbon atoms, suggesting that may be steroid skeleton. The DEPT-135 experiment showed the presence of five CH3, eight CH2, and seven CH groups, and seven quaternary C-atoms. The molecular formula was established as C27H44O7 by high resolution electron spray ionization-mass spectroscopy (HRESI-MS) positive ion mode m/z 481.3179. The signals in mass spectrum are 463, 445, and 427 peaks corresponding to losses of one, two, three, or four water molecules characteristic for ecdysterone skeleton reported in the literature. Based on the spectral analysis (HNMR, 13CNMR, DEPT, HMQC, IR, HRESI-MS) the compound V1 is thus concluded to have ecdysteriod skeleton and conclusively conforms with 2β, 3β 14α, 20R, 22R, 25-hexahydroxy-5 β cholest-7-ene-6- one, or 2, 3, 14, 20, 22, 25 hexahydroxy cholest-7-ene-6-one commonly known as 20-hydroxyecdysone.

Keywords: vitex, phytochemical, purification, isolation, chromatography, spectroscopy

Procedia PDF Downloads 328

Authors: Kara J. Coffman-Rea, Karen E. Samonds

Abstract:

Microplastic pollution is an urgent global threat to our planet and human health. Microplastic particles have been detected within our food, water, and atmosphere, and found within the human stool, placenta, and lung tissue. However, most spectrometric microplastic detection methods require chemical digestion which can alter or destroy microplastic particles and makes it impossible to acquire information about their in-situ distribution. MALDI TOF MS (Matrix-assisted laser desorption ionization-time of flight mass spectrometry) is an analytical method using a soft ionization technique that can be used for polymer analysis. This method provides a valuable opportunity to both acquire information regarding the in-situ distribution of microplastics and also minimizes the destructive element of chemical digestion. In addition, MALDI TOF MS allows for expanded analysis of the microplastics including detection of specific additives that may be present within them. MALDI TOF MS is particularly sensitive to sample preparation and has not yet been used to analyze environmental microplastics within their specific location (e.g., biological tissues, sediment, water). In this study, microplastics were created using polyethylene gloves, polystyrene micro-foam, and polyethylene terephthalate cable sleeving. Plastics were frozen using liquid nitrogen and ground to obtain small fragments. An artificial tissue was created using a cellulose sponge as scaffolding coated with a MaxGel Extracellular Matrix to simulate human lung tissue. Optimal preparation techniques (e.g., matrix, cationization reagent, solvent, mixing ratio, laser intensity) were first established for each specific polymer type. The artificial tissue sample was subsequently spiked with microplastics, and specific polymers were detected using MALDI-TOF-MS. This study presents a novel method for the detection of environmental polyethylene, polyethylene terephthalate, and polystyrene microplastics within a complex sample. Results of this study provide an effective method that can be used in future microplastics research and can aid in determining the potential threats to environmental and human health that they pose.

Keywords: environmental plastic pollution, MALDI-TOF MS, microplastics, polymer identification

Procedia PDF Downloads 223

Authors: N. Chougui, R. Larbat

Abstract:

The first economic importance of Opuntia ficus-indica relies on the production of edible fruits. This food transformation generates a large amount of by-products (seeds and peels) in addition to cladodes produced by the plant. Several studies showed the richness of these products with bioactive substances like phenolics that have potential applications. Indeed, phenolics have been associated with protection against oxidation and several biological activities responsible of different pathologies. Consequently, there has been a growing interest in identifying natural antioxidants from plants. This study falls within the framework of the industrial exploitation of by-products of the plant. The study aims to investigate the metabolic profile of three by-products (cladodes, peel seeds) regarding total phenolic content by liquid chromatography coupled to mass spectrometry approach (LC-MSn). The byproducts were first washed, crushed and stored at negative temperature. The total phenolic compounds were then extracted by aqueous-ethanolic solvent in order to be quantified and characterized by LC-MS. According to the results obtained, the peel extract was the richest in phenolic compounds (1512.58 mg GAE/100 g DM) followed by the cladode extract (629.23 GAE/100 g DM) and finally by the seed extract (88.82 GAE/100 g DM) which is mainly used for its oil. The LC-MS analysis revealed diversity in phenolics in the three extracts and allowed the identification of hydroxybenzoic acids, hydroxycinnamic acids and flavonoids. The highest complexity was observed in the seed phenolic composition; more than twenty compounds were detected that belong to acids esters among which three feruloyl sucrose isomers. Sixteen compounds belonging to hydroxybenzoic acids, hydroxycinnamic acids and flavonoids were identified in the peel extract, whereas, only nine compounds were found in the cladode extract. It is interesting to highlight that the phenolic composition of the cladode extract was closer to that of the peel exact. However, from a quantitative viewpoint, the peel extract presented the highest amounts. Piscidic and eucomic acids were the two most concentrated molecules, corresponding to 271.3 and 121.6 mg GAE/ 100g DM respectively. The identified compounds were known to have high antioxidant and antiradical potential with the ability to inhibit lipid peroxidation and to exhibit a wide range of biological and therapeutic properties. The findings highlight the importance of using the Opuntia ficus-indica by-products.

Keywords: characterization, LC-MSn analysis, Opuntia ficus-indica, phenolics

Procedia PDF Downloads 207

Authors: Azziz Assoumani, Francois Lestremau, Celine Ferret, Benedicte Lepot, Morgane Salomon, Helene Budzinski, Marie-Helene Devier, Pierre Labadie, Karyn Le Menach, Patrick Pardon, Laure Wiest, Emmanuelle Vulliet, Pierre-Francois Staub

Abstract:

Seven French wastewater treatment plants (WWTP) were monitored for 53 contaminants of emerging concern within a nation-wide monitoring campaign in surface waters, which took place in 2018. The overall objective of the 2018 campaign was to provide the exercise of prioritization of emerging substances, which is being carried out in 2021, with monitoring data. This exercise should make it possible to update the list of relevant substances to be monitored (SPAS) as part of future water framework directive monitoring programmes, which will be implemented in the next water body management cycle (2022). One sampling campaign was performed in October 2018 in the seven WWTP, where affluent and sludge samples were collected. Surface water samples were collected in September 2018 at three to five sites upstream and downstream the point of effluent discharge of each WWTP. The contaminants (36 biocides and 17 surfactants, selected by the Prioritization Experts Committee) were determined in the seven WWTP effluent and sludge samples and in surface water samples by liquid or gas chromatography coupled with tandem mass spectrometry, depending on the contaminant. Nine surfactants and three biocides were quantified at least in one WWTP effluent sample. Linear alkylbenzene sulfonic acids (LAS) and fipronil were quantified in all samples; the LAS were quantified at the highest median concentrations. Twelve surfactants and 13 biocides were quantified in at least one sludge sample. The LAS and didecyldimethylammonium were quantified in all samples and at the highest median concentrations. Higher concentration levels of the substances quantified in WWTP effluent samples were observed in the surface water samples collected downstream the effluents discharge points, compared with the samples collected upstream, suggesting a contribution of the WWTP effluents in the contamination of surface waters.

Keywords: contaminants of emerging concern, effluent, monitoring, river water, sludge

Procedia PDF Downloads 118