Search results for: size exclusion chromatography

Authors: Ambika Selvaraj

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Magnetic iron oxide nanoparticles (IO) of < 20nm (superparamagnetic) become promising tool in cancer therapy, and integrated nanodevices for cancer detection and screening. The obstacles include particle heterogeneity and cost. It can be overcome by developing monodispersed nanoparticles in economical approach. We have successfully synthesized < 7 nm IO by low temperature controlled technique, in which Fe0 is sandwiched between stabilizer and Fe2+. Size analysis showed the excellent size control from 31 nm at 33°C to 6.8 nm at 10°C. Resultant monodispersed IO were found to be stable for > 50 reuses, proved its applicability in biomedical applications.

Keywords: low temperature synthesis, hybrid iron nanoparticles, cancer therapy, biomedical applications

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Authors: Mohamed Izzharif Abdul Halim, Niamh Nic Daeid

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Determining the source of pen inks used on a variety of documents is impartial for forensic document examiners. The examination of inks is often performed to differentiate between inks in order to evaluate the authenticity of a document. A ballpoint pen ink consists of synthetic dyes in (acidic and/or basic), pigments (organic and/or inorganic) and a range of additives. Inks of similar color may consist of different composition and are frequently the subjects of forensic examinations. This study emphasizes on blue ballpoint pen inks available in the market because it is reported that approximately 80% of questioned documents analysis involving ballpoint pen ink. Analytical techniques such as thin layer chromatography, high-performance liquid chromatography, UV-vis spectroscopy, luminescence spectroscopy and infrared spectroscopy have been used in the analysis of ink samples. In this study, application of Diamond Attenuated Total Reflectance (ATR) FTIR is straightforward but preferable in forensic science as it offers no sample preparation and minimal analysis time. The data obtained from these techniques were further analyzed using multivariate chemometric methods which enable extraction of more information based on the similarities and differences among samples in a dataset. It was indicated that some pens from the same manufactures can be similar in composition, however, discrete types can be significantly different.

Keywords: ATR FTIR, ballpoint, multivariate chemometric, PCA

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Authors: Humara Bano, Nyla Anjum

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Disability in any form has great impact not only for the person facing it but also for its family members too. This effect may be so severe that may lead to mal adjustment of any member of the family in society as well. This impact has also been multiplied due to negative attitudes of the society, unawareness about the needs of special needs and no legislation for the parents of children with special needs. As a result not only the separations among the parents have been reported but also the normal siblings in the home are also badly affected in their daily lives. The situation is more challenging when more than one child with disability is present in the family. The main objectives of this paper are to unfold the relationship of variety of disabilities (hearing, visual or physical impairment, mental retardation, speech impairment) in i) developing depression in home setting, ii) social exclusion, iii) anxiety and aggression and iv) development of insecure feelings among family members of the persons with disabilities, as well as, v) to identify coping strategies to manage the special needs by family members too. To reach on conclusion about fifty families (having any sort of disability in their homes) have been interviewed on basis of convenient sampling. Correlation, ANOVA and different analysis have been used to identify the relationship of disability in developing depression among family members in line of above mentioned problems. Results revealed that depression due to disability among families is a common phenomenon and adversely have affected their lives in daily routines as well as in following their life achievements. Coping with the situation and recommending various remedies by parents is the positive reflection of this study too that can help to families in managing their mental health.

Keywords: depression, anxiety and aggression, social exclusion, parents of children with special needs

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Authors: Asmaa Mandour, Ramzia El-Bagary, Asmaa El-Zaher, Ehab Elkady

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Background: An UHPLC (ultra high performance liquid chromatography) method for the simultaneous determination of norfloxacin (NOR), metronidazole (MET) and tinidazole (TNZ) using monolithic column is presented. Purpose: The method is considered an environmentally friendly method with relatively low organic composition of the mobile phase. Methods: The chromatographic separation was performed using Phenomenex® Onyex Monolithic C18 (50mmx 20mm) column. An elution program of mobile phase consisted of 0.5% aqueous phosphoric acid : methanol (85:15, v/v). Where elution of all drugs was completed within 3.5 min with 1µL injection volume. The UHPLC method was applied for the stability indication of NOR in the presence of its acid degradation product ND. Results: Retention times were 0.69, 1.19 and 3.23 min for MET, TNZ and NOR, respectively. While ND retention time was 1.06 min. Linearity, accuracy, and precision were acceptable over the concentration range of 5-50µg mL-1for all drugs. Conclusions: The method is simple, sensitive and suitable for the routine quality control and dosage form assay of the three drugs and can also be used for the stability indication of NOR in the presence of its acid degradation product.

Keywords: antibacterial, monolithic cilumn, simultaneous determination, UHPLC

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Authors: Subhan Ahmad, Pradeep Bhargava, Ajay Chourasia

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Shear failure in reinforced concrete beams without shear reinforcement leads to loss of property and life since a very little or no warning occurs before failure as in case of flexural failure. Shear strength of reinforced concrete beams decreases as its depth increases. This phenomenon is generally called as the size effect. In this paper, a comparative analysis is performed to estimate the performance of shear strength models in capturing the size effect of reinforced concrete beams made with conventional concrete, self-compacting concrete, and recycled aggregate concrete. Four shear strength models that account for the size effect in shear are selected from the literature and applied on the datasets of slender reinforced concrete beams. Beams prepared with conventional concrete, self-compacting concrete, and recycled aggregate concrete are considered for the analysis. Results showed that all the four models captured the size effect in shear effectively and produced conservative estimates of the shear strength for beams made with normal strength conventional concrete. These models yielded unconservative estimates for high strength conventional concrete beams with larger effective depths ( > 450 mm). Model of Bazant and Kim (1984) captured the size effect precisely and produced conservative estimates of shear strength of self-compacting concrete beams at all the effective depths. Also, shear strength models considered in this study produced unconservative estimates of shear strength for recycled aggregate concrete beams at all effective depths.

Keywords: reinforced concrete beams; shear strength; prediction models; size effect

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Authors: Sultan Husein Bayqra, Ali Mardani Aghabaglou, Zia Ahmad Faqiri, Hassane Amidou Ouedraogo

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In this study, the effect of shape and size of the concrete specimen on the compressive and splitting tensile strength of the concrete mixtures in the absence and presence of steel fiber was investigated. For this aim, ten different concrete mixtures having w/c ratio of 0.3, 0.4, 0.5, 0.6 and 0.7 with and without fiber were prepared. In the mixtures containing steel fibers having aspect ratio (L/D) of 64 were used by 1% of the total mixture volume. In all concrete mixtures, CEM I 42,5R type Portland cement and crushed Lime-stone aggregates having different aggregate size fractions were used. The combined aggregate was obtained by mixing %40 0-5 mm, %30 5-12 mm and %30 12-22 mm aggregate size fraction. The slump values of concrete mixtures were kept constant as 17 ± 2 cm. To provide the desired slump value, a polycarboxylate ether-based high range water reducing admixture was used. In order to investigate the effect of size and shape of concrete specimen on strength properties 10 cm, 15 cm cubic specimens and 10×20 cm, 15×30 cm cylindrical specimens were prepared for each mixture. The specimens were cured under standard conditions until testing days. The 7- and 28-day compressive and splitting tensile strengths of mixtures were determined. The results obtained from the experimental study showed that the strength ratio between the cylinder and the cube specimens increased with the increase of the strength of the concrete. Regardless of the fiber utilization and specimen shape, strength values of concrete mixtures were increased by decreasing specimen size. However, the mentioned behaviour was not observed for the case that the mixtures having high W/C ratio and containing fiber. The compressive strength of cube specimens containing fiber was less affected by the size of the specimen compared to that of cube specimens containing no fibers.

Keywords: compressive strength, splitting tensile strength, fiber reinforced concrete, size effect, shape effect

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Authors: O. E. Ogunjinmi, N. O. Olawore, L. A. Usman, S. O. Ogunjinmi

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An essential oil is any concentrated, hydrophobic liquid containing volatile aroma compounds produced by plants. It has been established that several factors affect the component of the plants such as the texture of the soil, relative humidity, wind, and collection time. This study is aimed at investigating the effect of collection time on the chemical composition of this essential oil. Pulverized leaves (500 g) of Hoslundia opposite harvested in the morning (7 am) and afternoon (2 pm) of the same day were separately hydrodistilled using Clevenger apparatus to obtain the essential oils from the leaves. The leaf oils collected in the morning (7 am) and afternoon (2 pm) harvests yielded 0.54 and 0.65 %w/w respectively. Analysis of the leaf oil obtained in the morning, using gas chromatography (GC) and gas chromatography combined mass spectrometry (GC-MS) revealed the presence of twenty-three (23) compounds which made up 81.8% of the total oil while nineteen (19) compounds (93.2%) were identified in the afternoon leaf essential oil. The most abundant components of the leaf oil collected in the morning (7 am) harvest were p-cymene (28.7%), sabinene (7.1%) and 1,8-cineole (6.6%) Meanwhile the major components of leaf oil in the afternoon (2 pm) harvest were p-cymene (26.4%), thymol (15.3%), 1,8-cineole (15.0%) and g-terpinene (10.4%). The composition pattern of leaf oil obtained in the morning and afternoon harvests of Hoslundia opposite revealed significant differences in qualitative and quantitative.

Keywords: essential oil, Hoslundia opposita, para cymene, 1, 8-cineole

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Authors: Mike Dee

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Urban public spaces are sutured with a range of surveillance and sensor technologies that claim to enable new forms of ‘data based citizen participation’, but also increase the tendency for ‘function-creep’, whereby vast amounts of data are gathered, stored and analysed in a broad application of urban surveillance. This kind of monitoring and capacity for surveillance connects with attempts by civic authorities to regulate, restrict, rebrand and reframe urban public spaces. A direct consequence of the increasingly security driven, policed, privatised and surveilled nature of public space is the exclusion or ‘unfavourable inclusion’ of those considered flawed and unwelcome in the ‘spectacular’ consumption spaces of many major urban centres. In the name of urban regeneration, programs of securitisation, ‘gentrification’ and ‘creative’ and ‘smart’ city initiatives refashion public space as sites of selective inclusion and exclusion. In this context of monitoring and control procedures, in particular, children and young people’s use of space in parks, neighbourhoods, shopping malls and streets is often viewed as a threat to the social order, requiring various forms of remedial action. This paper suggests that cities, places and spaces and those who seek to use them, can be resilient in working to maintain and extend democratic freedoms and processes enshrined in Marshall’s concept of citizenship, calling sensor and surveillance systems to account. Such accountability could better inform the implementation of public policy around the design, build and governance of public space and also understandings of urban citizenship in the sensor saturated urban environment.

Keywords: citizenship, public space, surveillance, young people

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

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

Keywords: anti-cancer, Hela cancer cell, MDA-Md-231 cancer cell, Virgularia gustavina

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Authors: Mulatu Kassie Birhanu

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Electro-oxidation of glycerol is an important process to convert the less price glycerol into other expensive (essential) and energy-rich chemicals. In this study, nickel was electro-deposited on laboratory-made carbon ceramic electrode (CCE) substrate using electrochemical techniques that is cyclic voltammetry (CV) to prepare an electro-catalyst (Ni/CCE) for electro-oxidation of glycerol. Carbon ceramic electrode was prepared from graphite and methyl tri-methoxy silane (MTMOS) through the processes called hydrolysis and condensation with methanol in acidic media (HCl) by a sol-gel technique. Physico-chemical characterization of bare CCE and modified (deposited) CCE (Ni/CCE) was measured and evaluated by Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). Electro-oxidation of glycerol was performed in 0.1 M glycerol in alkaline media (0.5 M NaOH). High-Performance Liquid Chromatography (HPLC) technique was used to identify and determine the concentration of glycerol, reaction intermediates and oxidized products of glycerol after its electro-oxidation is performed. The conversion (%) of electro-oxidation of glycerol during 9-hour oxidation was 73% and 36% at 1.8V and 1.6V vs. RHE, respectively. Formate, oxalate, glycolate and glycerate are the main oxidation products of glycerol with selectivity (%) of 75%, 8.6%, 1.1% and 0.95 % at 1.8 V vs. RHE and 55.4%, 2.2%, 1.0% and 0.6% at 1.6 V vs. RHE respectively. The result indicates that formate is the main product in the electro-oxidation of glycerol on Ni/CCE using the indicated applied potentials.

Keywords: carbon-ceramic electrode, electrodeposition, electro-oxidation, Methyltrimethoxysilane

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Authors: George Madalin Danila, Mihaiella Cretu, Cristian Puscasu

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Glycol-based anti-freeze liquids, commonly composed of ethylene glycol or propylene glycol, have important uses in automotive cooling, but they should be handled with care due to their toxicity; ethylene glycol is highly toxic to humans and animals. A fast, accurate, precise, and robust method was developed for the simultaneous quantification of 7 most important glycols and their isomers. Glycols were analyzed from diluted sample solution of coolants using gas-chromatography coupled with mass spectrometry in single ion monitoring mode. Results: The method was developed and validated for 7 individual glycols (ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, dipropylene glycol and tripropylene glycol). Limits of detection (1-2 μg/mL) and limit of quantification (10 μg/mL) obtained were appropriate. The present method was applied for the determination of glycols in 10 different anti-freeze liquids commercially available on the Romanian market, proving to be reliable. A method that requires only a two-step dilution of anti-freeze samples combined with direct liquid injection GC-MS was validated for the simultaneous quantification of 7 glycols (and their isomers) in 10 different types of anti-freeze liquids. The results obtained in the validation procedure proved that the GC-MS method is sensitive and precise for the quantification of glycols.

Keywords: glycols, anti-freeze, gas-chromatography, mass spectrometry, validation, recycle

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Authors: Sivapan Choo-In

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This research aims to study the Zinc (Zn) concentration in fine particulate matter on Rajchawithee roadside in rush hour. 30 Samples were collected in Jun to August 2013 by 8 stage non-avaible cascade impactor. Each samples (filter paper) were digest with nitric acid and analyed by atomic absorption spectrophotometer for Zinc determination. The highest value for the mean fraction (18.00 ± 9.28 %) is the size 9.0 – 110.0 micron follow by the range 3.3 – 4.7 micron (14.77 ± 14.66 %) and 1.1 – 2.1 micron (14.01 ± 11.77 %) .The concentration of Zn in the particulate matter of range 0.43 – 0.7 μm, 0.7 – 1.1 μm, 1.1 – 2.1 μm, 2.1 – 3.3 μm, 3.3 – 4.7 μm, 4.7 – 5.8 μm, 5.8 – 9.0 μm, 9.0 – 10.0 μm, were 41.56 – 217.62 μg/m3 (175.86 ± 32.25 μg/m3), 152.60 – 217.24 μg/m3 (187.71 ± 17.42 μg/m3), 142.90 – 214.67 μg/m3 (180.95 ± 18.71 μg/m3), 155.48 – 218.19 μg/m3 (183.22 ± 19.94 μg/m3), 151.72 – 217.39 μg/m3 (181.85 ± 17.57 μg/m3), 133.86 – 220.17 μg/m3 (178.78 ± 23.45 μg/m3), 160.00 – 220.35 μg/m3 (182.58 ± 18.08 μg/m3), 153.30 – 226.70 μg/m3 (181.52 ± 20.05 μg/m3), repectively. The Zn concentration in each size of particulate matter was not statistically significant different (p > .005)

Keywords: air pollution, particulate matter, size distribution, zinc

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Authors: R. Marandi, H. Shahrir, T. Nejad Ghaffar Borhani, M. Kamaruddin

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In the present study, a steady state population balance model was developed to predict the polymer particle size distribution (PSD) in ethylene gas phase fluidized bed olefin polymerization reactors. The multilayer polymeric flow model (MPFM) was used to calculate the growth rate of a single polymer particle under intra-heat and mass transfer resistance. The industrial plant data were used to calculate the growth rate of polymer particle and the polymer PSD. Numerical simulations carried out to describe the influence of effective monomer diffusion coefficient, polymerization rate and initial catalyst size on the catalyst particle growth and final polymer PSD. The results present that the intra-heat and mass limitation is important for the ethylene polymerization, the growth rate of particle and the polymer PSD in the fluidized bed reactor. The effect of the agglomeration on the PSD is also considered. The result presents that the polymer particle size distribution becomes broader as the agglomeration exits.

Keywords: population balance, olefin polymerization, fluidized bed reactor, particle size distribution, agglomeration

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Authors: Abdelkader Nouri, M’hamed Bouslama, Faouzi Saidi, Hassan Maaref, Michel Gendry

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Self-organized InAs quantum dots (QDs) have been grown on 3,1% InP (110) lattice mismatched substrate by Solid Source Molecular Beam Epitaxy (SSMBE). Stranski-Krastanov mode growth has been used to create self-assembled 3D islands on InAs wetting layer (WL). The optical quality depending on the temperature and power is evaluated. In addition, Atomic Force Microscopy (AFM) images shows inhomogeneous island dots size distribution due to temperature coalescence. The quantum size effect was clearly observed through the spectra photoluminescence (PL) shape.

Keywords: AFM, InAs QDs, PL, SSMBE

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Authors: Stella Sten, Peter Hedström, Joakim Odqvist, Susanne Norgren

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Two functionally graded cemented carbide samples have been produced by local addition of Titanium carbide (TiC) to a pressed Tungsten carbide and Cobalt, WC-10 wt% Co, green body prior to sintering, with the aim of creating a gradient in both composition and grain size in the as-sintered component. The two samples differ only by the in-going WC particle size, where one sub-micron and one coarse WC particle size have been chosen for comparison. The produced sintered samples had a gradient, thus a non-homogenous structure. The Titanium (Ti), Cobalt (Co), and Carbon (C) concentration profiles have been investigated using SEM-EDS and WDS; in addition, the Vickers hardness profile has been measured. Moreover, the Ti concentration profile has been simulated using DICTRA software and compared with experimental results. The concentration and hardness profiles show a similar trend for both samples. Ti and C levels decrease, as expected from the area of TiC application, whereas Co increases towards the edge of the samples. The non-homogenous composition affects the number of stable phases and WC grain size evolution. The sample with finer in-going WC grain size shows a shorter gamma (γ) phase zone and a larger difference in WC grain size compared to the coarse-grained sample. Both samples show, independent of the composition, the presence of abnormally large grains.

Keywords: cemented carbide, functional gradient material, grain growth, sintering

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Authors: Yao-Te Yen, Chao-Hsin Cheng, Meng-Shun Huang, Shan-Zong Cyue

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'Poppy-seed defense' has been a serious problem all over the world, that is because the opiates metabolites in urine are difficult to distinguish where they come from precisely. In this research, a powerful analytic method has been developed to trace the opiates metabolites in urine by Gas-Chromatography Isotope Ratio Mass Spectrometry (GC-IRMS). In order to eliminate the interference of synthesis to heroin or metabolism through human body, opiates metabolites in urine and sized heroin were hydrolyzed to morphine. Morphine is the key compound for tracing between opiates metabolites and seized heroin in this research. By matching δ13C and δ15N values through morphine, it is successful to distinguish the opiates metabolites coming from heroin or medicine. We tested seven heroin abuser’s metabolites and seized heroin in crime sites, the result showed that opiates metabolites coming from seized heroin, the variation of δ13C and δ15N for morphine are within 0.2 and 2.5‰, respectively. The variation of δ13C and δ15N for morphine are reasonable with the result of matrix match experiments. Above all, the uncertainty of 'Poppy-seed defense' can be solved easily by this analytic method, it provides the direct evidence for judge to make accurate conviction without hesitation.

Keywords: poppy-seed defense, heroin, opiates metabolites, isotope ratio mass spectrometry

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Authors: Shahriar Ghammamy, Maryam Gholipoor

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Metronidazole nano -powders with the average mean particle size around 90 nm were synthesized by high-energy milling using a planetary ball mill is provided. The Scattering factors, milling of time,the ball size and ball to powder ratio on the material properties powder by the Ray diffraction (XRD) study, scanning electron microscopy (SEM), IR. It has been observed that the density of nano-sized grinding balls as ball to powder ratio depends. Using the dispersion factor, the density Can be reduced below the initial particle size was achieved.

Keywords: metronidazole, ball-milling, nanoparticles, characterization, XRD diffraction

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Authors: Taufik Hidayat, Yudha Nurhantari, Bambang U. D. Rianto

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Introduction: The examination of the Short Tandem Repeats (STR) locus on nuclear DNA is very useful in solving the paternity cases. The purpose of this study is to know the description of paternity cases and paternity index/probability of paternity analysis based on Indonesian allele frequency at Sardjito Hospital Yogyakarta. Method: This was an observational study with cross-sectional analytic method. Population and sample were all cases of disputed paternity from January 2011 to June 2015 that fulfill the inclusion and exclusion criteria and were examined at Forensic Medicine Unit of Sardjito Hospital, Medical Faculty of Gadjah Mada University. The paternity index was calculated with EasyDNA Program by Fung (2013). Analysis of the study was conducted by comparing the results through unpaired categorical test using Kolmogorov-Smirnov test. This study was designed with 95% confidence interval (CI) with α = 5% and significance level is p < 0,05. Results: From 42 disputed paternity cases we obtained trio paternity cases were 32 cases (76.2%) and duo without a mother was 10 cases (23.8%). The majority of the fathers' estimated ages were 21-30 years (33.3%) and the mother's age was 31-40 years (38.1%). The majority of the ages of children examined for paternity were under 12 months (47.6%). The majority of ethnic clients are Javanese. Conclusion of inclusion was 57.1%, and exclusion was 42.9%. The Kolmogorov-Smirnov test obtained p-value = 0.673. Conclusion: There is no significant difference between paternity index/probability of paternity based on Indonesian allele frequency between trio and duo of paternity.

Keywords: disputed paternity, paternity index, probability of paternity, short tandem

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Authors: Sujatha Edla

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Introduction: New compounds and possible uses for the bioactive substances produced by freshwater cyanobacteria are constantly being discovered through research. Certain molecules are hazardous to the environment and human health, but others have potential applications in industry, biotechnology, and pharmaceuticals. These discoveries advance our knowledge of the varied functions these microbes perform in different ecosystems. Cyanobacterial silver nanoparticles (AgNPs) have special qualities and possible therapeutic advantages, which make them very promising for a range of medicinal uses. Aim: In our study; the attention was focused on the analysis and characterization of bioactive compounds extracted from freshwater cyanobacteria Planktothricoides raciorskii and its comparative study on Cyanobacteria-mediated silver nanoparticles synthesized by cell-free extract of Planktothricoides raciorskii. Material and Methods: A variety of bioactive secondary metabolites have been extracted, purified, and identified from cyanobacterial species using column chromatography, FTIR, and GC-MS/MS chromatography techniques and evaluated for antibacterial and cytotoxic studies, where the Cyanobacterial silver nanoparticles (CSNPs) were characterized by UV-Vis spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) analysis and were further tested for antibacterial and cytotoxic efficiency. Results: The synthesis of CSNPs was confirmed through visible color change and shift of peaks at 430–445 nm by UV-Vis spectroscopy. The size of CSNPs was between 22 and 34 nm and oval-shaped which were confirmed by SEM and TEM analyses. The FTIR spectra showed a new peak at the range of 3,400–3,460 cm−1 compared to the control, confirming the reduction of silver nitrate. The antibacterial activity of both crude bioactive compound extract and CSNPs showed remarkable activity with Zone of inhibition against E. coli with 9.5mm and 10.2mm, 13mm and 14.5mm against S. paratyphi, 9.2mm and 9.8mm zone of inhibition against K. pneumonia by both crude extract and CSNPs, respectively. The cytotoxicity as evaluated by extracts of Planktothricoides raciorskii against MCF7-Human Breast Adenocarcinoma cell line and HepG2- Human Hepatocellular Carcinoma cell line employing MTT assay gave IC50 value of 47.18ug/ml, 110.81ug/ml against MCF7cell line and HepG2 cell line, respectively. The cytotoxic evaluation of Planktothricoides raciorskii CSNPs against the MCF7cell line was 43.37 ug/ml and 20.88 ug/ml against the HepG2 cell line. Our ongoing research in this field aims to uncover the full therapeutic potential of cyanobacterial silver nanoparticles and address any associated challenges.

Keywords: cyanobacteria, silvernanoparticles, pharmaceuticals, bioactive compounds, cytotoxic

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Authors: Gui Yang Wu, Bo Wang, Xin Wang

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Nowadays, 5G service-based interface architecture uses text-based payload like JSON to transfer business data between network functions, which has obvious advantages as internet services but causes unnecessarily larger traffic. In this paper, a new 5G application payload size reduction method is presented to provides the mechanism to negotiate about new capability between network functions when network communication starts up and how 5G application data are reduced according to negotiated information with peer network function. Without losing the advantages of 5G text-based payload, this method demonstrates an excellent result on application payload size reduction and does not increase the usage quota of computing resource. Implementation of this method does not impact any standards or specifications and not change any encoding or decoding functionality too. In a real 5G network, this method will contribute to network efficiency and eventually save considerable computing resources.

Keywords: 5G, JSON, payload size, service-based interface

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Authors: H. Abdolvand, M. Riazat, H. Sohrabi, G. Faraji

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An experimental investigation into the Tube Backward Extrusion (TBE) process on AZ31 magnesium alloy is studied. Microstructures and grain size distribution of the specimens before and after TBE process are investigated by optical microscopy. Tensile and Vickers microhardness tests along extrusion direction were performed at room temperature. It is found that the average grain size is refined remarkably from the initial 33 µm down to 3.5 µm after TBE process. Also, the microhardness increased significantly to 58 HV after the process from an initial value of 36 HV.

Keywords: tube backward extrusion, AZ31, grain size distribution, grain refinement

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Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

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Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

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Authors: He Yuhai, Ahmad Ziad Bin Sulaiman

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Tongkat Ali, or Eurycoma longifolia, is a traditional Malay and Orang Asli herb used as aphrodisiac, general tonic, anti-Malaria, and anti-Pyretic. It has been recognized as a cashcrop by Malaysia due to its high value for the pharmaceutical use. In Tongkat Ali, eurycomanone, a quassinoid is usually chosen as a marker phytochemical as it is the most abundant phytochemical. In this research, ultrasound and enzyme were used to enhance the extraction of Eurycomanone from Tongkat Ali. Ultrasonic assisted extraction (USE) enhances extraction by facilitating the swelling and hydration of the plant material, enlarging the plant pores, breaking the plant cell, reducing the plant particle size and creating cavitation bubbles that enhance mass transfer in both the washing and diffusion phase of extraction. Enzyme hydrolyses the cell wall of the plant, loosening the structure of the cell wall, releasing more phytochemicals from the plant cell, enhancing the productivity of the extraction. Possible effects of ultrasound on the activity of the enzyme during the hydrolysis of the cell wall is under the investigation by this research. The extracts was analysed by high performance liquid chromatography for the yields of Eurycomanone. In this whole process, the conventional water extraction was used as a control of comparing the performance of the ultrasound and enzyme assisted extraction.

Keywords: ultrasound, enzymatic, extraction, Eurycoma longifolia

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Authors: Samy Selim

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Natural products are still major sources of innovative therapeutic agents for various conditions, including infectious diseases. Peganum harmala L. oil had wide range uses as traditional medicinal plants. The current study was designed to evaluate the antibacterial activity of P. harmala essential oil. The chemical constitutes and toxicity of these oils was also determined to obtain further information on the correlation between the chemical contents and antibacterial activity. The antibacterial effect of the essential oils of P. harmala oil was studied against some foodborne pathogenic bacteria species. The oil of plant was subjected to gas chromatography-mass spectrometry (GC/MS). The impact of oils administration on the change in rate of weight gain and complete blood picture in hamsters were investigated. P. harmala oil had strong antibacterial effect against bacterial species especially at minimum inhibitory concentration (MIC) less than 75.0 μg/ml. From the oil of P. harmala, forty one compounds were identified, and the major constituent was 1-hexyl-2-nitrocyclohexane (9.07%). Acute toxicity test was performed on hamsters and showed complete survival after 14 days, and there were no toxicity symptoms occurred. This study demonstrated that these essential oils seemed to be destitute of toxic effect which could compromise the medicinal use of these plants in folk medicine.

Keywords: analysis mass spectrometry, antibacterial activities, acute toxicity, chemical constitutes, gas chromatography, weight gain, Peganum harmala

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

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

Keywords: alcohol dehydrogenases, DES, gas chromatography, RasADH

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Authors: Renata Gerhardt, Detlev Belder

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Raman spectroscopy has attracted much attention as a structurally descriptive and label-free detection method. It is particularly suited for chemical analysis given as it is non-destructive and molecules can be identified via the fingerprint region of the spectra. In this work possibilities are investigated how to integrate Raman spectroscopy as a detection method for chip-based chromatography, making use of a droplet interface. A demanding task in lab-on-a-chip applications is the specific and sensitive detection of low concentrated analytes in small volumes. Fluorescence detection is frequently utilized but restricted to fluorescent molecules. Furthermore, no structural information is provided. Another often applied technique is mass spectrometry which enables the identification of molecules based on their mass to charge ratio. Additionally, the obtained fragmentation pattern gives insight into the chemical structure. However, it is only applicable as an end-of-the-line detection because analytes are destroyed during measurements. In contrast to mass spectrometry, Raman spectroscopy can be applied on-chip and substances can be processed further downstream after detection. A major drawback of Raman spectroscopy is the inherent weakness of the Raman signal, which is due to the small cross-sections associated with the scattering process. Enhancement techniques, such as surface enhanced Raman spectroscopy (SERS), are employed to overcome the poor sensitivity even allowing detection on a single molecule level. In SERS measurements, Raman signal intensity is improved by several orders of magnitude if the analyte is in close proximity to nanostructured metal surfaces or nanoparticles. The main gain of lab-on-a-chip technology is the building block-like ability to seamlessly integrate different functionalities, such as synthesis, separation, derivatization and detection on a single device. We intend to utilize this powerful toolbox to realize Raman detection in chip-based chromatography. By interfacing on-chip separations with a droplet generator, the separated analytes are encapsulated into numerous discrete containers. These droplets can then be injected with a silver nanoparticle solution and investigated via Raman spectroscopy. Droplet microfluidics is a sub-discipline of microfluidics which instead of a continuous flow operates with the segmented flow. Segmented flow is created by merging two immiscible phases (usually an aqueous phase and oil) thus forming small discrete volumes of one phase in the carrier phase. The study surveys different chip designs to realize coupling of chip-based chromatography with droplet microfluidics. With regards to maintaining a sufficient flow rate for chromatographic separation and ensuring stable eluent flow over the column different flow rates of eluent and oil phase are tested. Furthermore, the detection of analytes in droplets with surface enhanced Raman spectroscopy is examined. The compartmentalization of separated compounds preserves the analytical resolution since the continuous phase restricts dispersion between the droplets. The droplets are ideal vessels for the insertion of silver colloids thus making use of the surface enhancement effect and improving the sensitivity of the detection. The long-term goal of this work is the first realization of coupling chip based chromatography with droplets microfluidics to employ surface enhanced Raman spectroscopy as means of detection.

Keywords: chip-based separation, chip LC, droplets, Raman spectroscopy, SERS

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Authors: Emily Adams, Eddie Donaghy, David Henderson, Lauren Ng, Caroline Sanders, Rowena Stewart, Maria Wolters, Stewart Mercer

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Ongoing review abstract: Older People Experiencing Homelessness (OPEH) can have mental and physical indicators of aging 10–20 years earlier than the general population and experience premature mortality due to age-related chronic conditions. Emerging literature suggests digital interventions could positively impact PEH’s well-being. However, the increased reliance on digital delivery may also perpetuate digital inequalities for socially excluded groups, including PEH. The potential triple disadvantage of being older, homeless, and digitally excluded creates a uniquely problematic situation that warrants further research. This scoping review aims to investigate and synthesise the range and type of digital interventions available to OPEH and the organisations that support OPEH. The following databases were searched on 28th July 2023: Medline, Scopus, International Bibliography of the Social Sciences (IBSS)‎, Applied Social Sciences Index & Abstracts (ASSIA)‎, Association for Computing Machinery Digital Library (ACMDL) and Policy commons. A search strategy was developed in collaboration with an academic librarian. The presentation will include: An introduction to OPEH and digital exclusion Overview of the results of this review: OPEH usage of digital platforms Current digital interventions available The role of support organisations Current gaps in the evidence, future research and recommendations for policy and practice

Keywords: homeless, digital exclusion, aging, technology

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Authors: Sanja Podunavac-Kuzmanović, Strahinja Kovačević, Lidija Jevrić, Evgenija Djurendić, Jovana Ajduković

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There are several methods for determination of the lipophilicity of biologically active compounds, however chromatography has been shown as a very suitable method for this purpose. Chromatographic (C18-RP-HPLC) analysis of a series of 24 17-picolyl and 17-picolinylidene androstane derivatives was carried out. The obtained retention indices (logk, methanol (90%) / water (10%)) were correlated with calculated physicochemical and lipophilicity descriptors. The QSRR analysis was carried out applying principal component regression (PCR) and partial least squares regression (PLS). The PCR and PLS model were selected on the basis of the highest variance and the lowest root mean square error of cross-validation. The obtained PCR and PLS model successfully correlate the calculated molecular descriptors with logk parameter indicating the significance of the lipophilicity of compounds in chromatographic process. On the basis of the obtained results it can be concluded that the obtained logk parameters of the analyzed androstane derivatives can be considered as their chromatographic lipophilicity. These results are the part of the project No. 114-451-347/2015-02, financially supported by the Provincial Secretariat for Science and Technological Development of Vojvodina and CMST COST Action CM1105.

Keywords: androstane derivatives, chromatography, molecular structure, principal component regression, partial least squares regression

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Authors: Nikola Toshikj, Michel Ramonda, Sylvain Catrouillet, Jean-Jacques Robin, Sebastien Blanquer

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Biodegradable and biocompatible block copolymers have risen as the golden materials in both medical and environmental applications. Moreover, if their architecture is of controlled manner, higher applications can be foreseen. In the meantime, organocatalytic ROP has been promoted as more rapid and immaculate route, compared to the traditional organometallic catalysis, towards efficient synthesis of block copolymer architectures. Therefore, herein we report novel organocatalytic pathway with guanidine molecules (TBD) for supported synthesis of trimethylene carbonate initiated by poly(caprolactone) as pre-polymer. Pristine PTMC-b-PCL-b-PTMC block copolymer structure, without any residual products and clear desired block proportions, was achieved under 1.5 hours at room temperature and verified by NMR spectroscopies and size-exclusion chromatography. Besides, when elaborating block copolymer films, further stability and amelioration of mechanical properties can be achieved via additional reticulation step of precedently methacrylated block copolymers. Subsequently, stimulated by the insufficient studies on the phase-separation/crystallinity relationship in these semi-crystalline block copolymer systems, their intrinsic thermal and morphology properties were investigated by differential scanning calorimetry and atomic force microscopy. Firstly, by DSC measurements, the block copolymers with χABN values superior to 20 presented two distinct glass transition temperatures, close to the ones of the respecting homopolymers, demonstrating an initial indication of a phase-separated system. In the interim, the existence of the crystalline phase was supported by the presence of melting temperature. As expected, the crystallinity driven phase-separated morphology predominated in the AFM analysis of the block copolymers. Neither crosslinking at melted state, hence creation of a dense polymer network, disturbed the crystallinity phenomena. However, the later revealed as sensible to rapid liquid nitrogen quenching directly from the melted state. Therefore, AFM analysis of liquid nitrogen quenched and crosslinked block copolymer films demonstrated a thermodynamically driven phase-separation clearly predominating over the originally crystalline one. These AFM films remained stable with their morphology unchanged even after 4 months at room temperature. However, as demonstrated by DSC analysis once rising the temperature above the melting temperature of the PCL block, neither the crosslinking nor the liquid nitrogen quenching shattered the semi-crystalline network, while the access to thermodynamical phase-separated structures was possible for temperatures under the poly (caprolactone) melting point. Precisely this coexistence of dual crosslinked/crystalline networks in the same copolymer structure allowed us to establish, for the first time, the shape-memory properties in such materials, as verified by thermomechanical analysis. Moreover, the response temperature to the material original shape depended on the block copolymer emplacement, hence PTMC or PCL as end-block. Therefore, it has been possible to reach a block copolymer with transition temperature around 40°C thus opening potential real-life medical applications. In conclusion, the initial study of phase-separation/crystallinity relationship in PTMC-b-PCL-b-PTMC block copolymers lead to the discovery of novel shape memory materials with superior properties, widely demanded in modern-life applications.

Keywords: biodegradable block copolymers, organocatalytic ROP, self-assembly, shape-memory

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Authors: Nigus Maregu Demewoz, Shu-Kai Yeh

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Low-density nanocellular foam is a fascinating new-generation advanced material due to its mechanical strength and thermal insulation properties. In nanocellular foam, reducing the density increases the insulation ability. However, producing a nanocellular foam of densities less than 0.3 with a cell size of less than 100 nm is very challenging. In this study, poly (methyl methacrylate) (PMMA) was blended with Polyether block amide (PEBAX) to study the effects of PEBAX on the nanocellular foam structure of the PMMA matrix. We added 2 wt% of PEBAX in the PMMA matrix, and the PEBAX nanostructured domain size of 45 nm was well dispersed in the PMMA matrix. The foaming result produced a new generation special bouquet-like nanocellular foam of cell size less than 50 nm with a relative density of 0.24. Also, we were able to produce a nanocellular foam of a relative density of about 0.17. In addition to thermal insulation applications, bouquet-like nanocellular foam may be expected for filtration applications.

Keywords: nanocellular foam, low-density, cell size, relative density, PMMA/PEBAX

Procedia PDF Downloads 74