Day 1 :
Keynote Forum
Gilles Goetz
Pfizer, USA
Keynote: :EPSA: a novel supercritical fluid chromatography technique enabling the design of permeable cyclic peptides
Time : 09:35-10:15
Biography:
Gilles Goetz is a Principal Scientist at Pfizer in Groton, Connecticut, USA. He received his BSc (1991) and PhD (1995) at the University of Strasbourg in France. After his Post-doctoral studies at the University of Hawaii (1996-97) and of Neuchatel (CH) (1998-99) studying marine and fungal natural products, he joined Monsanto in 2000. There, he worked through mergers and acquisitions for Pharmacia and Pfizer successively in the natural product group, the HTS group (analytical support), and the purification group. In 2010, he transferred to the expert purification group at Pfizer Groton and in 2011 to the molecular properties group. He is a part of the team influencing medicinal chemistry design through insights into molecular properties such as polarity, lipophilicity, shape, and conformation that will impact molecular behaviors like solubility, permeability, and efflux. They develop and use mainly chromatographic techniques (EPSA) to assess those properties, and work towards predicting molecular behaviors.
Abstract:
Applications of a new chromatographic method using SFC technology developed recently at Pfizer are described here. The EPSA method, as readout of polarity, correlates retention on a specific stationary phase with the exposed polarity of a molecule. Changes in retention can be interpreted by changes in polarity induced by the presence of intra-molecular hydrogen bonding (IMHB): indeed, IMHBs tend to impact molecular conformation, inducing hidden polarity that results in a decrease in analyte retention on the EPSA support. We demonstrate here the impact of this method on multiple beyond rule of five projects (NS5A, Oxytocin Receptor, CXCR7 Modulator, others). Given that conformational changes (induced and/or stabilized by the formation of IMHB) increases potential for membrane permeability, we show here that EPSA, and the EPSA prediction model, have significant impact in peptide drug design.
Keynote Forum
Károly Héberger
Hungarian Academy of Sciences, Hungary
Keynote: Separation selectivity of liquid chromatographic columns: a comparison by nonparametric methods
Time : 10:15-10:55
Biography:
Károly Héberger has completed his PhD, Cand. scient., DSc and t. Prof. In his early career, he investigated liquid phase oxidation (radical) processes and determined rate constants by kinetic ESR spectroscopy. Later, he studied quantitative structure activity (property) relationships like QSAR, QSPR and QSRR. Now, he deals with chemometrics such as multivariate data evaluation techniques, principal component analysis, stepwise linear regression, partial least squares regression, variable selection, model building and validation, pattern recognition (supervised and unsupervised), classification of food products, clustering, method comparison and ranking etc. His scientific results were presented in more than 160 papers (including book chapters) and has given more than 300 lectures (or posters) with h-index=34 and i-10 index=83 (Web of Science). The papers were cited above 3500 times.
Abstract:
There are two legitimate aims for column selection: i) to determine similar ones to an existing one and ii) to find diverse (orthogonal) one(s) for optimal separation. Several different methods have already been elaborated to compare selectivity of chromatographic columns. All comparisons realize empirical approaches and based on measuring retention data of several well-chosen test compounds. Proper multivariate analyses can find similarities and differences in retention behavior of test compounds and stationary phases. As an illustration we adopted Wilson et al.’s data of 67 test compounds and 10 highly similar columns (C18-bonded silica stationary phases). The inherent characteristic groupings by physical properties were revealed with correct statistical tests and several independent methodologies. Generalized pair correlation method (GPCM)2 and sum of (absolute) ranking differences (SRD)3,4 unambiguously showed the same ranking pattern. The clustering by SRD is delivered to the reference. Therefore, all columns have been chosen as gold standard once and only once (comparison with one variable at a time). All lines of boxes correspond to an SRD ordering always with a different reference column (Figure 1). COVAT heatmaps show destroying the true pattern if the hydrophobic-subtraction model (HSM) evaluation is used. The ranking (clustering) pattern of chromatographic columns based on retention data (log k values) of 67 compounds and selectivity parameters of hydrophobic-subtraction model (HSM) provided various column groupings. Loss of information is inevitable for using the HSM data handling. Processing of retention data resulted in patterns that are consistent with differences in the columns’ physicochemical parameters, whereas HSM results are deviating to a higher or lesser degree, depending on the particular chemometric approach. GPCM, SRD and COVAT procedures can be carried out on any data sets partially and on the whole to select the most similar and dissimilar columns, though our calculations were completed to the data set of Wilson et al.
Keynote Forum
Hong Xue
Hong Kong University of Science and Technology, Hongkong
Keynote: Dispersed mobile-phase countercurrent chromatography
Time : 11:10-11:50
Biography:
Hong Xue has obtained her MD from the Shanghai Second Military Medical University in 1983, PhD from the Institute of Medical Sciences and Department of Biochemistry, University of Toronto in 1992, and carried out Post-doctoral studies at the Department of Genetics, University of Glasgow before joining the Department of Biochemistry, Hong Kong University of Science & Technology (HKUST). Currently, she is the Director of Applied Genomics Center of HKUST, and Professor of Life Science at Hong Kong University of Science and Technology. Her group research focuses on genomics, bioinformatics and evolution biology to decipher the mechanisms of human complex diseases, in particular, schizophrenia. The group is also interested in translational research on novel therapeutics and diagnostics for complex neuropsychiatric disorders including anxiety, depression and neurodegenerative disorders, with a focus on GABAA receptors as the drug targets. In order to effectively isolate active components from medicinal herbs, her group has recently developed a novel chromatographic method designated as Disbursed Mobile-Phase Countercurrent Chromatography (DMCC). In 2003, she and her team discovered the association between schizophrenia and a segment of the GABRB2 gene encoding the b2-subunit of GABAA receptors, the positive selection of genotypes and haplotypes in this segment, determinant role of this segment in the alternate splicing of the b2 subunit protein, and the differential modulation of the GABA-induced membrane current by the long and short forms. These discoveries represent therefore the first instance where a schizophrenia-susceptibility gene has been linked to protein processing and further to electrophysiological response of neurons, thereby opening the door toward understanding the mechanism of schizophrenia etiology leading from gene to neuronal phenotype.
Abstract:
Countercurrent distribution based on liquid-liquid partition is a powerful separation method with minimal incurrence of loss of solutes, but its industrial application has been limited by cumbersome shifting of immiscible solvents. Although centrifugation has been employed to facilitate equilibration between phases, process scaling-up remains difficult. In this study, a dispersed mobile-phase countercurrent chromatography (DMCC) method has been developed to adapt the countercurrent distribution principle to a continuous column chromatography format. Continuous solute-exchange between two immiscible phases within a series of separation columns is achieved by mechanical dispersion of an influx of mobile phase into an upward stream of small droplets travelling through the columns filled with stationary phase. The diameter, length and number of columns and the number of stationary phases employed in the different columns can be varied to match the requisite scale and resolution of operation. Illustrations of DMCC were provided by examples of solute separations where the fractionated solutes could be collected either from the eluate of the series of columns or from drainage of the stationary phases in the individual columns at the end of a chromatographic run.
- Applications of Chromatography | Analytical Chromatography | High Performance Liquid Chromatography | Polymer and the Environment | Biopolymers
Chair
Károly Héberger
Hungarian Academy of Sciences
Session Introduction
Gómez-López Alicia
Mycology Reference and Research Laboratory, Spain
Title: Triazoles therapeutic drug monitoring: from recommendation to applicability
Time : 11:50-12:15
Biography:
Gómez-López Alicia (representative investigator of this research team) has been part of the CNM Mycology Reference Laboratory since 2000. Since her incorporation as a PhD student, has participated in several research projects related to research in human fungal infection. In 2007 she was in charge of creating a new research line into the Laboratory. This is a line of cutting-edge research in Medical Mycology, which seeks to define relationships between dose and therapeutic response, and also better explain the clinical significance of resistance, by evaluating parameters PK/PD of antifungals and their relationship with efficacy. New strategies using alternative models of infection are now on going in this field with interesting perspectives and applications. This research is also evaluating the effect of the patient genetic background in treatment efficacy (pharmacogenetic). This new line is nowadays working actively in the lab. Each year new staff is incorporating to advance in this research by means of competitive applications. Thanks to these resources new methods have been developed and validated, contributing positivity to assist the national health system in fungal infection management.
Abstract:
The past three decades have seen a considerable expansion in antifungal drug research that led to the clinical development of antifungal agents with different pharmacologic properties. The new antifungal triazoles (fluconazole FCZ, voriconazole VCZ, itraconazole ICZ, posaconazole PCZ and isavuconazole ISvZ) are widely used for the management of invasive fungal infections (IFI). With the exception of fluconazole, these triazoles exhibit significant inter- and intrapatient pharmacokinetic variability and are associated to multiple drug interactions. Thus, unexpected blood concentrations often need to be evaluated in patients treated with them, to prevent treatment failure or toxicity. A large number of recent studies suggested that the efficacy and tolerance of azoles can be increased through TDM. Measuring blood concentrations of these antifungals and their metabolites could be used for quick identification of patients with impaired metabolism, a suitable strategy to improve effectiveness of this type of treatment. So, to facilitate dosage adjustment, easy, accurate and precise TDM methods need to be routinely used.
Objective: The aim of the study was to describe systemic azoles pharmacokinetic in a collection of clinical samples using a validated HPLC-PDA assay. The method also allows the simultaneous quantification of triazoles and some of their major metabolites (voriconazole N-oxide VCZ N-oxide, and hidroxy-itraconazole OH-ICZ) in the same run.
Abraham George
ADNOC Refining Research Centre, UA
Title: Methyl tertiary butyl ether in heavy hydrocarbon matrix: identification and quantification using gas chromatography headspace technique
Time : 12:15-12:40
Biography:
Abraham George is working as the Section Head of Analysis at ADNOC Refining Research Centre. He has 25 years of experience in the area of Petroleum Inspection and Laboratory Analysis. He has completed his Bachelor's Degree in Chemistry and obtained his Master’s Degree in Business Administration from Mahatma Gandhi University, India. He worked in various capacities in managing laboratories in India, Saudi Arabia and in UAE, and involved in inspection and analysis of entire range of crude Oil, petroleum products and other materials. He is a certified Lead Auditor in ISO 9001:2008 QMS from Lloyds Register Quality Assurance.
Abstract:
Statement of the Problem: Petroleum product slop generated in products distribution terminals contains different products handled within the terminal, specifically unleaded gasoline which contains MTBE (Methyl tertiary butyl ether) blended as additive. These slops are injected into the atmospheric residue stream feeding the refinery vacuum distillation unit as a recycling option. Due to this optional blending of MTBE containing slops to the Vacuum distillation (VD) feeds, there are concerns over possibility of MTBE carry over in the vacuum distillation products, which might have an impact on the hydrocracking catalyst and the quality of the products specifically naphtha. The objective of this case study is to determine the MTBE content in the vacuum distillation products like light vacuum gas oil and heavy vacuum gas oils (LVGO and HVGO). Since there are no standard test methods exists to determine the content MTBE in VD products. The purpose of this study is to develop a chromatographic method for identification and quantification of MTBE in heavy hydrocarbon matrices.
Methodology & Theoretical Orientation: Various heavy hydrocarbon matrices starting with light vacuum gas oil, heavy vacuum gas oil, and straight run residue were selected as representative heavy hydrocarbon matrix. Temperature conditions from 90°C to 180°C with an increment of 30°C were selected for study in GC-HS and optimized GC headspace parameters and GC parameters for all the matrices.
Findings: After the laboratory study using various heavy hydrocarbon matrices at various temperatures, it is observed that gas chromatography headspace technique can be used for the identification and quantification of MTBE. Also, derive a theoretical equation for the quantitation in specific matrix. Results obtained theoretically and practical measurements are well within the repeatability window of the gas chromatography headspace technique.
Dawei Cao
Chinese Academy of Engineering Physics, China
Title: Application of metal-organic framework material in hydrogen isotope chromatographic separation and analysis
Time : 12:40-13:05
Biography:
Dawei Cao is a PhD student under the supervision of Prof. Shuming Peng in China Academy of Engineering Physics and Prof. Zhengjun Zhang in Tsinghua University. He completed his Graduate degree from Amoy University in 2012. His current research concentrates on the separation and analysis of hydrogen isotopes.
Abstract:
Hydrogen isotope separation is among the key technological problems, in the utilization of nuclear fusion energy and moreover, in gas atmosphere in the process flow of ITER fuel cycle it is more than complexity. Thus, making effective separation and analysis of hydrogen isotopic mixtures is necessary and an urgent task to be addressed. As hydrogen isotopes share almost identical shape, size and chemical properties, separating and analyzing of hydrogen isotopes is really not an easy task. In this letter, ultralow temperature separation of H2/D2 mixture through quantum sieving was experimentally examined on two metal-organic framework (MOF) materials, with an extreme two-dimensional confinement formed within the material of {[Fe(OH)(H2bta)](H2O)}n experienced by hydrogen molecules, an extraordinary separation factor of H2/D2 as high as 41.4±0.4 at 20 K was finally experimentally obtained. Furthermore, MOF material CPL-1 ([Cu2(pzdc)2(pyz)]n) was further tested as the stationary phase of gas chromatography for the analysis of H2/HD/D2 mixtures with a large specific surface area and uniform pore size, CPL-1 showed a better adsorption of H2/D2 in capacity than that of MnCl2@γ-Al2O3 and γ-Al2O3 and CPL-1 packed column showed more rapidly in signal detection, i.e., less retention time, than that of MnCl2@γ-Al2O3 toward H2/HD/D2 under a condition of 77 K and carrier gas (Ne) flow rate of 3 ml/min. With a sampling volume of 0.25~2.0 ml, GC with CPL-1 packed column showed good linear respondence toward measurement of H2/HD/D2 mixtures with mean relative error less than 4%, showing promising potential use of MOF material in hydrogen isotope chromatographic analysis.
Juan GarcÃa-Góngora
University of Lausanne, Schwitzerland
Title: Analysis by fast GC-MS of cocaine and minor alkaloids: an added value for law enforcement
Biography:
Abstract:
The present work is focused on the optimization and validation of the analytical methods by fast-GC-MS for the determination of cocaine and identification of minor alkaloids and most common cutting agents in powders seized by the law enforcement. Optimization procedure was a deal between the sensibility, signal saturation and time analysis for the identification of minor alkaloids in the presence of a large amount of substances as it occurs in some real cases. Injection temperature and volume, split ratio as well as the temperature ramp for the separation were the optimized instrumental variables. The validation was performed using inter-laboratory samples of cocaine. For this purpose, the accuracy profile procedure was applied in order to evaluate the capability of the method to quantify samples with a known accuracy and a fixed risk at 5%. The analytical method was accredited by the Swiss Accreditation Service (SAS) according to the UNE-EN ISO/IEC 17025:2005 guidelines. The method is used as a routine analysis in the forensic laboratory and allows not only the quantification of cocaine but also the profiling analysis of the minor alkaloids in less than 6 min per run. The profiling study provides information as an added value to the law enforcement, since it provides information about links among cocaine street samples using Pearson correlation coefficients, principal components analysis (PCA) and hierarchical cluster analysis (HCA).
F.Picchioni
University of Groningen, The Netherlands
Title: Synthesis, processing and application of renewable and/or biobased polymeric products
Time : 14:30-14:55
Biography:
F.Picchioni has completed his PhD in 2000 from the University of Pisa (Italy) and postdoctoral studies from the Technical University of Eindhoven (The Netherlands). Since 2013 he is full professor and chair of the group Chemcial Product Engineering at the University of Groningen (The Netherlands). He has published more than 100 papers in reputed journals.
Abstract:
The development of new (or improved) chemical products finds its starting point in the definition of a chemical structure for a given application. Already at this stage of the design process, sustainability-driven consideration can be taken into account. In the last 20 years, a clear trend can be detected in the use of monomeric units derived from biomass for the design of new polymeric materials. However, “going green” might not provide an exhaustive answer to the sustainability issue as it could still result in the use of polluting polymeric products. The case of polyethylene produced from ethanol (via ethylene) is paradigmatic in this context. The combination of biomass derived synthetic strategies with relatively novel concepts from the polymer world, such as self-healing and re-workability (conceptually linked to the underlying concept of thermally reversible networks), represents a viable option. In this work we will provide an overview of our current research activities at the University of Groningen dealing with the synthesis, processing and application of renewable and/or biobased polymeric materials. Starting with the use of starch in bioplastics and the corresponding “green” processing strategy (in supercritical CO2), the concept of thermally reversible networks will be subsequently introduced. Application of the latter to oil-based resins (e.g. epoxy) and then to bio-based ones (e.g. vegetable-oil derivatives) will be discussed in terms of the necessary synthetic steps and the final product properties (including reworkability).
Mohammed A. Meetani
United Arab Emirates University, UAE
Title: Development and validation of GC-NCI-MS method for detection and quantitation of synthetic Cathinones in plasma and urine: effect of CI reagent gas on method sensitivity
Time : 14:55-15:20
Biography:
Dr. Mohammed A. Al-Meetani has received his PhD Degree in applied analytical chemistry from Colorado School of Mines, Colorado, USA in 2003. His research encompasses various topics in the areas of pyrolysis mass spectrometry of the peptide and proteins, degradation of organic water pollutants using advanced oxidation processes, determination of human derived chemicals in ground and wastewater, and development of analytical methods for detection and determination of designer drugs of abuse. Dr. Meetani’s work has resulted over 40 articles in reputed journals and international conference proceedings. He has worked at different international universities and research institutes such as national renewable energy laboratory (NREL), CO, USA, University of Wyoming, Wy, USA, and Sam’s Nobel Foundation, OK, USA.
Abstract:
A statement of the Problem: the latest version of new designer substances (NDS) is called “bath salts” and they g spread in the drug of abuse market. Bath salts are a group of central nervous system stimulants that consists mainly of synthetic cathinone derivatives. They are chiral substances that exist as a racmic mixture. Objectives: Development and validation of sensitive and selective method for enantioseparation and quantitation of synthetic cathinones “bath salts” has been done by using GC-MS (SIM) with chemical ionization source in negative mode (NCI). Methodology: Indirect chiral separation of thirty six synthetic cathinone compounds has been conducted by using optically pure chiral derivatizing agent (CDA) called (S)-(–)-N- (trifluoroacetyl)pyrrolidine-2-carbonyl chloride (L-TPC) which converts cathinone enantiomers into diastereoisomers that can be separated on achiral GC-MS columns. Ultra inert 60 m column was used. Slow heating rate (2 oC/min) on the GC oven has resulted an observed enhancement in enantiomer peak resolution. An internal standard, (+)-cathinone, was used for quantitation of synthetic cathinone. Conclusion & Significance: Method validation in terms of linearities, limits of detection (LOD), limits of quantitation (LOQ), recoveries and reproducibilities have been obtained for fourteen selected compounds that ran simultaneously as a mixture after being spiked in urine and plasma. Unlike the Electron Impact ion source (EI), NCI showed higher sensitivity by three orders of magnitude by comparing with the previous results.. Moreover, signal intensity improvement observation after changing the CI reagent gas from methane to isobutane, argon or methane/ammonia (95:5) will be discussed.
Maryam Salimi
Tehran Province Water and Wastewater Company, Iran
Title: A simple method based on solid-phase extraction coupled with HPLC for determination of Ibuprofen and Diclofenac belong to group of Painkiller and anti-inflammatory drugs in wastewater samples from wastewater treatment plant in the south of Tehran
Time : 15:20-15:45
Biography:
Abstract:
In this study, a simple, efficient and reliable HPLC method was developed for determination of ibuprofen and diclofenac belong to group of Painkiller and anti-inflammatory drugs in wastewater influents and effluents from WWTP. The method involves pre-concentration and clean-up by solid phase extraction (SPE). Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) on a reversed- phase C18 column using by gradient elution with methanol , acetonitrile and a 0.05 M phosphate-buffer (pH=4.5) at a flow-rate of 1 ml min-1 with diode array detector (DAD). The recoveries for all samples were more than 70%. The calibration curves obtained for studied drugs show reasonable linearity (R2 > 0.99) and the Limits of quantification were 0.05 ng ml-1 and 0.1 ng ml-1for ibuprofen and diclofenac, respectively. The described method was applied to the determination of the drugs in wastewater samples from WWTP in the south of Tehran.
Giulia Caron
University of Torino, Italy
Title: The Block Relevance (BR) analysis to interpret chromatographic data: application to IAM chromatography in permeability studies
Time : 15:20-15:45
Biography:
Giulia Caron’s primary scientific activity was lipophilicity, then she moved to the design, experimental determination and computational prediction of physicochemical properties related to ADME properties and to permeability measurements. The integration of Intramolecular Hydrogen Bonding (IMHB) considerations in drug design and the development and application of a tool named Block Relevance (BR) analysis to provide a mechanistic interpretation of QSAR/QSPR models based on the PLS algorithm are two of her main field of interest. To fit new drug discovery exigences she is now focusing on defining a set of experimental and in silico tools for molecular properties evaluation in the bRo5 chemical space
Abstract:
Statement of the Problem: The Block Relevance (BR) analysis is a computational tool that can be conveniently used to characterize and compare chromatographic scales. Immobilised Artificial Membranes (IAM) chromatography is expected to predict drug membrane permeability, a pivotal molecular property in drug discovery processes. The purpose of this study is to extract by BR analysis the balance of intermolecular interactions governing IAM descriptors (log KwIAM, ï„log KwIAM) and verify their relationship with passive permeability. Methodology: Experimental: The RP-HPLC analyses were performed with 20 mM ammonium/acetate at pH 7.0 in water or in mixture with acetonitrile at various percentages. The stationary phase was IAM.PC.DD.2: its surface is formed by covalently bonding the membrane forming phospholipids to silica (Regis, 10cmx4.6cm 10um packing 300Å pore size). The flow rate was 1.0 ml/min. Computational: VolSurf+ (Vs+) software (version 1.0.7, http://www.moldiscovery.com) was used to generate PLS models with default settings and four probes (OH2, DRY, N1, and O probes that mimic, respectively, water, hydrophobic, HBA, and HBD properties of the environment). BR analysis was performed using an in-house software. Findings: BR analysis showed that
successful prediction of permeability using log KwIAM alone is unlikely to occur but its combination with PSA can reasonably well predict PAMPA log Peff of neutral and ionized compounds. Conversely, ï„log KwIAM is a polarity descriptor and thus plays a very relevant role in the prediction of cellular permeability Conclusion: IAM chromatography provides two descriptors (log KwIAM and ï„log KwIAM) of interest in the prediction of permeability, which is a crucial issue of any drug discovery project. Overall, this study highlights that, prior to their application to biological/toxicological topics, any chromatographic descriptor should be characterized for its information content using a tool like BR analysis.
Chengjian Xiao
China Academy of Engineering Physics, China
Title: Application of Cryogenic Preparative Chromatography in Hydrogen Isotopes Separation
Biography:
Abstract:
The separation of large-scale hydrogen isotopes is important in the process of nuclear fusion energy development and utilization. So far, there are few hydrogen isotope separation techniques suitable for industrial scale applications, and cryogenic preparative chromatography has advantages in terms of simple equipment, reliable operation, large separation factor, high product purity, and low retention of tritium. In this paper, a cryogenic chromatography method for reprocessing Tokamak exhaust gas is described. The experimental apparatus consists of a column with carbon molecular sieve used as exhaust storing and purification unit, four columns with 5A molecular sieve operated at the temperature of liquid nitrogen to adsorb hydrogen isotopes. In order to raise the efficiency and to shorten the total time of isotope separation and the total length of columns between two columns, a disproportionate equilibrator for isotope exchange of HD and HT was inserted. After passing through the cascade columns, the protium, deuterium and tritium are separated cleanly. The overall recoveries of deuterium and tritium for cleanup isotope separation procedure are greater than 97%, and the protium removing efficiency is larger than 98%. Further refining the process operating parameters, be able to get an ideal result, and is expected to meet the requirements of self-sustaining tritium fuel cycle.
Swati Sharma
Banaras Hindu University, India
Title: L-Alanine induced Thermally Stable Self-Healing Guar gum hydrogel as Potential Drug Vehicle for Sustained Release of Hydrophilic Drug
Time : 16:50-17:15
Biography:
Swati sharma is persuing her Ph.D programe in polymer chemistry, from Institute of science, Banaras Hindu university. She has published four papers in reputed journal, and three are in under review. She is now Ph.D research scholar in chemistry department, Banaras hindu university, INDIA.
Abstract:
Hydrogels are 3D polymeric networks, which are hydrophilic and cross-linked via covalent or non-covalent interactions. Because of their soft nature with similar physical properties to soft tissues attracts more attention in biomedical application but due to its weak mechanical strength and non-healable nature, its application are still restricted in biomedical field. This article introduces a simple approach of preparing self-healable guar gum-graft-acrylic acid (GG-PAA) hydrogel using first time L-alanine as a cross-linking agent which alters the various properties of hydrogel such as mechanical strength (G’=90,570Pa). A series of guar gum (GG) based hydrogel were synthesized by varying the concentration of L-alanine (from 0.4-1% w/v) which was used as a cross-linking agent. Hydrogel was characterized by HRSEM and Rheology studies which explore the morphology and mechanical strength of hydrogel; further it was investigated that synthesized GG based hydrogel showed good swelling ability with excellent self-healing property. The highly water soluble drugs have a tendency to burst rapidly into human body which is undesirable and thus, this hydrogel may be helpful to overcome this problem too and found fruitful applications in biomedical field.
- Hyphenated Techniques in Chromatography | Advances in Gas Chromatography | Polymer Rheology | Nanomaterials and Nanotechnology
Chair
F.Picchioni
University of Groningen, The Netherlands
Session Introduction
Joanna Fiedor
AGH-University of Science and Technology, Poland
Title: Chromatographic purification of photosynthetic water-soluble and membrane proteins for spectrometric analysis
Biography:
Joanna Fiedor has received her PhD degree in Biochemistry from the Jagiellonian University, Kraków, Poland. During 1997-1999, she visited the Ludwig-Maximilians University (LMU) in Munich, Germany, and in 2002 the Kwansei Gakuin University, Sanda, Japan. Currently, she is an Assistant Professor at the AGH-University of Science and Technology, Kraków, Poland. Her research interests are focused on: natural biocompounds (carotenoids) in relation to human health, and biotechnological applications of phototrophic microorganisms.
Abstract:
Purple non-sulphur phototrophic bacteria constitute a unique group of “photosynthetic” organisms capable of adjusting their metabolism in response to the alteration of environmental growth conditions. In the presence of light and absence of oxygen, bacterial cells develop extensive system of intracytoplasmic membranes, hosting entire “photosynthetic machinery”. It comprises different types of pigment-protein complexes involved in capturing and extremely effective conversion of light energy into chemical energy. Recently, purple bacteria have been gaining considerable attention due to their increasing potential in a range of scientific and industrial applications. In the present study two species of anoxygenically grown phototrophic bacteria were used. Following the isolation of their membranes, the components of the photosynthetic apparatus were separated and purified by the application of weak anion exchange chromatography. This chromatographic technique is characterized by relative simplicity, vast availability as well as high effectivenes of structure’s separation. Hence, it proved to be one of the most useful methods for isolation and purification of membrane as well as water-soluble proteins. Application of ion-chromatography resulted in preparation of a series of photosynthetic (pigment-) protein structures of adequate purity for spectrometric analysis. Here, total reflection X-ray fluorescence spectrometry (TXRF), one of the well-established spectroscopic techniques applied for the precise elemental profiling of organic and inorganic samples, was used to perform comprehensive examination of the elements present in bacterial proteins.
Miroslav Ryska
Quinta-Analytica s.r.o., Czech Republic
Title: :The Use of Isotopiocally Labeled Internal Standards in Quantitative LC/MS – The Way of The Full Compensation of Negative Impact of “Matrix Effect
Biography:
Mr. Miroslav Ryska (1938) holds an undergraduate degree from Charles University, along with an M.S. in Physical Chemistry from Moscow State University and a PhD. from the Institute of Macromolecular Chemistry of Czechoslovak Academy of Sciences. From 1961 to 1978 he worked at the Institute of Macromolecular Chemistry of the Czechoslovak Academy of Sciences. In 1978 - 1997 he worked as a researcher in the field of MS and its application in research of metabolism and pharmacokinetics of drugs at the Research Institute for Pharmacy and Biochemistry in Prague. He has written more than 100 publications mainly on the topic of mass spectrometry, trace analyses, analyses of drugs, metabolites and quantitative analysis. In the 1990’s Mr. Ryska acted as an Editor of two international journals, The Journal of Mass Spectrometry and Rapid Communication in Mass Spectrometry. He founded Quinta-Analytica s.r.o.in 1997
Abstract:
The source of the “Matrix effect” as a consequence of analyte ions suppression or ions enhancement must be sought in the presence of unknown impurities from matrix. They are participating in the complex ionization process in parallel or competing ion-molecular reactions. Not only impurities from extracts but impurities adsorbed in the ion source and/or in the analytical system may play an important role. These adsorbed substances cannot be fully removed from the system by any cleaning procedure.
To fully compensate for the negative impact of the “Matrix effect“, use of isotopically labeled internal standards (isotope dilution technique) proved to be the only effective technique. This applies especially to LC/MS/MS determination of drugs and
their metabolites in complex extracts of biological matrices. The isotope dilution technique is successful regardless of the method of purification, the ionization technique (APCI or ESI) and the type of the equipment used. The isotope dilution technique proved to be 100% effective for the compensation of matrix effect influences in 181 analytical methods developed and validated. The strict requirements of EMA guidelines to investigate different plasma sources for the assessment of the matrix effect in the analytical method validation are discussed.
Tuzimski T
Medical University in Lublin, Poland
Title: Optimization of extraction conditions, identification and quantitative analysis of xenobiotics (e.g., pesticides, dyes, bisphenols) in natural and biological samples and food products using high-performance liquid chromatography (HPLC) combined with modern detection techniques (DAD, MS, MS/MS)
Biography:
Tuzimski T is an Adjunct Professor in the Department of Physical Chemistry at Faculty of Pharmacy with Medical Analytics Division, Medical University of Lublin, Poland. He received MA Degree and PhD (in 1995 and 2002, respectively), and Doctor of Sciences (habilitation) Degree (in 2012) at the Faculty of Pharmacy with Medical Analytics Division, Medical University of Lublin. His scientific interest includes the theory and application of liquid chromatography, extraction (QuEChERS) and detection techniques. He is authored or co-authored more than 77 scientific papers (IF=100, H-index=17). He is a Member of an Editorial Board of the Acta Chromatographica. He is a Quest Editor of special sections on pesticide residues analysis in the JAOAC International. He is co-authored and co-edited with Professor Joseph Sherma the book entitled “High Performance Liquid Chromatography in Pesticide Residue Analysis” (2015) and the book “Determination of Target Xenobiotics and Unknown Compounds Residue in Food, Environmental and Biological Samples” (2018; CRC Press). Dr. Tuzimski is a promoter of one doctorate (2017) and research work of six masters of pharmacy, and supervised the research work of 10 masters of pharmacy.
Abstract:
Bisphenols are a class of chemicals with two hydroxyphenyl functionalities, which include bisphenol A (BPA) and several analogues such as BPS, BPB, BPF, BADGE, BADGE•2H2O, and BADGE•2HCl. The release of BPA into the food depends on the type, pH and lipid content of food, temperature, and contact time. Due to their fat content, both breast and dietary milk could be polluted by many xenobiotics characterized by lipophilic properties. Milk and dairy products are widely consumed by infants, children, and many adults throughout the world, and occurrence of quantifiable amounts of BPA represents a matter of public health concern. European Commission (EU) has established a migration limit of 0.6 mg/kg for BPA in food or food simulant from plastic materials and articles intended to come in contact with foodstuffs (Regulation (EU) No. 10/2011) and has interdicted the BPA use in the fabrication of baby bottles (Regulation (EU) No.321/2011). Considering that many estrogenic effects caused by BPA occur at concentrations below the recommended safe daily exposure and that children are particularly vulnerable, a new risk assessment has been strongly recommended for consumer health protection.
The aim of the experiments was to determination of xenobiotics (BPA and its analogues, pesticides, dyes, medicines) in natural and biological samples (e.g., breast milk) and food products. Author proposed a rapid, efficient, and reliable method for extraction of different class/groups of xenobiotics from natural samples, based on modified QuEChERS procedure. The novelty of the experiments concern possibility of utilizing relatively new and innovative zirconium based sorbents (Z-Sep and Z-Sep Plus) for clean-up of analyzed extracts. Average recovery; repeatability and matrix effect were accounted for finally selected extraction conditions. Validation of the chromatographic methods (linearity, limits of detection (LODs) and quantification (LOQs)) was also carried out.
Xiaolong Fu
China Academy of Engineering Physics, China
Title: Sol-gel processed metal-organic framework capillaries for hydrogen isotopes separation
Biography:
Xiaolong Fu has obtained his PhD in Physical Chemistry from Institute of Chemistry, Chinese Academy of Sciences, in 2015. Then, he has joined the Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics. He mainly focused on the novel microporous and mesoporous materials and applications in hydrogen isotopes separations.
Abstract:
Hydrogen isotopes are most likely fuels of future nuclear fusion plants. And fast analysis of hydrogen isotopes is very important. Cryogenic gas chromatograph with capillary column is one of the best methods for analyzing hydrogen isotopes. Recently, significant progress has been made to shorten analysis time and realize on-line analysis by cryogenic gas chromatograph, with promising potential for application. However, due to the same chemical properties and the identical kinetic diameters, separation and quantitative analysis hydrogen isotopes is difficult by using their minute difference. Herein, we reported a new method in preparation of metal-organic frameworks capillary column via sol-gel process. Metal-organic frameworks thin film was uniformly coated on the inner wall of the capillary column and the hydrogen isotopes were separated within one minute.
Károly Héberger
Hungarian Academy of Sciences, Hungary
Title: :Column Selection in Liquid Chromatography
Biography:
Károly Héberger Ph.D., Cand. Sci., D.Sc., t.Prof.. in his early carrier he investigated liquid phase oxidation (radical) processes, and determined rate constants by kinetic ESR spectroscopy. Later he studied Quantitative - structure activity (property) relationships. QSAR, QSPR and QSRR. Now he deals with chemometrics: multivariate data evaluation techniques, principal component analysis, stepwise linear regression, partial least squares regression, variable selection, model building and validation, pattern recognition (supervised and unsupervised), classification of food products, clustering, method comparison and ranking, etc. His scientific results were presented in more than 160 papers (including book chapters) and more than 300 lectures (or posters). Hirsch index=34 and i-10=index 83 (Web of Sci). The papers were cited above 3800 times (without self - citations and cross - references). More information can be found at: http://aki.ttk.mta.hu/scientist/heberger/
Abstract:
A lot of protocols have been elaborated for stationary phase selection, (further on column selection) in chromatography.1-4
One of the earliest developed procedure was the Tanaka system1: six selectivity parameters have characterized commercial packing column materials. Later, Euerby improved the system2 and defined the Column Difference Factor (CDF).3 Snyder and Dolan have utilized five selectivity parameters and elaborated the so called hydrophobic-subtraction model with a cornerstone of column selectivity function (Fs).4 Hoogmartens et al. have applied only four selectivity parameters and defined the Fmetric.5 Their approach is known as KUL column selection system (CSS). All above approaches are empirical and all of them is based on measurement of some well-chosen reference compounds and calculation of Euclidean distance between the concerned and a reference column.
Our chemometric approach compares the column selection systems using some simple pattern recognition methods: (icon (polygon, radar or spider-web) plot and stacked plots. Ten similarity measures (Euclidean and Manhattan distance, Kendall tau, Spearman rho, Person’s correlation coefficient, generalized pair correlation methods with various statistical test options as e.g. Williams’ t test, conditional Fisher’s exact test, McNemar test, etc. have shown some contradictory behavior, still their data fusion allows us to compare and rank the column ranking systems.
A significant loss of information arises during the application of the hydrophobic-subtraction model.
We could not only rank and group the column classification protocols, but to select the most suitable similarity (or dissimilarity) measure for selection of the most similar and dissimilar i.e. orthogonal chromatographic system.
Work is under way to determine the smallest number of reference compounds responsible for all dominant interactions in chromatography and hence classification of chromatographic columns will be possible with the smallest efforts without having significant information loss.
Meliha Ekinci
Ege University, Turkey
Title: Radioanalytical chromatography techniques for newly developed radiopharmaceutical: 99mTcibandronate sodium
Biography:
Meliha Ekinci has obtained her Master’s degree in Radiopharmacy at Ege University, Turkey in 2015. She is currently a PhD student and also a Research Assistant at Radiopharmacy Department, Ege University, Turkey. She has published 12 research papers and review articles and 26 conference presentations. Her main research interest focuses on radiolabeling and evaluating newly developed radiopharmaceuticals for diagnosis of different cancer types, especially breast cancer, and novel drug delivery systems (nanoparticles, microemulsions, etc.). She has completed four scientific research projects, and is currently working on three projects about New Radiopharmaceuticals. She is a Member of professional societies like European Federation of Pharmaceutical Sciences (EUFEPS) and Society of Radiopharmaceutical Sciences (SRS) and some local societies like Turkish Pharmacists Association 3rd Region Izmir Pharmacist Chamber. She has 35 citations up to now.
Abstract:
Statement of the Problem: Bisphosphonates (BPs) are chemically stable pyrophosphate analogues, and used to treat pathological conditions associated with bone mass loss. Radiolabeled BPs, which used as bone-seeking radiopharmaceuticals for imaging or therapy hold an important place in nuclear medicine, radiopharmaceuticals are radioactive drugs containing a pharmaceutical compound and a suitable radionuclide. While biologically active molecule or drug acts as a carrier and determines localization, the radionuclide permits external detection. FDA approved radiopharmaceuticals as drugs and it is mandatory to satisfy the guidelines for quality control tests which include the radiochemical, radionuclidic and chemical purity as well as checks for pharmaceutical concerns. In the past 10 years, separation and quality control methods such as radioactive thin layer chromatography (RTLC), high performance liquid chromatography (HPLC) and electrophoresis have widely used in radiopharmaceutical studies. In radiopharmaceutical research laboratories, it is important that the labeled compound is obtained in high yields. Radiolabeled agents may contain impurities like unlabeled radionuclide used for radiolabeling, with degradation products formed during oxidation or reduction of radionuclide and secondary complexes which should be formed during radiolabeling reaction. Thus, the estimation of impurities in the radiolabeled compounds is significant.99mTc-ibandronate sodium (99mTc-IBD), was developed and quality control studies were achieved by using RTLC and paper electrophoresis methods. For this purpose, different stationary and mobile phases were used and ideal TLC system conditions were developed. Furthermore, paper electrophoresis studies were performed for each formulation. 99mTc-IBD complex was prepared by using different reducing agent concentrations. Some parameters like effect of antioxidant agent and pH on labeling yield were also investigated. For quality control methods, Whatman 1 MM and 3 MM papers, silica gel (SG) coated fiber sheets and instant thin layer chromatography SG (ITLC-SG) plates were used as stationary phase and acetone, physiologic solution, methylethylketon, acetonitrile/water/ trifluoroacetic acid, butanol/ethanol/water solutions were used as mobile phases.
M.A. Ebiad
Egyptian petroleum research institute, Egypt
Title: Distribution of naphthalene, phenanthrene and their alkyl substituents in some Egyptian crude oils as a tool of thermal maturity assessment
Biography:
M A Ebiad is an Assistant Professor, and Researcher of Physical Chemistry at Egyptian Petroleum Research Institute. Since the last three years he has been the Head of Gas Chromatography Lab, Analysis and Evaluation Department. He has active effort in the demonstrations of central lab for services. He has 20 research articles in different physical chemistry research area. He develops many gas chromatographic applications in the lab such as PVT study, geochemistry, trace analysis for sulfur and inverse gas chromatography. He also participate in three research projects using GC-MS: Project for biomarker for Suez Gulf region as a data base for Egyptian crude oil, supported by EPRI; STDF project “Finger printing of some Egyptian crude oil via GC-MS in relation to their biomarker” and; Gas analyzer MS (HIDDEN) in STDF project "The development of recent catalysts and membrane reactors for dry reforming of natural gas using CO2
Abstract:
The distribution of alkylated polycyclic aromatic compounds (PACs) is highly variable in hydrocarbon mixtures. This is because the concentrations are controlled by both the nature of the source organic matter and the conditions of diagenesis/thermal maturation. Different organic matter sources yield bitumen’s with varying amounts of PACs and different patterns of alkylation. Aromatic fractions separated from seven different Egyptian crude oils, having different geological origins, were analyzed by gas chromatography– mass spectrometry (GC/MS) especially for the generated alkylnaphthalenes and alkylphenanthrenes. Naphthalene (N), methylnaphthalenes (MN), dimethylnaphthalenes (DMN), trimethylnaphthalenes (TMN) and tetramethylnaphthalenes (TeMN) has been identified in the m/z (128, 142, 156, 170 and 184) mass chromatograms. Phenanthrene (P), methylphenanthrene (MP), dimethylphenanthrene (DMP), and trimethylphenanthrene (TMP) isomers have been identified in the m/z (178, 192, 206 and 220) mass chromatograms. Ratios depending on the differences in the thermal stability of the isomers were applied (e.g. MPI, MPr, MNr, DMNr, TMNr2, etc.). The ratios of β-substituted to α-substituted isomers of both alkylnaphthalenes and alkylphenanthrenes revealed higher maturity of ND1 from Quassim formation in Nile Delta basin compared to other samples. WD1 oil samples from Faghur basin is characterized by a high abundance of 1,3,7- and 2,3,7-trimethylnaphthalenes (TMN) with (TMNr2=1.154) and high Pristan/Phytan ratio (Pr/Ph=2.63) compared to WD2 from the same basin suggesting in-reservoir mixing of crude oils of different maturities.
Biography:
Adeyemi A Abati has completed his MBBS in 2004 at Obafemi Awolowo University Teaching Hospital Ile–Ife Nigeria, he was trained at the Department of Infectious Diseases during his residency and he provided several superior care and consultation that resulted in overall improvement of department patient’s satisfaction Quotient. He focused on patient’s treatment and re-evaluated several methods of therapy management dependent on infection types tailored to patient’s individual patient history and efficacy of previous treatments. He completed is Master’s degree in Public Health at the same institution. He has been practicing in Department of Infectious Disease at Lagos University Teaching Hospital, one of the top three infection disease hospital in Nigeria and also doing his PhD at the moment. He holds certifications from Nigerian Board of Internal Medicine for Hematology and Infectious Disease and also awarded the Ward of the Developing Leader in Medicine from Nigerian Medical Association, in 2010 for his excellent contribution towards the general treatment reduction of infectious disease in Nigeria
Abstract:
In Nigeria, Hepatitis C virus (HCV) infection is primarily spread through injection drug use. There is an urgent need to improve access to care for HCV among persons with opioid use disorders who inject drugs. The purpose of our study was to determine the prevalence of HCV, patient characteristics, and receipt of appropriate care in a sample of patients treated with buprenorphine for their opioid use disorders in a primary care setting. This study used retrospective clinical data from the electronic medical record. the study population included patients receiving buprenorphine in the office based opioid treatment (Obot) clinic within the adult primary medicine clinic at Lagos Medical Center between October 2008 and August 2015 who received a conclusive HCV antibody Ab test within a year of clinic entry. We compared characteristics by HCV serostatus using Pearson’s chi-square and provided numbers/percentages receiving appropriate care. The sample comprised 300 patients. slightly less than half of all patients (n=134, 27.7%) were HCV Ab positive, and were significantly more likely to be older Hausas and Yoruba’s, have diagnoses of post-traumatic stress disorder (PTSD) and bipolar disorder, have prior heroin or cocaine use, and be HIV- infected. among the 134 HCV Ab positive patients, 126 (67.7%) had detectable HCV ribonucleic acid (RNA) indicating chronic HCV infection; only eight patients (2.21%) with chronic HCV infection ever initiated treatment. Nearly half of patients (47.7%) receiving office-based treatment with buprenorphine for their opioid use disorder had a positive Hepatitis C virus antibody screening test, although initiation of HCV treatment was nearly non- existent (2.21%).
F.Picchioni
University of Groningen, The Netherlands
Title: Product development and simulations for Enhanced Oil recovery (EOR)
Biography:
F.Picchioni has completed his PhD in 2000 from the University of Pisa (Italy) and postdoctoral studies from the Technical University of Eindhoven (The Netherlands). Since 2013 he is full professor and chair of the group Chemcial Product Engineering at the University of Groningen (The Netherlands). He has published more than 100 papers in reputed journals.
Abstract:
Chemical Enhanced Oil Recovery (EOR) is currently and mainly based on the use of partially hydrolyzed polyacrylamide as water-soluble polymer for mobility control. This choice is predominantly related to technological (thickening efficiency) as well as economic considerations. However, the presence of salt in the underground water significantly reduces the effect of such polymer on the solution rheology. This becomes even less when the polymer is used in combination with alkali. Therefore the amount of polymer required is significantly higher than expected on the basis of simple rheological models, which in turn has a clear negative effect on the economics of the process. Against this backdrop, the search for alternative water-soluble polymers has been gaining a predominant attention at both academic and industrial level. In this work we report on the synthesis and use of branched non-ionic polyacrylamide solutions for EOR. The polymers have been prepared by controlled radical polymerization to yield well-defined structure with variable number and length of the arms. The rheological behavior has been investigated as function of the macromolecular architecture as well as of concentration and presence of salt. The obtained results clearly indicate the validity of this approach since the thickening capability of the branched polymers is clearly improved with respect to the linear ones. Moreover, the non-ionic character of the material renders it insensitive in terms of solution viscosity to the presence of salts. Last but not least, the branched structure also confers to this material a slightly more prominent resistance to alkaline hydrolysis with respect to the linear ones.
Fernando X. Moreira
University of Porto, Portugal
Title: :Liquid chromatography tandem mass spectrometry for the doping control of beta-agonists and corticosteroids in racing pigeons
Biography:
Fernando Moreira is a Professor at School of Health of Polytechnic Institute of Portugal and PhD student of Forensic Sciences in Medicine Faculty of University of Porto, currently developing control doping methods at the Toxicology Laboratory of Department of Biological Sciences of Faculty of Pharmacy of University of Porto. His expertise is in developing analytical methods for the detection and quantification of substances in complex biological matrices that also enables the clarification of pharmacokinetics events of drugs.
Abstract:
Statement of the Problem: Pigeon racing is an ancient sport, practiced by fanciers all over the world, on a weekly basis. Although the natural skills of pigeons are truly amazing, with these birds traveling hundreds of kilometers for several hours in a row, fanciers still struggle to find strategies to improve them. Unfortunately, the use of performance enhancing drugs in racing pigeons is one of these common strategies, threatening animal welfare, compromising equality of opportunity and ensuring unfair financial gains for cheaters. Despite the existence of rules and legislation that forbidden the administration of drugs to pigeons for performance enhancing purposes, it is generally acknowledged that doping control is being neglected in several countries. The number of studies presenting analytical methods for the control of these illicit practices in pigeons is minimal, probably given the nature of the available analytical matrix (faeces), and the low dosages applied to these small animals. Methodology: A liquid chromatography tandem mass spectrometry method was developed and validated for the detection and quantification of a beta-agonist (clenbuterol) and three corticosteroids (betamethasone, prednisolone and budesonide) in faeces from pigeons, after an extraction protocol combining liquid-liquid extraction and solid-phase extraction. Main results: The newly developed method was validated concerning selectivity, linearity (with coefficients of determination always greater than 0.99), accuracy (87.5–114.9 %), inter-day and intra-day precisions, limits of detection (0.14-1.81 ng/g) and limits of quantification (0.49-6.08 ng/g), stability and extraction recovery (71.0 %-99.3 %). The method adequacy was evidenced after the unequivocal detection of betamethasone in faeces from two racing pigeons that had been orally administered betamethasone. Conclusion & Significance: The method performance is suitable for doping control analysis purposes and can be easily adapted to doping control laboratorial routine procedures in order to enforce current laws.
Biography:
Dr. Poyraz has completed his PhD at Auburn University (Alabama/USA). He is an assistant professor of Department of Textile Engineering at Adiyaman University. He has published 22 papers in reputed journals and has been serving as a scientific researcher for his field of interest.
Abstract:
A hybrid electrode material (HEM), composed of carbonized conducting polymer (CP), i.e. polypyrrole nanofibers (PPy NFs), nanostructured zinc oxide (nano-ZnO) and carbon nanotubes (CNTs), was prepared for energy storage applications. HEMs were obtained through a one-step, hassle-free, rapid and highly efficient microwave (MW) energy-based approach. The overall morphology and content of the nano-ZnO and CNT compounds could be altered by simply changing the process parameters, i.e. ratios in the feedstock mixture or the MW process time. The thermal and morphological features, crystalline nature, elemental composition and also the electrochemical performance of the as-prepared HEMs were thoroughly investigated by using relevant material characterization methods such as scanning and transmission electron microscopy (SEM, TEM), energy dispersive X-ray spectroscopy (EDX), cycling voltammetry (CV) and galvanostatic charge/discharge (CD) tests. It was revealed that by synergistically blending the high conductivity from CNTs, the ultra-high porous surface area from carbonized NFs and the abundant pseudo-capacitive features from nano-ZnO in its structure, the as-synthesized HEMs could afford to exhibit promising capacitive performance (~ 190 F/g at 2 mV/s), excellent long-term CD stability (~ 90% during 2000 cycles), high energy and power densities (~ 35 Wh/kg at 500 W/kg) along with high specific surface area (~ 35 m2/g) for energy storage applications.
H. TAOUIL
Hassan II University of Casablanca, Morocco
Title: :Detection of Ca2+, Mg2+, CO32- and SO42- in Wells of Talsint Region (Eastern Morocco) by Ionic Chromatography
Biography:
Abstract:
Applications using supercritical water often encounter the presence of inorganic compounds in feed streams, most often with a minor concentration. These compounds can lead to damage of the equipment via erosion, scaling and corrosion or can influence and disturb the main reaction and processes inside the systems. In order to avoid these problems and to predict the influence of these compounds, it is vital to possess knowledge of the chemical composition of the most common inorganic compounds in supercritical water. For this, the spatial variation of calcium, magnesium, bicarbonate and sulfate were investigated during low flow periods of the year 2011 at five wells level in the Takamine area, Talsint region, Eastern Morocco, using ionic chromatography method. The obtained results show that in the majority of wells, their values are higher than the values set by the WHO (Ca2+: 270 mg.L-1; Mg2+: 50 mg.L-1 and SO42-: 500 mg L-1). However, the total permanent hardness values in all studied stations were found higher indicating that these waters are very hard. These can be explained by the calcareous nature of the geological terrain where traversed by water. Finally, the majority of the studied water wells have a scale or corrosion character. This result limits the use of groundwater as drinking and cooling water in this area.
- Poster Presentation
Location: Salon 2+3
Chair
Gilles Goetz
Pfizer, USA
Session Introduction
Maryam Salimi
Tehran Province Water and Waste water Company, Iran
Title: :Optimization of dispersive liquid-liquid microextraction (DLLME) method for determination of 2, 4-D and MCPA in water by HPLC with using Box-Behnken design
Biography:
Maryam Salimi worked (2000-2006) as Analytical Chemist in QC Laboratory of Pharmaceuticals and worked (2006-2018) as a Researcher and Analytical Chemist in Organic Laboratory of Tehran Province Water and Wastewater Company.
Abstract:
This paper describes the optimization of DLLME method for determination of Chlorophenoxy herbicides including 2, 4 D and MCPA by high-performance liquid chromatography (HPLC). For DLLME, a mixture of extraction solvent (Ethyl acetate, 0.35 ml for 2,4 D and 0.6 ml for MCPA) and dispersive solvent (acetonitrile, 0.65 ml for 2,4 D and 0.4 ml for MCPA), were rapidly injected into water sample for the formation of cloudy solution. The analysis was performed on a high-performance liquid chromatography (HPLC) system with a C18 column (250×4.6 mm, i.e.), and mobile phase contain of 0.05 M H3 PO4/acetonitrile (90:10) to 100 acetonitrile in 30 minutes. The flow rate was 1 mL min−1, and the chromatogram was monitored at a wavelength of 280 nm. In this study, the effects of concentration of sample, pH, volume of solvent extraction, extraction time in the distributed liquid-liquid extraction have been examined and optimal conditions were obtained using the Box-Behnken
Miriam Sannomiya
Universidade de São Paulo, Brazil
Title: The effect of seasonality on the production of essential oils from leaves of Eugenia uniflora
Biography:
Miriam Sannomiya has completed her PhD from University of Campinas and Post-doctoral studies from São Paulo State University at Araraquara. She is an Assistant Professor level 2 at this University since 2008. She worked with the natural products’ research in her Masters’, PhD and Post-doctoral studies. She has experience in Organic Chemistry with emphasis on chemistry of natural products, mainly in the following subjects like bioprospecting of natural products (Fabaceae, Malpighiaceae, Byrsonima, Lonchocarpus, Platymiscium, Machaerium, flavonoids and galloylquinic acid derivatives) and effects in the production of secondary metabolites. She is a Professor at Graduate Program in sustainability at the School of Arts, Sciences and Humanities since 2017. She has published more than 40 papers in reputed journals and has been serving as an Editorial Board Member of repute.
Abstract:
Eugenia uniflora L., popularly known as “cherry”; refers to a highly adapted to urban environments species and highly contaminated by airborne pollutants. In this sense, a comparative study of the content of essential oils present in the leaves of E. uniflora specimens occurring in the metropolitan region of São Paulo and in the municipal park at Mogi Cruzes-SP as well as the study of chemical composition in different seasons, can allow a better understanding of the contribution of each of these variables in the production of secondary metabolites. The chemical analysis of the different leaf extracts by GC/MS of 2 individuals of Eugenia uniflora showed a difference in the chemical profile due to its location as well as the seasonality. Regarding the essential oils, it was possible to observe that the samples collected in Mogi das Cruzes (São Paulo- Brazil) Park show a greater diversity of secondary metabolites than the samples that occur in the vicinity of the School of Arts, Sciences and Humanities (USP-Campus Leste), which is located in the Tietê Ecological Park, in the vicinal of the Ayrton Senna highway. The data showed a greater diversity of secondary metabolites in the oil samples extracted in the Tietê Park region. The greater contact with the atmospheric gases like CO2 emitted by the means of transport, can serve as source of C for the production of secondary metabolites. The higher production of the secondary metabolites during the winter and spring seasons, can be associated in the transference of the essential oils to the leaves for the pollination process. The low production of secondary metabolites during summer is possibly associated with high water precipitation during this season, which removes much of the CO2 from the atmosphere, thereby decreasing the supply of C to produce the compounds.
Beatriz Fucuda Nascimento
Universidade de São Paulo, Brazil
Title: Phenolic compounds present on the leaves of Eugenia uniflora identify by HPLC - IR
Biography:
Beatriz Fucuda Nascimento has completed her graduation at the age of 23 years from University of Mogi das Cruzes. Before that she did technical course, during one year and a half, which in that time, her goal was work in industrial branch. During her graduation, she did the internship at University of São Paulo, in an Organic lab with emphasis on Chemistry of Natural Products, directed by the Professor Doc. Miriam Sannomiya. During her internship, she discorvered the academic world and how grateful it is to work in research. Currently, she is working to improve her curriculum lattes in search of getting a master’s degree, either working to publish papers or going to congresses.
Abstract:
Eugenia uniflora L. are popularly known as “brazilian cherry” and it is consumed by brazilian people, known as antihypertensive, antirheumatic, diuretic, antipyretic astringent and for the treatment of digestive disorders. Studies report an anti-inflammatory effect throught the infusion of dry leaves. E. uniflora belongs to Myrtaceae family. This family presents 132 genus and 5.671 species, where these species are recognized by the presence of essencial oils, flavonoids, phenolic compounds, alkaloids and saponins.The plant material of E. uniflora was collected on Tropical Municipal Park Francisco Affonso de Mello, located in Mogi das Cruzes, São Paulo – Brazil. After drying and milling, the leaves of E. uniflora was extracted by percolation in 80% ethanol solution. A portion of 20 g of the dryed extract was resuspended in ethyl acetate and water 1:1 (v/v). The fraction ethyl acetate was evaporated, obtaining 3,3 g. This fraction was dissolved in 12 mL of methanol/water 80:20 (v/v) and after centrifugation, the superior part was fractionated in column LH-20 (methanol as mobile phase), getting 108 fraction of 5 mL each. Analyses made with TLC using as mobile phase chloroform/methanol/water 80:18:2 (v/v), allowed grouping the fractions of same chromatographic profile. The study of the fractions 16-28, 29-32 and 33-39 and analyses in scale semipreparative resulted in the isolation of 7 compouds. The analyses of the spectroscopy datas of RMN 1H, 13C, bidimentional experients of HSQC, HMBC e COSY, allowed to identify the compounds as being gallic acid, ethyl gallate, 3-galloyl quinic acid, 5-galloyl quinic acid, quercetin-3-O-rhamnopyranoside and miricetin-3-O-rhamnopyranoside. The ethyl gallate was described by the first time in E. uniflora.
Sevil Çetinkaya
Kirikkale University, Turkey
Title: Kinetics and Thermodynamics of Asphaltene Adsorption on Nanocomposite PolyHIPEs
Biography:
Sevil Çetinkaya is a Professor of Inorganic Chemistry in the Department of Chemistry at Kirikkale University. She obtained her Ph.D. in Inorganic Chemistry at Hacettepe University in 2003. She joined the Kirikkale University as an Assistant Professor in 2006 and became an full Professor in 2013. Her current research interests focused on organometallic chemistry, design, preparation and applications of nanomaterials and porous carbon materials.
Abstract:
Asphaltene precipitation is one of the most important problems of the petroleum industry. Asphaltene collapses during petroleum processing and extraction from the well, blocking the pipes and causing many problems. For this reason, asphaltene should be removed from heavy oils. The main objective of this study was to synthesize new nanocomposite materials to be used in oil industry to prevent asphaltene deposition. The adsorption of asphaltenes from toluene solutions onto NiO/polyHIPE nanocomposite was investigated in detail. Asphaltene adsorption capacities of the polyHIPE-based nanocomposites were determined. Asphaltene adsorption kinetics and isotherms were obtained. It was seen that the pseudo-second-order model provided a good fit for the experimental data while the pseudo-first-order model did not. It is concluded that the synthesized and characterized polymer nanocomposites are important for the oil industry owing to having potential use as an adsorbent. The authors thank the Scientific and Technological Research Council of Turkey (TUBÄ°TAK) for the financial support for this study (Project No. 214Z074).
Rabia YeÅŸil
Kirikkale University, Turkey
Title: Synthesis of Mn3O4/PolyDCPD Nanocomposite Materials by HIPE and ROMP Approaches
Biography:
Rabia Yeşil is currently a MSc student in the Department of Chemistry at Kirikkale University (Turkey). She graduated from Kırıkkale University Chemistry Department in 2015. She is working on a research project as a scholar. Her research interests include nanocomposite synthesis and applications.
Abstract:
In recent years, polyHIPEs with high porosity derived from high internal emulsions are being widely studied. PolyHIPEs are important in some areas such as cell culture, pure protein constructions, enzyme immobilization, water and carbon dioxide treatment, hydrogen storage and sensor materials. Due to unstable and brittle structure, their uses in industrial areas have not become more widespread. To improve the poor mechanical properties of polyHIPE foams, polyDCPD was prepared via ring opening metathesis polymerization (ROMP). In this study, dicyclopentadiene (DCPD)-based nanocomposite materials containing Mn3O4 nanoparticle (NP) have been synthesized for the first time. Nanocomposites were synthesized by the polymerization of a continuous phase of high internal phase emulsions containing Mn3O4 NPs. In these syntheses, deionized water was used as an internal phase, Pluronic-L121 was used as surfactant, and ruthenium alkylidene catalyst was used as the initiator. The effect of nanoparticle amounts on the structure of nanocomposites was examined in detail (Fig. 1). The prepared nanocomposites were characterized by SEM, BET surface area, FTIR, DSC and TGA analysis. Authors would like to thank Kirikkale University Scientific Research Projects Coordination Unit (Turkey) (Project No. 2017/073) for financial support of this work.
Kuralay Korzhynbayeva
Nazarbayev University, Kazakhstan
Title: Rheological behaviour of polymers as the key for developing the extrusion die design
Biography:
K.Korzhynbayeva has completed his PhD at the age of 30 years from Al-Farabi Kazakh National University and postdoc at the Nazarbayev University School of Science and Technology. She has published more than 15 papers in international an kazakhstani journals.
Abstract:
Today, the World was observing an increased demand in polymers – low-cost and lightweight materials that currently substitute traditional materials such as metals, glass and paper in many applications. The design flexibility that the polymers offer make them extremely valuable for such end industries as construction, packaging, automotive, telecommunication and other related industries.
Polypropylene (PP) is a flexible polymer with diverse applications, including flexible packaging, polymer banknotes, and engineering materials. PP has low density, a higher melting point (about 160 oC) and excellent chemical resistance. This suggests that PP is suitable for injection molding (for heavier-duty applications such as safety helmets, electrical tools, TV casing, etc.), blow molding (for stronger containers such as bottles, tubs, fuel tanks) and extrusion processing techniques (for packaging). Extrusion technique is the most common mashines in polymer processing industry. Extrusion is one of the promising method to prepare different thin films for packaging, which can be defined as the act of a shaping a polymer material by forcing through a die by means of pressure [1].
Rheological data of polymers can be used in determining whether or not a type of polymer can be extruded. It helps in determining the optimal design of extrusion die design, screw geometries of an extrusion technique, various mould cavities for injection moulding.
Viscoplasticity of polymers are characterized by a yield stress, below which the materials will not deform, and above which they will deform and flow according to different constitutive relations. Viscoplastic models include the Bingham plastic, the Herschel Bulkley model, and the Casson model. The Casson model can be used to estimate values of parameters that help characterize the rheological behavior of a polymer materials that exhibit yield stress.
In this work we report about trials to use the Casson model for certain type of polypropylene homo- and copolymers used by local companies. Based on these rheological data, we intent improved designs of the coathanger die for local PP thin film are presented with Casson and power law models. More detailed information of our presented work will be provided on the Poster session.