Day 1 :
Keynote Forum
Norberto A. Guzman
Princeton Biochemicals, Inc., U.S.A
Keynote: Immunoaffinity Capillary Electrophoresis Technology: A Powerful Tool for the Understanding of the Role of Food-Derived Peptides in Wellness and Disease
Biography:
Dr. Norberto Guzman received a B.Sc. degree in biochemistry from the University of Chile, Santiago, Chile; a M.Sc. degree in biochemistry (cell and molecular biology) from the Medical College of Georgia, Augusta, Georgia, U.S.A.; and a Ph.D. degree in biochemistry from a Joint Graduate Program of the University of Medicine and Dentistry of New Jersey-Robert Wood Johnson Medical School and Rutgers, The State University of New Jersey, New Brunswick, New Jersey, U.S.A. Dr. Guzman has worked for the last 30 years in academic medical institutions, diagnostic and pharmaceutical companies, including Mount Sinai School of Medicine, Roche Diagnostic Systems, Hoffman-La Roche, and Johnson & Johnson. He is currently the Chief Scientific Officer at Princeton Biochemicals, Inc. Princeton, New Jersey, U.S.A. His main research interest is in the studies of protein biomarkers in biological fluids using miniaturized immunoaffinity capillary electrophoresis instruments.
Abstract:
The human body is home to a unique microbial population, including bacteria, archaea, fungi, and viruses. Most of the human body’s microbiota is located in the gut and its composition changes throughout life, with lower diversity in infants and elderly people. A woman’s microbiota even changes during pregnancy. The main role of the microbiota is to degrade larger polymeric substances into smaller compounds that serve as nutrients for the rest of the microbiota community and for the human body as nutrients and building-block components of genetic materials, proteins, polysaccharides, lipids and other molecules essentials for life. Both human and animal research are increasingly showing the influence of diet on the microbiota, and its potential in maintaining health and preventing disease. A better understanding of the dysregulation of microbiota host interactions is generating a paradigm shift in science understanding between bacteria and the human health environment. Changes to the type and the diversity of bacteria in the microbiota is known as dysbiosis, and has been linked to a variety of diseases, including obesity, immune-related and inflammatory bowel disease, cancer and cardiovascular disease.
Our laboratory has been interested in comprehending the effect of food-derived peptides that are generated by the microbiota from casein and gluten, and transported to the blood stream that have been associated in some people with certain non-communicable diseases such as autism, schizophrenia, type I diabetes, heart disease, celiac disease, sudden infant death syndrome, mild allergies, and other disorders. We are using a portable point-of-care instrument, based on immunoaffinity capillary electrophoresis (IACE), for the determination of casomorphins and gliadins in biosamples. IACE is a two-dimensional technology that consists of the use of immuno-capture techniques found in some immunoassays, such as enzyme-linked immunosorbent assay (ELISA) and pairs it with a high-resolution analytical separation technique, such as capillary electrophoresis.
Conceptually, research and development into the role of diet, biology of the gut and its microbiota, and the way that each of these parameters influence health and disease, have a potential to open a whole new arena of healthcare, playing a key role in prevention, prediction and treatment of disease.
Keynote Forum
Dušan Berek
Polymer Institute, Slovak Academy of Sciences, Slovakia
Keynote: Retention Mechanisms in Liquid Chromatography of Synthetic Polymers
Biography:
Employed at Polymer Institute, Slovak Academy of Sciences in Bratislava. Served as elected member of the Presidium of the Slovak Academy of Sciences, President of the Slovak Chemical Society, Chairman of the Czecho-Slovak and Slovak National Committee of Chemistry for IUPAC. Corresponding member of the Central European Academy of Sciences and member of the Learned Society of the Slovak Academy of Sciences. Author or co-author of two monographs and 250+ scientific papers in extenso published in refereed periodicals, proceedings and chapters of books, as well as 60+ patents (four of them were licensed) - cited more than 2,000x. Presented over 110 invited plenary, key and main lectures, as well as over 900 regular lectures and poster contributions on symposia and conferences and during lecturing tours to over fourty countries. Elected „Slovak scientist of the year 1999“ and „Slovak innovator of the year 2001“.
Abstract:
At present, methods of liquid chromatography, LC, provide the most important information on both average values and distributions of molecular characteristics – molar mass, chemical structure (composition) and physical architecture (topology) of synthetic macromolecules.
Gel permeation (size exclusion) chromatography, GPC/SEC, is commonly employed for determination of molar mass of macromolecules. Its basic retention mechanism is steric exclusion based on the changes of conformational entropy of coiled macromolecules entering the pores of the column packing. However, GPC/SEC cannot give information about polymer molar mass in presence of the changing second or even third molecular characteristic. To simultaneously determine two molecular characteristcs of complex polymer such as copolymers or polymer blends, the entropy controlled retention mechanism is combined, coupled with the interaction retention mechanisms. The most common interaction retention mechanism employed in coupled LC methods is adsorption i.e. the distribution of solute between a solid surface and a volume of its solution in a mobile phase. Adsorption usually results from the polar interactions among active sites on macromolecules and on the column packing surface, which are controlled by eluent polarity and less often by temperature. The appropriate stationary phase is bare silica gel. Another LC retention mechanism is absorption, (enthapic partition), the distribution of a solute between the volumes of mobile and stationary phases. The practically applicable volume of LC stationary phase is produced by the chemical attachment, bonding of appropriate groups usually C18 alkyl groups onto a carrier, mainly silica gel.
In practice, both adsorption and enthalpic partition retention mechanisms are applied either isocratically or applying mobile phase with the gradually changing composition. All enthaphy based processes in the LC columns are accompanied with the large changes of conformational entropy of macromolecules so that all coupled polymer LC procedures present a combination of enthalpy and entropy based processes.
Keynote Forum
Károly Héberger
Hungarian Academy of Sciences, Hungary
Keynote: Separation selectivity of liquid chromatographic columns. A comparison by nonparametric methods
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 3500 times (without self - citations and cross - references). More information can be found at: http://aki.ttk.mta.hu/scientist/heberger/
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 ten highly similar columns (C18-bonded silica stationary phases).1 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 show 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.5 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 HSM evaluation is used.
The ranking (clustering) pattern of chromatographic columns based on retention data (logk values) of 67 compounds, and selectivity parameters of hydrophobic-subtraction model (HSM) provided various column groupings. Loss of information is inevitable if 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.1
Keynote Forum
Hong Xue
Hong Kong University of Science and Technology, Hong Kong
Keynote: Dispersed Mobile-Phase Countercurrent Chromatography
Time : 10:30-11:00
Biography:
Dr. Xue obtained her M.D. from the Shanghai Second Military Medical University in 1983, Ph.D. from the Institute of medical Sciences and Department of Biochemistry, University of Toronto in 1992, and carried out postdoctoral studies at the Department of Genetics, University of Glasgow before joining the Department of Biochemistry, Hong Kong University of Science & Technology (HKUST). Currently, Dr. Xue is Director of Applied Genomics Center of HKUST, and Professor of Life Science at Hong Kong University of Science and Technology. Dr. Xue’s 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, Dr. Xue and her team discovered the association between schizophrenia and a segment of the GABRB2 gene encoding the ï¢ï€²-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 ï¢ï€²ï€ 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| Hyphenated Techniques in Chromatography | Analytical Chromatography | Novel Techniques in Chromatography | Advances in Gas Chromatography
Session Introduction
Gilles Goetz
Pfizer, USA
Title: EPSA: A Novel Supercritical Fluid Chromatography Technique Enabling the Design of Permeable Cyclic Peptides
Biography:
Gilles Goetz is a Principal Scientist at Pfizer in Groton, Connecticut, USA. Gilles received his B.Sc. (1991) and Ph.D. (1995) at the University of Strasbourg in France. After post docs 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 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 5 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.
Abraham George
ADNOC Refining Research Centre, UAE
Title: Methyl Tertiary Butyl Ether in heavy hydrocarbon matrix: Identification and quantification using Gas Chromatography Headspace Technique
Biography:
Mr. 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 & Laboratory Analysis. He Graduated in Chemistry and obtained Master’s Degree in Business Administration from Mahatma Gandhi University, India. Worked in various capacities in managing laboratories in India, Saudi Arabia and in U.A.E 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 & Heavy Vacuum Gas Oils (LVGO & 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 Gasoil, Heavy Vacuum Gasoil, 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. 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 derived 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
China Academy of Engineering Physics, China
Title: Application of Metal-Organic Framework Material in Hydrogen Isotope Chromatographic Separation and Analysis
Biography:
Dawei Cao is a PhD candidate under the supervision of Prof. Shuming Peng (China Academy of Engineering Physics) and Prof. Zhengjun Zhang (Tsinghua University). He graduated 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 realizing the peaceful utilization of nuclear fusion energy, moreover, gas atmosphere in the process flow of ITER fuel cycle is more than complexity. Thus, making effective separation and analysis of hydrogen isotopic mixtures 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:
With a background in analytical chemistry, I had the opportunity of developing my thesis in collaboration with an enterprise dedicated to the production of fluorinated substances. The aim of the researches was focused on the development of fast and green analytical methods, for the quality control and production processes to be implemented. Through my experience in development of analytical methods, it has allowed me to work on a variety of analytes such as inorganics, organics in liquid or solid state in different fields: industrial, environmental and forensic ones.
The experience acquired in the drug department since 2012, following a 2-years postdoctoral position, has been focused to: the development of the actual analytical methods for the routine analysis of major and minor components in heroin and cocaine illicit drugs by fast GC-MS, reporting caseworks for the tribunal of justice as well as the collaboration to obtain the ISO accreditation 17025 for the laboratories of the Service of Expertise in the drug department.
Abstract:
The present work is focus on the optimization and validation of the analytical method 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 some 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 interlaboratory 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).
Lourdes Hernandez de la Rosa
Center of Molecular Immunology, Cuba
Title: DNA removal on different chromatography supports used for EPO purification by spike studies
Biography:
Lourdes Hernández has her expertise in the design of purification process for recombinant proteins. She has 10 years of experience in the field of Biotechnology and held positions within development and project management. She holds a Master in Science in Engineering for Biotechnology Process from Faculty of Chemical Engineering in the Higher Polytechnic Institute José Antonio Echeverría, Havana, Cuba. Lourdes has involve in the evaluation and application of the new designs of chromatography supports for increase the productivity of the productive process of recombinant protein such as EPO and monoclonal antibodies.
Abstract:
Chromatographic techniques are employed in the purification step of hr-EPO production process in order to obtain a reliable product with high purity. Anion exchange chromatography supports have proved high efficient in removing contaminants such as DNA. For that reason the DNA removal was determined by spike studies, on three anion exchange chromatographic supports: gel, membrane and monolithic column; used in intermediate purification stage. This study showed that membrane and monolith columns have very good results in the removal of contaminants at this step. Log removal values (LRV) greater than 3.5 were obtained from DNA spike clearance studies. Monolithic column was determined as the best technological proposal, with more than 4 LRV and 7.72 mg DNA per mL of adsorbent. Scaling-up 8 fold of this step using monolithic column resulted in good process performance and DNA clearance. The results of this study may be used in the selection of commercially available chromatography supports for intermediate purification steps for other recombinant protein.
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.
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:
Tomasz Tuzimski is adjunct professor in Department of Physical Chemistry at Faculty of Pharmacy with Medical Analytics Division, Medical University of Lublin, Poland. Tomasz Tuzimski received MA degree and PhD degree (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 include the theory and application of liquid chromatography, extraction (QuEChERS) and detection techniques. He is authored or co-authored more than 62 scientific papers (IF = 100, H-index = 17). He is member of the editorial board of the Acta Chromatographica. He is quest editor of special sections on pesticide residues analysis in the JAOAC Int. Tomasz Tuzimski 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 hab. Tomasz Tuzimski is promoter of one doctorate (2017) and research work of 6 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, BADGE • 2HCl. As industrial chemical, BPA is widely used in the production of polycarbonate (PC) plastics (used in food contact materials, such as food containers, baby food and water bottles), epoxy resins (used as internal coating in canned food and beverage to prevent the food to get in contact with the metal wall and the deterioration of cans) and as an antioxidant in polyvinyl chloride (PVC) plastics in materials intended to come into contact with food (packaging cling films). Due to endocrine disruptor potential and estrogenic activity of the compound, the BPA release from packaging or storage containers into foods and beverages is a great public health concern. 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 paper was determination of xenobiotics (BPA and its analogues, pesticides, dyes) in natural and biological samples (e.g., breast milk) and food products.
Valentin A. Krylov
N. I. Lobachevskii Nizhny Novgorod State University, Russia
Title: Peculiarities of gas chromatographic-mass spectrometric determination of o-phthalic acid esters in low alcohol wines coupled with emulsion liquid-phase microextraction preconcentration
Biography:
V. A. Krylov, Doctor of Chemistry, Professor, Head of the Division of Analytical Chemistry of the Nizhny Novgorod State University. In 1980 – 2015 he was the head of the Laboratory of Analytical Chemistry of High Purity Substances at the Institute of the Chemistry of High Purity Substances of the Russian Academy of Sciences. The main direction of scientific research of professor Krylov is the development of the theory and applications of chromatography for the analysis of high purity substances, environmental objects and development of methods of the microextraction. The attained detection limits for molecular impurities constitute 10–6 to 10–11wt % and hit a record low. He is the author of more than 200 scientific papers, including reviews on the analytical chemistry of high purity volatile substances, air and liquid-liquid microextractionpreconcentration.
Abstract:
Esters of o-phthalic acid are very dangerous for human health. Their occurrence in wines is connected with the inflow from the plasticized polymer seals, plastic piping, tanks and stoppers. In this study the high sensitive gas chromatographic-mass spectrometric determination of phthalates in low alcoholic beverages (champagne, red and white wine) coupled ultrasound-assisted emulsification-microextraction was developed. As extractants environmentally friendly hydrocarbons - n-heptane and hexane are proposed.The sources of possible systematic errors were investigated: leaking of o-phthalates from chromatographic septum; contamination of phthalate in solvents; influence of macro components of wines(sugar, alcohol,anthocyanins); the hydrolysis of o-phthalates and others. For the first time it is shown that the impact of these factors can lead to an overestimation or underestimation of the actual concentration of impurities by 1-2 orders of magnitude. The methods of accounting or elimination of systematic errors are proposed. Purification of solvents by Rayleigh distillation method allows to obtain samples with impurity content lower than (1-4)∙10-3mgL-1. Containers for sampling and storage of samples to be analyzed should be made of borosilicate glass or quartz. The content of o-phthalates in wines was 0.03 - 1 mgL-1. The largest concentrations are characteristic for diethyl-, di-n-butyl- and di(2-ethylhexyl) о-phthalates.
The limits of detection of esters of о-phthalic acid in low alcohol beverages achieved are at the level of 10-6–10-5 mgL-1 and are highly competitive with the best world results. Therelative expanded uncertainty of the determination of toxicants is at the level of 13- 30%.
Xiaolong Fu
China Academy of Engineering Physics, China
Title: Sol-gel processed metal-organic frameworks capillaries for hydrogen isotopes separation
Biography:
Xiaolong Fu obtained his Ph. D. in physical chemistry in Institute of Chemistry, Chinese Academy of Sciences in 2015. Then, he joined 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 seperations.
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 1 min.
Gómez-López Alicia
Mycology Reference and Research Laboratory, Spain
Title: Triazoles Therapeutic Drug Monitoring: From recommendation to applicability
Biography:
Alicia Gómez López (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.
Dr Gomez-Lopez has worked in the production of over 79 papers published in scientific journals in the field of mycology and antifungal (2100 times cited, h-index 29), as well as training of fellows, pre-doctoral students, laboratory technicians and other lab management activities.
A total of 50 abstracts have been accepted for poster presentation in national and international Conferences. She has also participated in two Conferences as invited speaker (Expert Sessions).
As a result of activity of the group a technology-based company was created in 2009, Micología Molecular SL. This is a spin-off Of the ISCIII and its activities are focused in the development of new tools to detect fungal infections.
One patent have been obtained for the diagnosis of mycosis.
Abstract:
Background: 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.
Method: The proposed method consists in a simple high-pressure liquid chromatography assay using a stepwise gradient elution profile. It enables the simultaneous quantification of systemic azoles in 150μL of serum samples, after a first step of protein precipitation and direct injection of resulting supernatant. The analytical run enables the specific characterization of azoles by its UV profile. For the validation procedure (following international guidelines) linearity, accuracy and precision parameters were determined. We tested this method by monitoring azole serum concentrations in real clinical samples and using external quality controls. An additional description of the rate metabolite/parent drug is also determined to assess the relevance of metabolites on routinely azole TDM.
Results: The selectivity of the chromatographic procedure and PDA detection allowed good resolution. No significant interfering peaks were detected at similar retention times of the tested compounds. The chromatographic assay took 15 minutes per sample; the retention times were found to be: 7.30 ± 0.3, 9.50 ± 0.3, 11.6 ± 0.3, 11.7 ± 0.3, 12.6± 0.3 and 13.4 ± 0.3 minutes for VCZ N-oxide, VCZ, PCZ, OH-ICZ, ISvZ and ICZ, respectively. The validation procedure establishes that the method was linear between concentrations ranging from 0.25 and 16 mg/L for all components (analytical range). The correlation coefficient was higher than 0.9. Regarding the 115 samples received as part of an international quality control program, we found a high correlation between target and calculated concentration. A high percentage of the remaining clinical samples were received to assess VCZ and Noxide-VCZ (46% and 44% respectively). A great variability in concentration was observed among all the samples evaluated. We also found a high percentage of subtherapeutic samples (sbTh, samples in which azole did not reach the established concentration for efficacy). The mean VCZ Metabolic Rate (MR), established as the ratio between VCZ N-oxide /VCZ for each sample was estimated in 1.7-2, ranging between 0.09 and 25. In the case of ICZ, the mean MR was 1.3-2. No metabolites have been described for PCZ, so no MR was calculated. Significant MR differences were observed between samples. Higher values were found in sbTh samples compared to those for which upTh concentrations were detected.
Conclusions: This method resulted very simple, fast, cheap and very useful for TDM application, to improve clinical management of antifungal therapy in critically ill patients. According to the results described here, we suggest a role of MR on azole TDM.
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:
Dr. Mohamed Abd El-Salam Ebiad Ass. Prof. Researcher of physical chemistry at Egyptian petroleum research institute. The last 3 years is a 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 article in different physical chemistry research area. He develop 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 project 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”. 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 bitumens 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) have 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 (eg. 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.