Day 1 :
- Track 1: Advances in Sample Preparation Techniques
Track 2: Membrane Processes
Track 3: High-Impact Application Fields
Session Introduction
Yongjae Lee
Food Protein R&D Center at Texas A&M University, USA
Title: Membrane & Other Separation Technologies and Their Application to Food Technology
Biography:
Dr. Yongjae Lee is a Head of Separation Science at Food Protein R&D Center at Texas A&M University, USA. In this occupation he directly leads the Separation group in the lab and in the pilot plant research on the separation technologies of food, dairy, feed, beverage, specialty ingredients, biotechnology and biofuel, and oil & gas. He also hosts short courses in the area of membrane, and other traditional and advanced separations techniques. He has more than 12 years of industrial experience in the field of microbiology, chemical engineering, and agricultural engineering. He has published several papers in journals and has presented numerous invited lectures in various national and international meeting. Dr. Lee holds a Ph.D. in Animals & Veterinary Science from the Clemson University, Clemson, South Carolina, USA and a Master’s degree in Food Science & Technology from the Louisiana State University, Baton Rouge, Louisiana, USA.
Abstract:
In food industry, separation technology is broadly used to separate, isolate, and purify a particular component from a mixture. These are essential in the food manufacturing process. A numerous separation technologies are available such as using membrane, centrifuge, decanter, spray dryer, freeze dryer, and extractor. Especially, membrane technology has been broadly used in the food industry since 5-6 decades due to their processing at a lower temperature and less energy-intensive. Typically, Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF), and Reverse Osmosis (RO) are commonly used pressure-driven membrane separation in the food processing. These types differ in membrane characteristics, pore size, and operating pressure. The major membrane applications in the food are dairy and beverage industries. Microfiltration widely used to remove bacteria and spore, fat, and casein from skim milk. Ultrafiltration is used to remove lactose, and increase or decrease the protein content. Nanofiltration is used to concentrate and partially demineralize liquid products. Reverse osmosis is mainly used to remove water from a mixture which increase the product concentration with dehydration. Despite the many advantages of membrane technology, it has the key disadvantage which is the fouling of the membrane. It causes a reduction in flux rate and thus decreasing productivity over time. Back flux and chemical cleaning process can be applied to minimize the fouling but not perfect. Advanced technology such as grafted coating, zeolite, and graphene can be applied to solve the fouling issues.
Catia Algieri
Institute on Membrane Technology ITM-CNR, Italy
Title: MFI Zeolite Membranes for Water Desalination
Biography:
Catia Algieri is researcher at the Institute on Membrane Technology (ITM-CNR, ITALY) from 2001. Her research activity is focused on the preparation and characterization of organic and inorganic membranes for gas separations, water treatment and catalytic reactions. She has published many papers in reputable journals and she has presented numerous invited lectures in different international congresses. She is member of the Editorial Board in Journal of Crystallography and referee of several international Journals.
Abstract:
Zeolite membranes due to their crystalline structure and to their pore diameters close to the molecular size of different species have attracted the interest of many researchers in the separation processes field. They can be also used as membrane reactors owing to their high thermal and chemical resistance. Considering all these properties, water separation from organic solvents and water treatmentare other possible applications of these membranes. For example, about the ion removal from water, very interested in desalination process is the employ of MFI membranes, because their pore size (about 5.5 Å) is lower than the major kinetic diameters of various hydrated ions.In this work MFI zeolite membranes were synthesized on ï¡-Al2O3 tubular supports. In particular, the membranes were prepared by a secondary growth method using the cross-flow seeding procedure. Subsequently, these membranes were characterized by means of single gas and pure water permeation tests and then used in vacuum membrane distillation to investigate their potential application in water desalination.The membrane performance in distillation process was investigated using both distilled water and salt solutions with different NaCl concentration (0.2, 0.6 and 1.2 M) and using two different operating conditions. In the first case the membranes were tested in a continuous way without washing treatment. In the second one the system was washed at the end of each experiment.The results evidenced high and constant fluxes and salt rejection values higher than 98% for all the concentration considered.
Kirk J. Ziegler
University of Florida, USA
Title: The Role of Surfactant Structure in the Separation of Single Walled Carbon Nanotubes (SWCNTs)
Biography:
Professor Ziegler received his PhD in 2001 from the University of Texas at Austin. After a postdoctoral position in Prof. Smalley’s laboratory, he joined the Chemical Engineering Department at the University of Florida in 2005. His research group focuses on understanding the role of interfaces in one-dimensional nanostructures, such as single wall carbon nanotubes (SWCNTs) and vertical arrays of nanowires. His work on SWCNTs has focused on understanding the effect of surfactant-nanotube interactions on dispersion and separation processes. The ability to control these interfaces allow for efficient separation of SWCNTs and their integration into composite structures.
Abstract:
Single-chirality single walled carbon nanotubes (SWCNTs) have unique optoelectronic properties that can be utilized in specific applications, such as photovoltaics and biosensor. However, due to the large variety of SWCNTs and the difficulty of separation, the application of chiral SWCNTs is limited. The post-synthesis separation of SWCNTs has been studied with great interest in the past decade. The most promising techniques include the selective adsorption of SWCNTs onto hydrogel stationary phases and the aqueous two-phase extraction. The surfactant structure surrounding single walled carbon nanotubes (SWCNTs) plays an important role in their separation by nearly any method. However, characterizing the structure of these molecular layers remains difficult. The structure of the surfactant or other molecules around the SWCNTs could also have important implications in toxicology and drug delivery. Using our understanding of the surfactant structure surrounding SWCNTs, we developed high-fidelity separations of nanotubes by both selective adsorption and two-phase extraction. Finally, we will describe how these mono-chiral suspensions can be used in various applications.
Prof. (Neal) Tai-Shung Chung
National University of Singapore, Singapore
Title: Advanced separation technologies based on polymeric membranes for clean water and clean energy
Biography:
Prof. Chung had worked for US industries for 15 years before joining NUS in 1995. He is a Subject Editor of Chemical Engineering Research and Design and editorial board members of 15 journals including J. Membrane Science, AIChE J., I & EC Research, Separation and Purification Reviews, and others. He was an inventor of Hyflux Kristal™ 600 ultrafiltration membranes. He received IES (Institution of Engineers, Singapore) Prestigious Engineering Achievement Award, Hyflux-SNIC (Singapore National Institute of Chemistry) Award in Environmental Chemistry in 2010, and Research Leadership Award at NUS in 2011. He became a Fellow in the Academy of Engineering Singapore in 2012. He received the 2014 Underwood Medal for Exceptional Research in Separations from IChemE (Institute of Chemical Engineers, UK).
Abstract:
Clean water, clean energy, global warming and affordable healthcare are four major concerns globally resulting from clean water shortages, high fluctuations of oil prices, climate changes and high costs of healthcare. Clean water and public health are also highly related, while energy is essential for sustainable prosperity. Among many potential solutions, advances in membrane technology are one of the most direct, effective and feasible approaches to solve these sophisticated issues. Membrane technology is a fully integrated science and engineering which consists of materials science and engineering, chemistry and chemical engineering, separation and purification phenomena, environmental science and sustainability, statistical mechanics-based molecular simulation, process and product design. In this presentation, we will introduce our efforts on advanced membrane separation technologies for clean water (nano-filtration, membrane distillation, forward osmosis) and clean energy (osmotic power generation, natural gas, hydrogen, and biofuel). Technology breakthroughs in each area will be highlighted.
Hiroshi Uyama
Osaka University, Graduate School of Engineering, Japan
Title: Fabrication of Porous Monolithic Materials of Reactive Polymers for Protein Purification
Biography:
Hiroshi Uyama received his B.S. (1985) and M.S. (1987) from Kyoto University. In 1988, he joined the Department of Applied Chemistry, Tohoku University, as Research Associate and obtained Ph.D. He moved to the Department of Materials Chemistry, Kyoto University in 1997. In 2004, he was appointed as a full professor at the Department of Materials Chemistry, Osaka University. He has published over 270 original papers, 170 book chapters and reviews, and 140 patens.
Abstract:
Along with the rapid development of diagnosis and proteomic science, the requirement for the purification of biomolecules like proteins, enzymes and nucleic acids becomes extremely urgent. Protein A chromatography and immobilized metal ion affinity chromatography are regarded as the most efficient and promising methods for the protein purification. For these two techniques, the solid support is the crucial part for the protein purification efficiency and specificity. Polymer-based monoliths with tunable bulk and surface properties have attracted considerable attention due to their unique open-cellular three-dimensional porous structure. Recently, we have developed fabrication of such monolithic materials by phase separation of polymer solutions. The present talk deals with functional monoliths based on reactive polymers such as cellulose and poly(vinyl alcohol-co-ethylene) for protein purification. Protein A was introduced on the monolith of these polymers via suitable chemical activation. For an application of immobilized metal ion affinity chromatography, ethylenediaminetetra acetic acid was introduced into these monoliths and nickel ions were located subsequently. IgG and His-tagged proteins were immobilized on these activated monoliths. The protein purification amount and efficiency were evaluated.
Simona Liguori
Stanford University, Energy Resources Engineering Dept., USA
Title: Inorganic Metallic Membranes for Gas Separation
Biography:
Simona Liguori is a Physical Science Research Associate at Stanford University. She earned her MS in Chemical Engineering and PhD in Environmental Science and Sustainability. Se has over 8 years of research experience in membrane and membrane reactor technology related to the highly pure hydrogen production from bio-fuels reactions via membrane reactors and CO2 separation. She published more than 20 peer-reviewed articles; more than 10 chapters on international books on membrane science. Referee for several international scientific journals.
Abstract:
Currently, membrane technology for gas separation covers an important role in reducing the environmental impact and costs of industrial processes. In particular, it offers a number of benefits over other gas separation technologies as higher energy efficiencies, greater operational flexibility as well as simplicity of operation and maintenance. At the moment, polymeric membranes are the most widely used for gas separation. Nevertheless, some issues still remain regarding the scalability and reliability of the polymeric materials under real operational conditions where the temperature is often too high for polymer stability. Metallic membranes, by contrast, usually require high temperature for operation and may be more beneficial in saving energy under high temperature conditions. In particular, inorganic H2 selective membranes have gained a great attention in the field of the hydrogen economy development. Due to the characteristics of hydrogen perm-selectivity with respect to all other gases, palladium and its alloys play the role of dominant material in this field. Metallic membranes could be also used for N2 removal from natural gas or from coalfired flue gases located nearby the boiler exit, which may result in increased concentrations of CO2 and pollutants with a significantly reduced gas volume in the downstream, allowing for traditional emissions controls to perform more efficiently and, consequently, lowering the overall energy consumption and capital and operating costs. However, some issues need to be addressed, such as the development of thin membranes with long-term thermal and mechanical stability and resistant to the surface poisoning.
Mohammed W. Hakami
Yanbu Industrial College, Saudi Arabia
Title: Discharge times of 3.0 micron superfine powders from a circulating fluidized bed of a binary mixture
Biography:
Dr. Mohammed Hakami has completed his PhD in Chemical Engineering from Swansea University, United Kingdom on October 2013 in the field of water treatment using membrane. His work is in membrane technology. He is interested in separation techniques and he teaches separation process courses at Yanbu Industrial College. E-mail: mohhakus97@gmail.com
Abstract:
The high gas velocities in Circulating Fluidized Beds (CFBs) often result in fine powders becoming discharged and lost in the fluid going out at the cyclone upside stream. Thus, residence times of these fines in the bed will drastically fall together with the overall performance of the whole fluidizing system. The discharge time, TD, represents the time needed for all the fines to be discharged out of the bed. Therefore, the loading of superfine in the bed decreases. The discharge times of micron-size superfines from a semi-batch CFB were investigated using a binary mixture of superfine aluminium hydroxide powders (3.0 μm mean size) and coarse FCC particles (66 μm mean size). The discharge times of superfines are believed to be affected not only by gas humidity, but also by the water content of the bed particles. The effects of the equilibrium water content of FCC particles on the discharge times of superfines were investigated under different gas velocities and starting loadings of superfines of 3 and 5 wt.%. At a certain gas velocity, the discharge times decreased sharply using FCC particles of higher moisture contents as 0.054–0.067 wt H2O/wtdry FCC, irrespective of the loading of superfines. Dry FCC particles and FCC particles of lower moisture contents as 0.038 wt H2O/wtdry FCC, were found not to be appropriate for CFB as extremely large discharge times of superfines were obtained at higher loadings of superfines. High gas relative humidity at 85% could not decrease the discharge times of superfines in the presence of totally dry bed particles.
Z. Mansooria
Amirkabir University of Technology, Iran
Title: Wall Roughness Effect on Particle Separation Rate of The Turbulent Gas-Solid flow in inclined pipes
Biography:
Zohreh Mansoori completed her PhD in Mechanical Engineering from Amirkabir University of Technology ( Polythechnic), Tehran, Iran. She is associate professor and the head of Energy Research center in Amirkabir University. She has published more than 35 papers in reputed journals and has been serving as an editorial board member of repute.
Abstract:
The effect of wall surface roughness on the separation of solid particles in the turbulent gas-solid flow in the pipes with different inclination angles is studied. Inclined pipes are used in many industrial applications such as pneumatic transfer lines, heat exchangers and gas transport pipelines. The numerical model for 3D pipe considering four- way interaction is used to solve turbulence intensities for dynamic field. Interaction of the particles with rough wall is modeled introducing available stochastic wall roughness models for the dispersed phase to the computational program. It is assumed that the particles collide the wall surface would be omitted. It is found that changes in the particle dispersion and particle concentration results in the separation rate change in the different regions of the pipe. Also, the wall roughness could affect the particle- wall collision and the solid particle separation rate.
Ping Hu
China University of Petroleum, China
Title: High-efficiently simultaneous oxidation of organo-arsenic and immobilization of arsenic in Fenton enhanced plasma system
Biography:
Dr. Ping Hu currently working as professor at China University of Petroleum, Tsingtao, Shandong Sheng, China. He has published several publications as the first author or corresponding author in journals including Dual enhancement-inhibition roles of polycarboxylates in Cr(VI) reduction and organic pollutant oxidation in electrical plasma system
Abstract:
Roxarsone (ROX) is heavily utilized in agricultural applications and poses a risk to the environment. The applicability of glow discharge plasma (GDP) for simultaneous oxidation of organo-arsenic and immobilization of arsenic is unprecedentedly evaluated in this study. The results show that ROX can be effectively oxidized to inorganic arsenic and this performance is evidently dependent on energy input. Adding Fe(II) significantly enhances the oxidation of ROX mainly because of the additional production of •OH via Fenton reaction in GDP, accompanied with which the generated arsenic can be immobilized in one process. Arsenic immobilization can be favorably obtained at pH 4.0-6.0 and Fe(II) concentration from 500 to 1000 mM. Based on the mineral compositions and the analysis (XRD/FTIR/XPS) of precipitate, a mechanism can be proposed that the oxidation of Fe(II) by H2O2 generated in situ in GDP significantly accelerates ROX transformation to the ionic As(V), which can immediately co-precipitate with Fe(III) ions or be adsorbed on the ferric oxyhydroxides, forming amorphous ferric arsenate-bearing ferric oxyhydroxides. Consequently, the Fenton enhanced GDP process exhibits as an economical and versatile strategy for organo-arsenic oxidation and arsenic immobilization, holding a premise for the remediation of organic arsenic wastewater.
Marek Trojanowicz
Institute of Nuclear |Chemistry and Technology, Poland
Title: Biosensors as Detectors in High Performance Separation Techniques
Biography:
Marek Trojanowicz has completed his M.Sc., Ph.D. and D.Sci. degrees in Department of Chemistry, University of Warsaw. Currently he is full professor in Institute of Nuclear Chemistry and Technology in Warsaw, Poland. He is author of 300 scientific papers, 2 monographic books and editor of 1 book in the field of flow analysis and automation of analytical measurements. His main scientific interests include design of electrochemical sensors and biosensors, flow analysis, liquid chromatography and capillary electrophoresis, application of ionizing radiation for water and waste treatment and application of chemical analysis in archaeometry.
Abstract:
Biosensors are analytical devices incorporating a biological material e.g. tissue, microorganisms organelles, cell receptors, enzymes, antibodies, nucleic acids etc. intimately associated with or integrated with a physicochemical transducers using optical, electrochemical, thermometric, or piezoelectric properties. They have a solid place in contemporary analytical chemistry, which is evident from their very strong position on the market of analytical instruments, mass production of many of them, uncounted applications in various fields, and a very large research potential directed for this field in academia and industry. This is field of modern science and technology, which immediately adapts current achievements and discoveries in various branches of science, electronics, material science and micromechanics. Hyphenation of biosensing with separation methods can be realized practically with all types of biosensors, and many different electro migration and chromatographic methods. This can be a very efficient way for improvement of selectivity of biosensing, and with suitable design of the flow-through cell and whole measuring setup with on-line sample processing, it allows also improving sensitivity of whole analytical procedure. Another especially valuable application of this concept is design of multi-analyte detection systems with application of enzymes that catalyze reactions of a group of products, or are inhibited by a group of similar compounds. Especially interesting examples of such systems include, for instance electro-antennographic detection in liquid chromatography, olfactory detection in gas chromatography, or single-cell based detection in capillary electrophoresis.
Sena Caglar
Istanbul University, Turkey
Title: Direct analysis of drugs in biological fluids by on-line chromatography
Biography:
Sena Caglar is a Research Assistant at the Istanbul University, Faculty of Pharmacy, Department of Analytical Chemistry. She had PhD and MSc degrees at the same department and studied Chemical Engineering. She conducted post-doctoral research at Medical Center of Munich University, Institute of Laboratory Medicine, Laboratory of Bio-Separation. She has researches on drug analysis in biological fluids by liquid chromatography mass spectrometry, on-line solid phase extraction coupled liquid chromatography, multidimensional chromatography and publications in drug analysis in pharmaceutical formulations and biological fluids by high performance liquid chromatography, spectrometry, degradation, pharmacokinetic and validation studies.
Abstract:
In pharmaceutical, bioanalytical and biomedical analysis of drugs and metabolites in biological fluids is essential for bioequivalence/bioavailability, therapeutic drug monitoring and drug abuse studies. An optimal and effective sample preparation method plays the most important role since the depletion of the matrix in biological fluids is the biggest issue for a trouble-free analysis. It is impossible to inject the biofluid directly to the chromatographic system with traditional methods but this challenge was overcome by the on-line methods. Combination of solid phase extraction (SPE) with high performance liquid chromatography allows direct analysis of small molecules (i.e., drugs) in biofluids. The method, in summary, depends on connection of the SPE column, coated with various packing materials, directly to the analytical column (where the analytes are separated) through a switchingvalve and injection of the sample to the system. Following the injection, i) the matrix components are depleted and ii) the analytes are separated in the column. Thus, sample preparation step from the biological fluid is completely eliminated and the sample can be directly injected to the system resulting with high reproducibility in the analyses.
- Track 6: Advances in ChromatographyTrack 7: Advances in Mass Spectrometry
Session Introduction
Pao-Chi Liao
National Cheng Kung University, Taiwan
Title: Metabolomics approaches for bio-marker discovery for toxicant exposure of di-isononyl phthalates (DINPs) using liquid chromatography-high resolution mass spectrometry (LC-HRMS)
Biography:
Pao-Chi Liao completed his PhD in Analytical Chemistry from Michigan State University (MSU) in 1995 before doing Postdoctoral research in the Department of Biochemistry at MSU. He joined as the Faculty at Department of Environmental and Occupational Health, National Cheng-Kung University, Taiwan in 1997, where he was promoted to full Professor in 2006, and named Distinguished Professor in 2011. His research interests and fields of specialty include analytical chemistry, mass spectrometry, proteomics, biomarker discovery, cancer biomarkers, lung cancer metastasis, and environmental and occupational health.
Abstract:
Di-Isononyl Phthalate (DINPs) is widely used as plasticizers and has effects on reproductive system. Three metabolomics approaches were used to explore DINP exposure markers in an LTQ/Orbitrap HRMS dataset obtained from liver enzyme incubation. The data processing techniques included Signal Mining Algorithm with Isotope Tracing (SMAIT), Mass Defect Filtering (MDF), and web-based XCMS. Fourteen metabolites were validated as DINP exposure markers using a rat model. Among the 14 exposure-related DINP metabolite signals, 8 have not been reported in the literature. The metabolomics platform can efficiently and systematically filter probable metabolite signals from a complex LC-HRMS dataset for toxic exposure marker discovery.
Vlad Orlovsky
SIELC Technologies, USA
Title: Evolution of mixed-mode from “mixing†silica gels to core-shell mixed-mode technology
Biography:
Vlad Orlovsky graduated with MSc in Organic Synthesis from Ufa Petrochemical University in 1987. In 1992, he moved to United States to continue developing his skills in organic chemistry. He joined Pfizer in 1993 as a Research Chemist. After working at Pfizer, he co-founded SIELC Technologies with a goal to develop better separation technologies. In collaboration with his colleagues, he developed over 23 new commercial stationary phases. His continuing research and development in this field resulted in development of the first ever core-shell mixed-mode stationary phases. He has 5 patents and a dozen publications in scientific journals.
Abstract:
In recent years, mixed-mode chromatography emerged as a powerful separation technique with alternative selectivity. Evolution of this technology covering old “mixing” approach and single ligand design is being discussed with the emphasis on selectivity benefits and critical applications. Comparison of single, dual, tri-modal columns are offered and evaluated. The first line of core-shell mixed-mode stationary phases is presented. Numerous examples in pharmaceutical, environmental, food and agricultural sciences are presented.
Biography:
Professor Asif Zaidi completed his PhD in Department of Physics & Astronomy. University of Waterloo from University of Waterloo in the year 2010. His research interests focus on controlled synthesis, separation, assembly and property regulation of functional inorganic nanomaterials and carbon materials. He has published more than 7 publications as the first author or corresponding author in journals including Small molecules from the decomposition of interstellar carbons
Abstract:
Solid methane at 77K was irradiated with laser pulses of wavelength 800 nm and energy of 275 μJ. Laser pulse duration was 100 fs. This irradiation experiment shows formation of higher molecular weight pure carbon clusters Cn where n = 1, 2, 3, ---, and the formation of alkane molecules of higher molecular mass than the original target molecule. These molecules have the composition (CH4)n where n = 1, 2, 3-- The time of flight spectrum also shows the formation of polyynes and cumulenes as ablation products. The laser ablation of graphite has been ex-tensively studied because of graphite’s unique properties. It is well known that the laser ablation of graphite with nanosecond pulses produces pure carbon clusters and fullerenes such as C50, C60 and C70 as well as more complex species including nanotubes, depending on ablation conditions. It is then important to investigate the ablation of molecular systems containing C-H sigma bonds using femtosecond laser pulses in order to see the effect of hydrogenation of the target molecule. The use of femto-second, rather than nanosecond laser pulses eliminates heating of the target. Alkanes are the simplest fully hydrogenated C-H molecular systems that occur naturally and methane (CH4), containing only C-H sigma bonds, is the simplest member of this family. A study of the ablation of solid methane is then important in understanding ablation in more complicated alkane systems. Experiments were carried out using a 5×10-7 torr vacuum chamber attached to a time of flight (TOF) spectrometer. By flowing methane gas onto a cold finger made of copper plate in the vacuum chamber, a 0.5 mm-thick film of solid methane (a van der Waals solid with a density of 0.522 gm cm-3) was obtained on the cold finger. Five to eight successive laser pulses chopped from a 100-fs 1-KHz 800nm 300-μJ mode-locked Ti:sapphire laser system were focused on the solid methane by a 10-cm focusing lens. Each focused laser pulse has a peak intensity 8×1014 W/cm2. A laser plume was generated which was extended from the cold finger surface up to a few millimeters above it. Positively charged particles generated in the laser plume were accelerated by a 4kV linear accelerator toward a micro-channel plate (MCP) detector. Signals from the MCP detector were recorded by a scope and sent to the PC.
Gerard Rosse
Dart NeuroScience, San Diego, CA
Title: Advances and Applications of Supercritical Fluid Chromatohgraphy in Drug Discovery
Biography:
Dr. Rosse is currently Associate Director, Structure Guided Chemistry, at Dart Neuroscience and serves as Adjunct Associate Professor at Drexel University. Prior he functioned in leadership and scientific positions in medicinal chemistry with Cephalon, Sanofi and F. Hoffman-La Roche. During his industrial tenure, he led multidisciplinary teams and invented pre-clinical candidates for a wide range of therapeutic indications including CNS, Inflammation, Metabolism, Oncology, and Antibacterial agents. Dr. Rosse’s career is also characterized by the implementation of innovative chemical technology and analytical chemistry platforms that accelerated the drug discovery process and reduced costs. He received the Ph.D. degree in chemistry from the University of Basel in Switzerland and postdoctoral training at Stanford University, California.
Abstract:
Innovative technologies to make better compounds and make them faster have been implemented. The presentation will focus on the design of a highly automated facility with a multistep process for the rapid analysis and purification of small molecules using Supercritical Fluid Chromatography-Mass Spectrometry (SFC-MS). The recent introduction of a new generation of SFC-MS instruments is revolutionizing the field of chromatography. The instrumentation and the robotic infrastructure to support the production of ~10,000 compounds/month will be discussed. Finally the benefits of an enhanced SFC-MS technology platform to increase productivity and decrease costs will be discussed.
Xiaoming Sun
Beijing University of Chemical Technology, China
Title: Nanoseparation-from Methodology to Application
Biography:
Professor Xiaoming Sun completed his PhD from Tsinghua University and postdoctoral studies in Prof. Hongjie Dai’s group at Stanford University. he is currently the vice president of inorganic chemistry department in Beijing University of Chemical Technology. His research interests focus on controlled synthesis, separation, assembly and property regulation of functional inorganic nanomaterials and carbon materials. He has published more than 60 research papers as the first author or corresponding author in journals including J. Am. Chem. Soc., Angew. Chem. Int. Ed., Adv. Mater. and Chem. Eur. J.. They have been cited more than 3500 times in total.
Abstract:
Density gradient ultracentrifugarion (DGU) separation method was established to obtain monodispersed colloidal nanostructures. Such separation method was demonstrated as a versatile method for acquisition of monodispersed colloidal nanoparticles which are hard to be synthesized. This separation method was applicable to both aqueous (polar) and organic (non-polar) solvents systems; and NPs with different size, density and morphology can be separated. Separation objects involve nearly all kinds of materials including metal and metal oxides/sulfides, carbon materials, semiconductors, etc. Synthesis-structure-property relationships were observed on the separated NPs, which guided synthetic optimization. Besides separation, concentration and purification of NPs could be achieved at the same time when a water/oil interface was introduced into the separation system. By introducing a reaction zone or an assembly zone in the gradient, we can monitor the reaction and assembly of NPs since reaction time could be controlled and chemical environments could be changed extremely fast. In short, “Lab in a tube” method paved a way for the research on nanoparticle synthesis optimization, purification, assembly and surface reactions.
Solich Petr
Charles University, Czech Republic
Title: Trends in development of stationary phases in chromatography
Biography:
Prof. Petr Solich has completed his PhD. from Charles University, Faculty of Pharmacy, Hradec Kralove, Czech Republic. He is the head of Department of Analytical Chemistry as well as head of University Research Centre UNCE at Faculty of Pharmacy, Charles University. He has published more than 180 papers in impacted analytically oriented journals, with h-index 28 and has been also serving as an editorial board member of journal Talanta.
Abstract:
High performance liquid chromatography is one of the most progressive separation techniques which allows identification and quantification in one step and is frequently used in clinical research for analysis of biological samples in connection with modern sample preparation. Choice of the sample preparation technique is key step which influence sensitivity, robustness, solvents and sample consumptions etc. Connection of modern, fast and robust sample preparation procedures and modern trends in liquid chromatography are useful base for clinical research. A huge expansion of new stationary phases was registered during last couple of years. Several different technologies with different characteristics were introduced into the market, among them Core shell technology using porous shell and solid core particles. These columns can be used in common HPLC instruments as well as in UHPLC systems. This technology promises to increase of resolution and maximizes throughput, and result in solvent saving and easier method transfer. The recently introduced HR monolithic technology is based on a unique sorbent material allowing good quality of separations in a minimal time. The main advantages of monoliths, apart from short analysis time, are long lifetime and immense robustness, in most cases far exceeding those of particulate columns. This new type of monoliths have at higher efficiency, better peak symmetry and longer lifetime compared with particulate columns.
Sawsan Amer
Cairo University, Egypt
Title: Quality by design approach for development of stability indicating method for determination of cefditoren pivoxil
Biography:
Professor Sawsan Amer completed her PhD in Department of Analytical Chemistry from Cairo University 1985. Her research interests focus on controlled synthesis, separation, assembly and property regulation of functional inorganic nanomaterials and carbon materials. He has published more than 7 publications as the first author or corresponding author in journals including Small molecules from the decomposition of interstellar carbons
Abstract:
A hybrid development strategy of Quality by Design (QbD) and One Factor at Time (OFAT) approaches were used to develop a stability indicating HPLC method for quantitative determination of cefditoren pivoxil (CTP) in bulk powder and pharmaceutical formulations. A forced degradation studies were performed under acid, alkaline, thermal and photolytic stress conditions. Chromatographic separation was achieved in less than 10 min. using a RP C-18 column, mobile phase [methanol: acetate buffer pH 4.5 (55:45, v/v)], flow rate 1.5 mLmin-1 and UV detection at 225 nm. Optimization of column, pH, and wavelength were implemented according to OFAT approach, while elution temperature and methanol content in the mobile phase were implemented considering QbD approach. The method was validated to meet official requirements including specificity, linearity, precision, accuracy and robustness. The drug response was linear (r=0.9999) in range of 89-672 μgmL-1, the limit of detection (LOD) and limit of quantitation (LOQ) were 5.31 μgmL-1 and 16.1 μgmL-1, respectively. The intra and inter-day precisions were 0.11% and 0.44% respectively. The proposed method was successfully applied for the determination of CTP in bulk and tablets with acceptable accuracy and precisions. The results demonstrated that the method would have a great value when applied in quality control and stability studies for CTP.
- Track 4: High Performance Liquid Chromatography
Track 5: Novel Techniques
Track 8: Product Related Processes
Session Introduction
Gerhard Kratz
Global Sales Director abcr GmbH Im Schlehert 10 76187 Karlsruhe Germany
Title: HPLC – High Performance Liquid Chromatography
Biography:
Gerhard Kratz has completed his studies at University of Applied Sciences in Berlin. His dissertation was about Planning, calculation and construction of a Fluidized bed reactor. Deepening during his studies was Water economy, chemical technology, plastic technology, varnish and paints, oil processing. First positions in industry were in pharmaceutical industry doing HPLC method development on various HPLC brands. Specialized in HPLC column selection and teaching customers in troubleshooting all over the world he is supporting several internet forums for HPLC questions.
Abstract:
Liquid chromatography was defined in the early 1900s by the work of the Russian botanist, Mikhail S. Tswett. His pioneering studies focused on separating compounds [leaf pigments], extracted from plants using a solvent, and in a column packed with particles. Tswett coined the name chromatography [from the Greek words chroma, meaning color, and graph, meaning writing—literally, color writing] to describe his colorful experiment. [Curiously, the Russian name Tswett means color.] Today, liquid chromatography, in its various forms, has become one of the most powerful tools in analytical chemistry. HPLC is the most used analytical testing method for pharmaceuticals and is also used in production to produce ultra-pure pharmaceuticals. For example Insulin, the last purification step is done with preparative HPLC (industrial scale chromatography), at most manufacturing processes! Stationary phases are different due to the different surface chemistry used to do the bonding. High pure Silanes are used to give each packing material its unique performance.
Eduard Rogatsky
Albert Einstein College of Medicine of Yeshiva University, USA
Title: 10 years of evolution in UHPLC-MS chromatography. Current trends.
Biography:
Eduard Rogatsky completed his M.Sc in physical chemistry from Belarus State University, PhD in bioanalytical chemistry from Bar-Ilan University (Israel) in 1999, and postdoctoral studies at Albert Einstein College of Medicine, NY. He joined the faculty there in 2001, and is currently a Senior Associate Scientist and Director of Mass Spectrometry in the Biomarker Analytical Resource Core Laboratory, Einstein-Montefiore Institute for Clinical and Translational Research, Bronx, NY, USA
Abstract:
Ultra High Performance Liquid Chromatography (UHPLC) was introduced in 2004 by Waters. This novel type of liquid chromatography system was designed to utilize resolution power of sub 2 µm particle size columns for fast high resolution separations. Different vendors also have developed novel chromatographic systems. Currently, UHPLC has become a typical chromatographic system, and within the last 10 years both UHPLC practitioners and instrument developers acquire new experience in that field. The author will share his thoughts and findings of utilization UHPLC technology with mass spectrometry detection in clinical settings.
Biography:
Eiji Yashima received his BS, MS, and PhD (1988) from Osaka University. In 1986, he joined Kagoshima University. After a Postdoc with David Tirrell at UMass (1988-1989), he moved to Nagoya University in 1991 and was promoted to a full Professor in 1998. He has published over 300 papers including 23 reviews and has been serving as an Editorial Board or Editorial Advisory Board Member of 10 international journals. His current research interests are in the design and synthesis of helical molecules, supramolecules, and polymers with novel structures and functions
Abstract:
The helix is ubiquitous in nature and one of the prevalent structural motifs for biological polymers, playing key roles in their sophisticated functions, such as chiral recognition, enantio-selective catalysis, and replication. Here, a quite unique helical polyacetylene is shown, whose main-chain helicity and axial chirality of the pendants are induced in the solid state accompanied by significant amplification of the chirality in a sequential or synchronized fashion upon interaction with a nonracemic alcohol. The induced macromolecular helicity and axial chirality are automatically memorized and further switched in the solid state. This unprecedented feature enables in this polymer the switchable chiral stationary phase (CSP) for separating enantiomers by high-performance liquid chromatography (HPLC) whose elution order or enantio-selectivity can be reversibly switched in the column for the first time. Separation of enantiomers by HPLC is now an essential technique for the research and development of chiral drugs in the pharmaceutical industry and a number of CSPs have been commercialized. However, none of them can switch the elution order of enantiomers, which is one of the most important issues to resolve.
Biography:
Imre Sallay was born and raised in Hungary, Budapest. He spent almost four years as researcher/teaching assistant at a local university in the Biochemistry Department. Fate assigned his first task to be HPLC separation of enzyme digested insulin fragments. Moved to Japan with a research scholarship for one-and-a-half years, but got entangled in a PhD course leading to a post-doc binding him irreversibly to the country. The first job at a laboratory supplier company landed him to the chromatography world. For the last 10 years he is travelling around the Globe tirelessly consulting API producer companies with especial attention to insulin manufacturing. He is passionate about the beauty of the science at work in silica based reversed phase chromatography. When not on the road he happily lives in Osaka with his ancient guinea pig.”
Abstract:
As peptide-based APIs are getting more complicated the bar is raised constantly in the downstream purification part. The tool-box available for scientists is bursting, new stationary phases are developed in a steady progress, but most unfortunately often there is no time to do a decent screening for choosing the optimal silica based reversed phases stationary phase for high pressure liquid chromatography. Though the importance is high, usually the last, so called polishing step has strong impact on the process economy. The presentation is moving through the important physicochemical parameters of the silica particles and pointing out the role they play in the process. Special attention is paid for the pore and particle size and how they determine the success of the purification. A sadly neglected point, the great importance of the ligand density or bonding density of the reversed phased silica is explained in details. The presentation is focused on large scale/ process scale purification, but the principles just as much apply to analytical HPLC work. Better integration connecting purification jobs from mg scale up to large industrial scale production is easy to achieve if the scientists manning those different stations have common understanding and common knowledge on the science behind the purification jobs.
Prof Andrew Shalliker
University of Western Sydney, Australia.
Title: New Column Technology Enabling Ultra-High Speed HPLC-MS
Biography:
Professor Shalliker completed his PhD in 1992 from Deakin University, Waurn Ponds, Australia. He completed postdoctoral studies at Queensland University of Technology, Brisbane (Australia) and the University of Tennessee, Knoxville, the latter under the mentorship of Distinguished Professor Georges Guiochon. He is currently a Professor in Analytical Chemistry at the University of Western Sydney and a Deputy Director of the Australian Centre for Research on Separation Science (ACROSS). He has approximately 130 publications.
Abstract:
The suite of chromatography columns referred to as Active Flow Technology (AFT) form the basis of ultra-high speed HPLC-MS analyses. This technology currently comprises three column designs; Parallel Segmented Flow (PSF); the Curtain Flow (CF) and the Reaction Flow (RF) columns. The key benefits of AFT arise from a new design of the outlet end fitting of the column, which enables the separation of the radial central flow from the wall or peripheral flow. This flow ratio can be adjusted (segmentation ratio), establishing virtual columns of almost limitless internal diameter. The benefits of this design effectively revolve around the establishment of wall-less columns, since they function far more efficiently than conventional HPLC columns, especially at high flow rates. As the radial central flow is separated from the peripheral or wall flow, the amount of mobile phase processed by a detection source is reduced. In fact, the amount of flow entering a detector is proportional to the segmentation ratio. Since these columns yield higher efficiency and a reduction in flow to the detector, separations can be undertaken at flow rates that would otherwise be difficult for an MS to process. We have used these columns at flow rates typically around 5 to 6 mL/min with MS detection, but since the outlet fitting segments the flow, just 1 mL/min has been required to be processed by the detector. This presentation details the design of these columns, their operation and their benefits in HPLC separations that incorporate MS detection.
Ali Aboel Dahab
Kings College London, UK
Title: Magnetohydrodynamic Electrophoresis: A novel fully validated method in bio/chemical analysis
Biography:
Dr Ali Aboel Dahab is a researcher and lecturer at the pharmaceutical research division, King’s College London. He is a member of several professional bodies such as Royal society of chemistry and Royal pharmaceutical society of Great Britain. He has published many papers in highly reputable journals and has been serving as an editorial board member of some reputed journals. He has worked as a consultant in the area of biopharmaceutical and toxicological analysis at deltaDot Ltd. He has a special interest in pharmacology, toxicological and chiral analysis, biological spectroscopy and the development of analytical techniques.
Abstract:
There is a continuing need for fully validated and cost effective separation methods to meet the increasingly exacting demands of medicine, pharmaceutical science, industry and the environmental field, covering areas such as proteomics, biotechnology and related sciences. This work sets out to address this issue by radically improving the performance of electrophoretic techniques particularly capillary electrophoresis (CE). Applications are expected in all areas of bio/chemical analysis. The full potential of CE is not being realised routinely because of the relatively poor reproducibility, the adverse effect of EOF (electroosmotic flow) and the non-optimal resolution obtained with molecules like proteins/peptides that can be adsorbed onto the capillary wall. There is a need for greater efficiency and stability in detecting all the components in complicated analytical profiles and better efficiency in achieving the fine separations normally required in chiral analyses. The work described here is based upon the application of magneto-hydrodynamic principles on CE (MHD-CE) with the mathematical principles derived from in-depth considerations of magneto-hydrodynamics' theory (patent pending). Preliminary experiments have proven the concepts and the following benefits have been observed: (1) Shorter migration times with improved repeatability and reproducibility; (2) Improved peak profiles, (3) Reduction in diffusion (D) and electric double layer (The double layer thickness or Debye ionic radius (ï¤); Reduced EOF and improved electrophoretic mobility, (4) Improved current density, (5) Improved efficiency and resolution. (6) The mathematical basis for the phenomenon is appropriate. It is hoped through the work on MHD-CE that an all-encompassing theoretical frame work will be established and MHDE gives the technique the push it has long needed.
Jaya Vejayan
University Malaysia Pahang, Malaysia
Title: Two Dimensional Electrophoresis (2DE) Guided Purification Novel Technique in the Isolation of Bioactive Proteins from Complex Mixtures
Biography:
Jaya Vejayan has completed his PhD from University Malaya, a premier university in Malaysia. In his MSc he was involved in isolating bioactive compounds from the medicinal plant, Ipomea pes caprae, known to be an antitoxin to jellyfish toxins. While in his PhD he used proteomics to study proteins in various snake venoms in Malaysia. Accordingly, he merged both knowledge together to derive the 2DE guided purification technique.
Abstract:
There are still many laboratories in the East which use the conventional two dimensional electrophoresis. Progressive developments in liquid chromatography and mass spectrometry in recent years led to the obvious demise of 2DE in the West. Nevertheless, due to its robustness, low cost in acquiring and maintenance, 2DE used widely in countries like Malaysia. Efforts required to be done to provide importance to this system. One such effort is been highlighted in this paper. In the natural product research, to isolate bioactive compounds from medicinal plants, an assay will be used to detect presence of the compound within fractions after each sequential chromatography techniques such as silica gel chromatography or HPLC. This technique that will eventually lead to pure compound is known as Bioassay Guided Isolation. Adopting the principle of this technique, 2DE guided purification technique has been derived in the field of proteomics. The technique is simple whereby in place of bioassay will be a 2DE mapped database of a complex mixture such as snake venom. Next, by performing the common separating techniques such as size exclusion or ion exchange or others, fractions will be screened for presence of protein of interest. The fractions showing obvious presence of protein or its subunit stained spots in 2DE will be accepted for further fractionation. The steps will be repeated till homogeneity is achieved. This technique will be illustrated accordingly by the isolation of rhodocetin. In this example, rhodocetin a potential therapeutic protein contained in Calloselasma rhodostoma snake venom will be purified successfully using 2DE guided purification technique.
Ekwere Mercy R
University of Calabar, Nigeria
Title: Thin layer chromatographic analysis of capsaicin and moisture contents from three varieties of capsicum peppers
Biography:
Ekwere Mercy R is a Senior Lecturer and a PhD student. He has a teaching and research experience in Biochemistry for 20 years.
Abstract:
Levels of pungency of capsicum species depends on the concentration of alkaloid compound, capsaicinoids, primarily of capsaicin found in the fruit and only in the plant genus, capsicum. In detecting capsaicin, taster fatigue occurs and tasters are not able to distinguish between the different capsaicinods, therefore the organoleptic test has been replaced with instrumental methods. The work sought to employ a cheap, affordable and readily available method. Crude capsaicin extracted previously from three varieties of capsicum genus [Bird eye pepper, X1- (Capsicum frutescens), chilli pepper -X2 and sweet pepper -X3 (Capsicum annum)] by a modified method of Kosuge et al. (1958) were separated and identified by means of thin layer partition chromatograph impregnated with silica gel G plates (SiO2) and developed in a closed chamber with 95% methanol. The pungent fractions for bird-eye and chilli peppers showed dominant spots at Rf 0.59±0.21, 0.95±0.03 and 0.67±0.01, 0.92±0.10 respectively. While bird-eye pepper had a third spot at Rf 0.93±0.00, a third spot for chilli pepper was not detected. However, sweet pepper had a spot at Rf 0.82±0.02, similar to the third spot as that of bird – eye. The separated fractions were identified by comparing their Rf values with those of authentic capsaicin standards and literature data. TLC method appears to be adequate for routine analysis and could suffice as an essential preliminary purification of capsaicin where scare equipment and most reagents are unavailable.
Asokan C
Sokoto State University, Nigeria
Title: Enhanced cleavage of amyloid ï¢ peptides in the casein injected inflammatory brain of mice
Biography:
Asokan C has completed his PhD from University of Madras and Postdoctoral studies from Columbia University, NY, USA. He is an Associate Professor at the Department of Biochemistry, Sokoto State University, Sokoto, Nigeria. He has published more than 36 papers in reputed journals and has been serving as an Editorial Board Member of repute.
Abstract:
The excessive accumulation of amyloid β-Peptides (Aβs) in the brain is the causative factor in all genetic as well as sporadic cases of Alzheimer’s disease (AD). Two enzymes namely beta-secretase and gamma-secretase are involved in the defective cleavage of Amyloid Precursor Protein (APP) and the alpha-secretase is involved in its normal processing. The core protein of the amyloid senile plaques within the brains of afflicted individuals contains peptide of 39-43 residues, but mostly terminating with residues 40 and 42. The longer Aβ42 is more abundant in the amyloid of the neuritic plaques while the shorter peptides (Aβ40) found more in the vascular deposits. Factors that lead to the over expression of Aβs are yet to be identified. In the present study, we have shown that the prolonged subcutaneous injection of casein, which is known to develop organomegaly of the liver, spleen and kidneys in mice (the Congo red stain of the liver confirmed the presence of a fibrillary protein deposits with amyloid characteristics in chronic inflammation and associated systemic amyloidosis) triggers about 20 times more Abeta accumulation (in sixty six days period) in the mice brain than that of the control mice which was confirmed as well as quantified by RP-HPLC. From the Mass Spectroscopic analysis, we have shown the occurrence of a new type of proteolytic zeta cleavage fragment, a 1-54 residue Abeta in the mice brain along with the Abeta peptides.
Gerard Rosse
Dart NeuroScience, San Diego, CA,
Title: Advances and Applications of Supercritical Fluid Chromatohgraphy in Drug Discovery
Biography:
Rosse is currently Associate Director, Structure Guided Chemistry, at Dart Neuroscience and serves as Adjunct Associate Professor at Drexel University. Prior he functioned in leadership and scientific positions in medicinal chemistry with Cephalon, Sanofi and F. Hoffman-La Roche. During his industrial tenure, he led multidisciplinary teams and invented pre-clinical candidates for a wide range of therapeutic indications including CNS, Inflammation, Metabolism, Oncology, and Antibacterial agents. Dr. Rosse’s career is also characterized by the implementation of innovative chemical technology and analytical chemistry platforms that accelerated the drug discovery process and reduced costs. He received the Ph.D. degree in chemistry from the University of Basel in Switzerland and postdoctoral training at Stanford University, California.
Abstract:
Innovative technologies to make better compounds and make them faster have been implemented. The presentation will focus on the design of a highly automated facility with a multistep process for the rapid analysis and purification of small molecules using Supercritical Fluid Chromatography-Mass Spectrometry (SFC-MS). The recent introduction of a new generation of SFC-MS instruments is revolutionizing the field of chromatography. The instrumentation and the robotic infrastructure to support the production of ~10,000 compounds/month will be discussed. Finally the benefits of an enhanced SFC-MS technology platform to increase productivity and decrease costs will be discussed.
Gaetane LESPES
University of Pau (UPPA), France
Title: Characterization of nanoparticles: how to meet the multiple challenges?
Biography:
Gaetane LESPES has completed his PhD at the age of 26 years from Pau University and a postdoctoral stay from Plymouth University. She founded and chairs the G-4F, Scientific Group of Field-Flow Fractionation that promotes the development of innovative approaches for nano- and micro-characterization in material sciences, medicine, food, and environment. She has published more than 75 papers in reputed journals and has been serving as an editorial board member of American Journal of Analytical Chemistry.
Abstract:
The development of nanotechnologies inevitably induce the need for analytical methods capable of characterizing nanomaterials such as nanoparticles and nanotubes. The challenge remains important due to the diversity in size, shape, chemical composition of natural and engineered nano-objects combined with the complexity of the surrounding media. Some years ago, Field-Flow Fractionation (FFF) coupled with UV, Multi-Angle Light Scattering (MALS) and atomic mass spectrometry (ICPMS) has been proposed as a powerful analytical strategy for such challenge. In this presentation FFF will be presented from its principle to its analytical performances. Different examples of applications in material sciences and environmental media will be presented in order to illustrate the capabilities of FFF-multidetection.
Biography:
Zahir Akhunzada is a PPD Consultant in the Analytical & Bioanalytical Development department at Bristol-Myers Squibb in New Brunswick, New Jersey where he is responsible for the analysis and characterization of proteins by MFI. Before joining PPD, he worked for Schering-Plough/Merck. He was Assistant Prof. at King Saud University Riyadh Saudi Arabia and a Guest Investigator at the VA Hospital in Newark, NJ. He has a broad range of expertise in R&D, spectroscopy, chromatography, wet analytical techniques and biologics. He acquired research experience in the Netherland, Pakistan and earned his PhD in Chemistry in 1992. He did his Post doctorate in Germany, has several research publications and co-authored, a textbook with Prof. Atta-ur-Rahman on “Streoselective Synthesis in Organic Chemistry”, published (1993) by Springer Verlag, New York.
Abstract:
The presence of sub-visible particles (SVPs) is a major challenge in the development of therapeutic protein formulations. Distinction between proteinaceous and non-proteinaceous SVPs is vital in monitoring the formulation stability. The current compendial method based on light obscuration (LO) has limitations in analyzing translucent particles, requires large analysis volume and therefore demands urgent need for an unambiguous method to characterize SVPs. A number of attempts have been made to characterize SVPs, albeit with limited success. This presentation reveals a method that successfully characterizes and distinguishes, both potentially proteinaceous and non-proteinaceous SVPs in protein formulations by using Microflow Imaging (MFI) in conjunction with the MVAS (MFI View Analysis Suite) software.
Fernanda Costa
Universidade Federal do Rio de Janeiro, Brazil
Title: Solvent System Selectivities in Countercurrent Chromatography Using Salicornia gaudichaudiana Metabolites as Practical Example with Off-line Electrospray Mass-Spectrometry Injection Profiling
Biography:
Fernanda das Neves Costa has completed her PhD at the Universidade Federal do Rio de Janeiro with an internship at Technische Universität Braunschweig (Germany) and Brunel University (England). Now she is an assistant professor at the same Univeristy in Rio de Janeiro, Brazil. She has published more 12 papers until the present moment.
Abstract:
Salicornia gaudichaudiana (Chenopodiaceae) is a halophyte plant that grows in high-level salt soil. Plant material is used as ‘green salt’ in food preparations for people with high blood pressure and kidney / heart diseases. Countercurrent chromatography (CCC) is a form of liquid-liquid partition chromatography in which the stationary liquid phase is retained in the apparatus without the use of a solid support. A large variety of solvent systems (SoSy) have been proposed and employed in CCC which, despite being an efficient technique, will not separate compounds of a complex mixture without the appropriated system. This study describes the influence of SoSy selectivity on the separation of S. gaudichaudiana metabolites. HEMW at 0.5:6:0.5:6 and HBuWat 1:1:2, medium polarity SoSy, gave good distribution of compounds between the two phases. Two CCC runs were performed at identical experimental conditions using the two SoSy. Odd fractions were analyzed by decoupled ESI-MS/MS for metabolite monitoring. Selected ion traces in the two reconstituted CCC-ESI-MS/MS allowed the visualization of the SoSy selectivity for major compounds. In general, HEMW at was more selective and distributed all compounds along the CCC separation with isolation of flavonol glycosides, although co-elution of dicaffeoylquinic acids occurred. HBuWat with less general compound selectivity fractionated isomeric caffeoyl-quinic acids. The SoSy selectivity in CCC is very important when having a target compound in a complex mixture. The strategic use of different SoSy in a specific sequence can influence the results. From the results of our study we could plan to isolate the flavonoids with HEMW at SoSy and then re-fractionate the sample with HBuWat for the isolation of caffeoyl-quinic acid isomers.
- Track 12: Large Scale Preparative Chromatography for the manufacturing of APIs
Session Introduction
Olivier Dapremont
AMPAC Fine Chemicals LLC, USA
Title: Implementation of a continuous chromatographic process for the manufacturing of an API
Biography:
Olivier Dapremont is a renowned expert in the implementation of continuous chromatography (SMB) for the purification of APIs. He started in 1992, developing the SMB technology for Prochrom in France, and then joined Chiral Technologies to manage the kilo separation laboratory using SMB. He joined AMPAC Fine Chemicals (then Aerojet) in California, in 2001 to be in charge of the development of continuous processes. He has developed more than 50 SMB separations at all scale. He is a member of the Prep Symposium Organizing Committee as well as a member of the SPICA Scientific Committee.
Abstract:
The advantages of continuous processing for commercial scale manufacturing are well known and accepted in many industries; reduction in the manufacturing footprint, increase in process safety, increased automation, reduction in manpower requirements, better economics are some of the known advantages. However, implementing a continuous process in an industry that is traditionally batch is often challenging. The regulatory aspects are certainly the most difficult to overcome as a shift in the approach to validation, process monitoring and even “batch” documentation is required to adapt to the specificity of the continuous nature of the process. The author will discuss the various aspects of the successful implementation of a continuous chromatographic process for the manufacturing of an API at commercial scale through actual examples.
Joseph Barendt
Chiral Technologies, Inc., USA
Title: Modern techniques for enantiomeric separation: From grams to tons
Biography:
Joseph Barendt earned his PhD in Chemistry at the University of Colorado, Boulder, followed by Postdoctoral work at UCLA. His career has been devoted to applying interdisciplinary technologies to improve organic synthetic routes for pharmaceutical products. Among his earlier accomplishments are the first commercial launches of enantioselective reducing agents and catalysts for the industry. In his current role as Chief Operating Officer of Chiral Technologies, he is responsible for all aspects of chiral chromatography, including analytical, kilo-lab separations, and metric ton quantities.
Abstract:
With ever-increasing complexity in pharmaceutical products, and the need for enantiomerically pure materials, today’s chemists are moving toward a “toolbox” approach in their research. The best toolboxes are those with the broadest range of tools to ensure that the every job can be completed. This presentation will use several case studies to explore various tools at the disposal of chemists seeking single enantiomers. Further, we will consider the unique constraints at every stage of the pharmaceutical process to better understand the proper selection of these tools from discovery through clinical trials.
Rob Driscoll
Robatel Inc., Pittsfield, MA
Title: Fast Centrifugal Partitioning Chromatograph for Extract Purification
Biography:
Rob Driscoll is a Senior Application Engineer at Robatel Inc. and has worked in the pharmaceutical and fine chemicals industries for 19 years. He is responsible for the start-up and optimization of centrifugal equipment and is responsible for the Kromaton centrifugal chromatography activities. He has a BS in Chemical Engineering from Michigan State University.
Abstract:
Centrifugal Chromatography has been developed to select and recover desired compounds at analytical, preparative, pilot, and industrial scales. Centrifugal portioning chromatography, a biphasic liquid process technology, is used for the fractionation and purification of biologic matrices, synthetic solutions, and natural products. According to the polarity and solubility of the desired molecule, FCPC permits the selection and recovery of desired compounds while achieving up to 99% purity levels. With no costly solid packing material or columns to replace, purification by FCPC reduces batch to batch costs and eliminates the risk of contamination between products. Assuring 100% recovery of samples, liquid-liquid centrifugal partition chromatography is extremely flexible allowing for both ascending and descending modes of operation with no loss of compounds due to adsorption, and no denaturing of sensitive molecules
Biography:
Marc Jacob joined Phenomenex as Global Product Manager for Chiral and Preparative Chromatography in 2011. Previously, he was Director of Process Development at Bachem (Torrance, USA) where he led efforts to develop and produce peptide Active Pharmaceutical Ingredient. Prior Bachem, he works for contract manufacturing organizations in the research, development and manufacturing of small molecules such as chiral amino acids and peptide building blocks. Jacob earned his Doctorate in Synthetic Organic Chemistry at the University of Montpellier
Abstract:
Over the last few decades, peptide synthesis technology has developed to allow for large scale manufacturing of peptides. The interest in using peptides as therapeutic agents has been a significant driver of this technology. Separation and isolation technology of the desired peptide product have also been developing along with the synthesis. The purification process typically includes chromatography separation for purifying the peptide active ingredient from crude synthetic peptide mixtures. A single step chromatographic process is most desired but a multiple step process is often necessary. When a multistep process is used, the first step is designed to isolate the desired material by removing most of the undesired components. The isolated material is then purified further by one or more different chromatographic steps to “polish” the material to the desired purity level. This presentation will cover the current state for large scale peptide manufacturing with focus on HPLC purification. The chemical and physical property of the purification packing material will be also discussed. Few example of peptide pharmaceutical ingredient with more than 20 amino acids will be presented.
Ammar Altemimi
Southern Illinois University at Carbondale, USA
Title: In-vitro antibacterial activity of optimized spinach extraction for food safety and preservation
Biography:
Ammar Altemimi worked as Lecturer (2005 - 2011) in Department of Food Science and Biotechnology, University of Basrah, Iraq. He taught biochemistry and biotechnology for undergraduate, food chemistry, dairy products. He is into: Developing academic programs, monitoring students’ educational progress, train and motivate other non-teaching staff, managing career counseling and other student service. He has published more than 5 papers in reputed journals such as Ultrsonic Sonochemistry Journal and Molecules Journal and has been serving as an Editorial Board Member and Reviewer of repute journals.
Abstract:
The aim of this study was to explore the potential antimicrobial activities of the optimized spinach extracts on Gram-negative and Gram-positive food-borne bacteria and evaluate the antimicrobial effect at the molecular level. The results indicate that the optimized spinach extract exhibited the antimicrobial activity against tested microorganisms. Moreover, the results obtained after the treatments of bacterial strains with elevated concentrations of the optimized spinach extracts revealed that the extract had potent lethal activities as the growth turbidity decreased as the concentration or time of exposure increased. In addition, the observation by the scanning electron microscope showed that cells of the bacterial strains were damaged after the treatment with the optimized spinach extract. The antimicrobial effect was explored at the molecular level, using random amplification of polymorphic DNA (RAPD) analysis of the genomic DNA extract from the control (untreated) and the optimized spinach extract -treated bacterial strains. The results demonstrate that the polymorphic bands were decreased for most treated microbes compared with untreated strains. All these results strongly point out the mutagenicity, lethal and antimicrobial effect of the optimized spinach extracts. The results indicate the possibility of using the leaves extract of spinach as a source of antibacterial compounds for treatment of infections caused by bacterial pathogens.
Zhuomin Zhang
Sun Yat-sen University, China
Title: Development of novel enrichment media of trace volatiles for real sample analysis
Biography:
Dr. Zhuomin Zhang has completed his PhD in 2007 from Sun Yat-sen University majoring in analytical chemistry. Now, he is an associate professor in Sun Yat-sen University. His research interests are sample preparation and chromatographic analysis. The main research field covers the development of novel enrichment media and device for gas sampling project and chromatographic analytical method for bio-odoromics. As a young scholar, he has published more than 40 papers in reputed academic journals.
Abstract:
Gas sampling techniques, especially for the enrichment and separation of trace gases from complicated matrix still remain one of the weak spots in analytical chemistry nowadays due to gas strong volatility, compared with liquid and solid sample. Efficient gas sampling techniques should possess the highest extraction capacity and selectivity and can be conveniently coupled with sequent analytical instruments. The core of developing efficient gas sampling techniques lies in the development of new enrichment media with higher extraction capacity and selectivity. In our previous reports, a series of novel enrichment media, including one-dimensional nano-arrayed, conjugated doping and Metal Organic Frame (MOF)-based coatings were developed, which mainly focused on the improvement of sampling capacity and selectivity for trace target gases from real samples with complicated matrices. The fabrication formats of these novel enrichment media, mainly involved sorbent tube, headspace stir bar and Solid-Phase Micro Extraction (SPME) coatings coupling with the consequent analytical instruments. These novels trace gas enrichment media have been successfully applied for the enrichment and analysis of trace target volatiles from food, environmental and biological samples.
- Track 9: Clinical chemistry, Biomarkers and Diagnostics assays
Track 10: Complementary separation techniques
Track 11: Green Technologies, Future Challenges and Trends
Session Introduction
Juan G. Santiago
Stanford University, USA
Title: Life in the shock wave: Accelerating DNA reactions with isotachophoresis
Biography:
Juan Santiago received his MS and PhD in Mechanical Engineering from the University of Illinois at Urbana-Champaign in 1992 and 1995. His research includes the development of microsystems for on-chip chemical analysis, drug delivery, sample preparation methods, and desalination of water. Applications of this work include molecular medical diagnostics, drug discovery, environmental monitoring, and the production of drinking water. He is a Fellow of the American Physical Society, a Fellow of the American Society of Mechanical Engineering, an Associate Editor of the journal Microfluidics and Nanofluidics, co-founder of several companies in the microfluidics area, co-inventor of micron-resolution particle image velocimetry, and director of the Stanford Microfluidics Laboratory. He served as Associate Editor of Lab on a Chip '08-'13. He has given 26 keynote and named lectures and more than 100 additional invited lectures. His work is cited about 1000 times per year. He has graduated 26 PhD students and advised eight postdoctoral researchers. 16 of his former advisees are now professors at major universities. He has authored and co-authored over 150 archival publications and 200 conference papers, and holds 36 patents (16 of which are licensed).
Abstract:
We use isotachophoresis (ITP) to achieve fast and specific analyses of molecular targets in complex mixtures. We use ITP to pre-concentrate and purify; molecular recognition for specificity; and ITP to control and increase the rate of chemical reactions between molecular probes and target macromolecules. ITP is an electrophoresis technique that uses two buffers which include a high mobility leading electrolyte (LE) and a low mobility trailing electrolyte (TE). Sample species with mobilities bracketed by those of the LE and TE focus into the TE-to-LE interface. For trace sample concentrations, multiple species focus in so-called peak mode wherein multiple analytes mix and strongly overlap within an order of 10 µm wide ionic concentration shock wave. This co-focusing mixes target species and pre-concentrates them to accelerate reactions. We have integrated DNA and RNA extraction with sequence-specific quantitation using a variety of mobile and immobile cDNA probes. We pre-concentrate target and probe molecules by >10,000x and achieve in 30 sec reactions which would normally take 4 days. We have shown specific and sensitive detection of target sequences in order 5 minutes with little or no off-chip sample preparation, and without target amplification.
Takayuki Kawai
RIKEN, Japan
Title: Ultra-sensitive capillary electrophoresis for single cell analysis
Biography:
Takayuki Kawai received MSc and PhD in School of Engineering, Kyoto University, for his research on highly sensitive micro-scale electrophoresis. He then became a Postdoc in AIST and University of Illinois to study micro-fluidics and capillary electrophoresis for high-performance bio-analytical chemistry. In 2014, he was promoted to Research Scientist in RIKEN where he started the current research on integrated single-cell analysis. He also has the position of a PRESTO Researcher in Japan Science and Technology Agency, which is awarded to very few outstanding young scientists in Japan. He has published 13 qualified papers to date.
Abstract:
Recently, single-cell analysis is becoming more and more important to understand cell-to-cell heterogeneity in the complicated life system. Although large molecules within the single cell can easily be visualized via immune-histochemical staining, simultaneous analysis of numerous compounds still remains one of the most challenging issues. Among several analytical techniques, Capillary Electrophoresis (CE) coupled to Laser-Induced Fluorescence (LIF) or Mass Spectrometer (MS) is an effective method due to its high separation efficiency, low sample requirements, and high detectability. In this presentation, ultra-sensitive CE-LIF/MS system is introduced that uses online sample pre-concentration techniques like Large-Volume Sample Stacking (LVSS) for the single cell analysis. So far, pM detectability has been achieved in the analysis of biogenic compounds such as amino acids and oligosaccharides. Successful demonstration of LVSS-CE-LIF chiral analysis of a single cell will finally be introduced.
Stanislav L. Karsten
NeuroInDx, Inc., USA
Title: KuiqpicKTM and UnipicKTM: versatile instruments for single cell acquisition and complex heterogeneous tissue microdissection
Time : 09:30-09:50
Biography:
Dr. Karsten has completed his PhD in Medical Genetics and Pathology from Uppsala University, Sweden in 2000 and postdoctoral studies in Functional Neurogenomics from UCLA in 2004. Currently, Dr. Karsten is a President and CEO of NeuroInDx, Inc., a California based company focused on the development of instrumentation for cell and tissue specific sample acquisition and analysis in biomedical research. Prior to his position at NeuroInDx, Dr. Karsten was an Assistant Professor of Neurology where his laboratory conducted research in neuroscience. Dr. Karsten’s research work was published in over 30 peer-reviewed journals including Nature, Neuron and PNAS and resulted in several patents
Abstract:
Cell specific studies are imperative for sound research in molecular biology and biomedical research. Tissue heterogeneity (e.g., brain) poses significant challenge for retrieval of cell and region specific information. Moreover, recent progress in single cell research creates strong demand for rapid acquisition of individual cells from both tissues cell cultures. However, existing approaches of single cell acquisition, such as flow sorting and laser assisted microdissection are costly, sophisticated and often methodologically limited. We have developed a line of versatile instruments (e.g., KuiqpicKTM, UnipicKTM) which are compatible with any inverted microscope and have a wide range of cell and tissue acquisition parameters. Both instruments permit rapid collection of individual cells from various cell cultures and tissues for a range of downstream applications including function single cell studies, high quality protein, RNA and DNA isolation and sequence analysis. Collection of cells may be performed directly from native tissues and cell cultures with low impact on cellular viability. Native, fresh frozen, and sucrose treated tissues could be used for microdissection. Here, the recent progress in the instrument’s automation is presented further widening potential areas of application
Asokan C
Sokoto State University. Nigeria
Title: Role Of α-B Crystallin On Serum Amyloid A Fibrils And Effect Of β-Amyloid With Systemic Amyloidotic Mice Brain
Biography:
DR. Asokan C has completed his PhD at the age of 27 years from University of Madras and postdoctoral studies from Columbia University. NY. USA. He is the Associate Professor, Department of Biochemistry, Sokoto State University, Sokoto. Nigeria. He has published more than 36 papers in reputed journals and has been serving as an editorial board member of repute
Abstract:
Enhanced expression of amyloid β-peptide (Aβ) and deposition is the main causative factor in Alzheimer’s disease (AD). Factors that lead to the genesis of accumulation and toxicity of Aβs are yet to be identified. While studying the effect of systemic amyloid on the functions of the mice brain, it was accidentally found that the mice brains contain accumulated Aβs, which are extractable with hexafluroisopropanol (HFIP) solvent. By purifying with semi preparative HPLC on HFIP extracts, two major fractions containing mixture of Aβs with variable composition were observed. We have characterized these mixtures by electron microscopic and spectroscopic methods. Our results indicate that, the accumulated Aβ fibrils have similar morphological and conformational characteristics as that of Aβs of AD brains.
Peter Mikuš
University in Bratislava, Slovakia
Title: Two-dimensional capillary electrophoresis separation and on-line tandem mass spectrometry detection of antigripal drugs and their metabolites in urine matrices
Biography:
Peter Mikuš has completed his PhD at the age of 30 years from Comenius University (Slovakia). He is Researcher, University Teacher, Associated Professor, and Director of the Toxicological and Antidoping Center at the Faculty of Pharmacy Comenius University in Bratislava (FPCU) as well as Head of the Department of Pharmaceutical Analysis and Nuclear Pharmacy FPCU. A research team of P.M. is focused on the development, validation and application of advanced hyphenated analytical methods, based on a combination of 2D-separation and spectral (UV-VIS, MS/MS) techniques, for pharmaceutical and biomedical research. He has published more than 60 papers in reputed CC journals.
Abstract:
The advanced two dimensional isotachophoresis (ITP) – capillary zone electrophoresis (CZE) hyphenated with tandem mass spectrometry (MS/MS, here triple quadrupole, QqQ) was developed in the present work to demonstrate analytical potentialities of this approach in the analysis of antigripal drugs in multicomponent ionic matrices. This was demonstrated on the determination of pg.mL-1 levels of pheniramine, its desmethyl metabolite and phenylephrine in directly injected (unpretreated) urine samples, suitable for the monitoring of concentration vs. time dependences of these species. The main benefits of ITP-CZE-ESI-QqQ in comparison with CZE-ESI-QqQ are considerably higher sensitivity / lower LODs obtainable and more favorable parameters of precision and recovery/accuracy when performing analyzes at lower concentration levels. The separation selectivity of ITP-CZE-ESI-QqQ towards the targeted analytes is enhanced via the heart cut effect while CZE-ESI-QqQ has the advantage of utilization of the EOF effect for the monitoring additional (e.g. neutral) species related to the targeted analytes. Anyway, the on-line ITP sample preparation provides, besides pre-concentration and separation selectivity, also the maximum reduction of ionic sample matrix constituents entering MS. In this way, MS can be effectively protected (long-term working life is ensured), potential detection interferences are minimized and signal to noise ratio of the detection response is maximized. Obviously, ITP-CZE-ESI-QqQ is superior than ITP-CZE-UV regarding sensitivity/lower LOD, selectivity and identification reliability but disadvantageous regarding cost of instrumentation/analysis and the scale (number) of CE electrolytes usable for MS. The ITP-CZE-ESI-QqQ method has a great potential to be routinely applied for monitoring various targeted ultra-trace ionic drugs in biomedical/clinical laboratories.
Mercy Ekwere
Department of Biochemistry, Nigeria
Title: Comparative sex hormonal indices of male and female rats exposed to uppercott (mixture of organophosphate/ pyrethroid) pesticide.
Biography:
The effect of oral administration of a mixture of cypermethrin and dimethoate (organophosphate and pyrethroid groups of pesticide, commonly called uppercott) on serum sex hormonal profile of male and female rats was assessed. 10 mg/kg and 20 mg/kg body weight of uppercott were given to separated male (M) and female (F) rats grouped as F2, M2 andF3, M3 respectively. Rats in groups F1, M1 served as control. After 28days, the animals were sacrificed; sera collected and assayed for follicle stimulating hormones (FSH), Luteinizing hormones (LH), testosterone, estradiol and progesterone. Results showed that all serum sex hormones, for both male and female rats, were significantly altered as doses increased from control via 10 mg/kg to 20 mg/kg. FSH and LH were significantly reduced (p<0.05) in both male and female rats (M1FSH, M2FSH and M3FSH were 3.36±0.32 mIU/ml, 2.32±0.31mIU/ml and 1.9±0.15mIU/ml and F1FSH-3.32±015, F2FSH- 2.48±0.17 and F3FSH, 1.96±0.13. Estradiol and progesterone in the female rats; and testosterone for male rats decreased significantly (p<0.05). Toxic effects of uppercott on testosterone and progesterone male and female rats respectively, were not significantly different (p>0.05) from each other. Uppercott significantly reduced all sex hormonal levels especially at higher dose. Constant exposure to high concentration of organophosphate and pyrethroid pesticides could have toxic effects on male and female fertility and reduce reproductive integrity. A limit should be placed on the use of such toxic pesticides/insecticides.
Abstract:
The effect of oral administration of a mixture of cypermethrin and dimethoate (organophosphate and pyrethroid groups of pesticide, commonly called uppercott) on serum sex hormonal profile of male and female rats were assessed. 10mg/kg and 20mg/kg body weight of uppercott were given to separated male (M) and female (F) rats grouped as F2, M2 and F3, M3 respectively. Rats in groups F1, M1 served as control. After 28days, the animals were sacrificed; sera collected and assayed for follicle stimulating hormones (FSH), Luteinizing hormones (LH), testosterone, estradiol and progesterone. Results showed that all serum sex hormones, for both male and female rats, were significantly altered as doses increased from control via 10mg/kg to 20mg/kg. FSH and LH were significantly reduced (p<0.05) in both male and female rats (M1FSH, M2FSH and M3FSH were 3.36±0.32mIU/ml, 2.32±0.31mIU/ml and 1.9± 0.15mIU/ml and F1FSH-3.32±015, F2FSH- 2.48±0.17 and F3FSH, 1.96±0.13. Estradiol and progesterone in the female rats; and testosterone for male rats decreased significantly (p<0.05). Toxic effects of uppercott on testosterone and progesterone male and female rats respectively, were not significantly different (p>0.05) from each other. Uppercott significantly reduced all sex hormonal levels especially at higher dose. Constant exposure to high concentration of organophosphate and pyrethroid pesticides could have toxic effects on male and female fertility and reduce reproductive intergrity. A limit should be placed on the use of such toxic pesticides/insecticides.
Asokan C
Department of Biochemistry, Nigeria
Title: Characteristics of Fibrillar form of β-Amyloid Peptide Fractions from Mice Brain affected by Systemic Amyloidosis.
Biography:
DR. Asokan C has completed his PhD at the age of 27 years from University of Madras and postdoctoral studies from Columbia University. NY. USA. He is the Associate Professor, Department of Biochemistry, Sokoto State University, Sokoto. Nigeria. He has published more than 36 papers in reputed journals and has been serving as an editorial board member of repute.
Abstract:
Enhanced expression of amyloid β-peptide (Aβ) and deposition is the main causative factor in Alzheimer’s disease (AD). Factors that lead to the genesis of accumulation and toxicity of Aβs are yet to be identified. While studying the effect of systemic amyloid on the functions of the mice brain, it was accidentally found that the mice brains contain accumulated Aβs, which are extractable with hexafluroisopropanol (HFIP) solvent. By purifying with semi preparative HPLC on HFIP extracts, two major fractions containing mixture of Aβs with variable composition were observed. We have characterized these mixtures by electron microscopic and spectroscopic methods. Our results indicate that, the accumulated Aβ fibrils have similar morphological and conformational characteristics as that of Aβs of AD brains.
Radim Vespalec
Academy of Sciences of the Czech Republic,Czech Republic
Title: Analytical task stemming from therapeutical prospects of electron deficient boron cluster compounds
Biography:
Radim Vespalec has received equivalent to PhD from the Institute of Physical Chemistry, Academy of Sciences of the Czechoslovak Republic, Praha, in 27. The scientific degree Dr.Sc. he received from Technical University of Pardubice in 57, the pedagogical Asoc. Prof. degree he received from Masaryk University Brno in 58. He is senior scientist in the Institute of Biophysics. Web of Science reports his 80 scientific articles He contributed to 3 monographs.
Abstract:
The existence, reactions, structures and properties of compounds occurring in nature, and their synthetic analogues are explainable by the idea of two-center two-electron bond. These families contain either electron exact or electron rich building blocks from the viewpoint of electron structure. Electron deficient building blocks have never been found in nature, and exist only in synthetic species. Boron cluster compounds (BCCs) create the most intensely investigated family of species with electron deficient cluster. Their existence has been explained by the accumulation of unique electron deficient bonds, which bind together three boron atoms or, sometimes, their substitutes, in clusters. Pronouncedly electron deficient clusters either determine or substantially affect properties of BCCs, and their prospects. Therapeutical prospects attract the highest attention now, and many compounds with boron clusters are synthesized as candidates for therapeutical uses. These compounds must pass through mandatory studies and checks, which require variety of chemical analyses, identically with other compounds. However, analytical methods do not exist for analyses of compounds with boron clusters. The pieces of knowledge from chiral separation of BCCs prove the dissimilarity of some analytical properties of species with and without boron clusters, and indicate the absence of criteria for the a priori estimation of different analytical properties for compounds with and without clusters. Thus, missing analytical methods cannot be derived from existing knowledge. Analytical research of BCCs motivated by their medical prospects is the best way to preventive elimination some obstacles, which may hamper medical uses of compounds with boron clusters.
Doo Soo Chung
Seoul National University, Korea
Title: Sensitive Speciation of Arsenic Compounds with Capillary Electrophoresis
Biography:
Doo Soo Chung has completed his PhD from Harvard University and postdoctoral studies from MIT and Iowa State University. He has published more than 100 papers in reputed journals.
Abstract:
Arsenic is naturally abundant in the crust of the earth and introduced into the aquatic system through dissolution and weathering of minerals. Chronic ingestion of arsenic in water may cause various diseases, including cancer and keratosis. A guideline for arsenic in drinking water has been set at 10 ppb of total arsenic by the World Health Organization (WHO). However, inorganic forms of arsenic, such as arsenites [As (III)] and arsenates [As (V)], are much more toxic than the organic forms as the mono methylarsonic acid (MMA) and dimethylarsinic acid (DMA). Hence the quantitation of specific arsenic species may be more meaningful than the total arsenic determination for the evaluation of the health risks from arsenic-contaminated drinking water. We report a highly sensitive way of arsenic speciation using a commercial Capillary Electrophoresis (CE) instrument equipped with a UV absorbance detector. We used a counter-flow electrokinetic supercharging technique to enhance the detection sensitivity. Electrokinetic supercharging is one of the most powerful sample stacking methods that combine field amplified sample injection and transient isotachophoresis. In counter flow electrokinetic supercharging, a constant counter pressure is applied during sample injection in order to counterbalance the movement of the injected sample zone, obtaining a pronounced increase in the amount of sample injected and the portion of the capillary available for electrophoresis.
Fabiano Freire Costa
Federal University of Juiz de Fora, Brazil
Title: Microfluidic Chip Electrophoresis Investigation of Major Milk Proteins: Study of Buffers Effects and Quantitative Approaches
Biography:
Dr. Fabiano completed his post-doctorate in advanced milk chemistry with the theoretical and practical combination of microfluidic chip electrophoresis, scanning electron microscopy, transmission electron microscopy, differential scanning calorimeter and static light scattering at the Embrapa Dairy Cattle National Research, Brazil in 2013. He joined at the Federal University of Juiz de Fora/Governador Valadares, Minas Gerais, Brazil in 2013 as a Professor. This led to the development of new methodology to analyze milk. Dr. Fabiano is member of the International Dairy Federation acting in the working groups: Analytical Methods for Additives & Contaminants (SCAMAC); Analytical Methods for Composition (SCAMC); Food Additives (SCFA) and Inventory of Methods and Procedures to Monitor the Integrity Supplier's Milk (TF-ISM-01).
Abstract:
The separation and quantification of major milk proteins are fundamental in dairy research. Therefore, accurate and rapid methods are profoundly important. The microfluidic chip technique is faster, and uses considerably fewer chemicals and materials than traditional techniques. The objective of this study was to improve experimental methods for separating and quantifying major milk proteins using the microfluidic chip technique. Deionized water, a total protein solubilization buffer (TPS buffer) and a separating milk protein buffer (SEP buffer) were added to the treatment of milk samples and their effects were evaluated. The results showed an excellent separation of whey proteins with α-lactalbumin migrating first, followed by β-lactoglobulin in the presence of both buffers. However, better results for major case in separation were achieved when the SEP buffer was added. The order of the migration time was: β-casein first, followed by αs-casein and κ-casein. The quantitative analysis showed significant differences among the percentages of protein fractions from both buffers. The results using microfluidic chip technology using the SEP buffer solution were comparable to those obtained by SDS-PAGE for these proteins and with the data reported in the literature.
Z. Mansoori
Amirkabir University of Technology, Iran
Title: Numerical investigation of gas- solid separation by liquid layer in horizontal pipes
Biography:
Zohreh Mansoori completed her PhD in Mechanical Engineering from Amirkabir University of Technology (Polythechnic), Tehran, Iran. She is associate professor and the head of Energy Research center in Amirkabir University of Technology. She has published more than 35 papers in reputed journals and has been serving as an editorial board member of repute.
Abstract:
Gas- solid separation is studied considering a liquid layer in the lower part of horizontal pipe. The particles falling in liquid layer could not go back in gas flow. The presence of solid particles on stratified wavy gas- liquid flows has been studied. In present paper, the numerical four- way simulation of solid particles in gas- liquid wavy stratified flow has been used. The computational model is shown to be able to evaluate the effect of the liquid layer on particles separation.