Day 1 :
Keynote Forum
Haifei Zhang
University of Liverpool, UK
Keynote: The development of spheres-on-sphere silica particles for fast and efficient HPLC separation
Time : 10:00-10:35
Biography:
Haifei Zhang is a Senior Lecturer in the Department of Chemistry at University of Liverpool. He has completed his undergraduate and Master degrees in Chemical Engineering and PhD in Physical Chemistry from Chinese Academy of Science. He has published 90 peer reviewed research papers with h-index of 29 and filed 9 international patents as a Co-inventor. He won the 12th Desty Memorial Award in 2007 for his innovative work in the manufacture of porous materials and their possible application in chromatography. He has also written five book chapters and one book (to be published by Wiley in 2018). His main research interests are on porous materials, colloids, carbon materials, and nanostructured materials for separation and energy storage applications.
Abstract:
Core-shell silica particles have been developed and employed by various manufacturers for fast and efficient HPLC separations with relatively low back pressure. However, core-shell silica particles are usually fabricated by the time-consuming layer-by-layer technique and usually followed by a lengthy classification process to obtain uniform particles. Recently, we have developed a one-pot synthesis method at room temperature to produce the unique spheres-on-sphere (SOS) silica particles. These SOS particles are comprised of silica nanospheres attached to silica microspheres. The size and number of silica nanospheres are tunable. The interstices between the surface silica nanospheres on the solid microspheres generate the macroporosity for fast and efficient HPLC separations with low back pressure, particularly for large bio-macromolecules. Importantly, these SOS particles are very uniform directly from synthesis (hence classification in unnecessary) and mesoporosity and additional functional particles may be introduced so that these particles can be efficiently used for fast separation of a wide range of analytes, including peptides, proteins, small molecules, and isomers. This talk will cover the preparation and characterization of SOS particles and their various applications in HPLC.
Keynote Forum
Sergio Guazzotti
Thermo Fisher Scientific, USA
Keynote: Ion chromatography solution for applied pharmaceutical markets
Time : 10:35-11:10
Biography:
Sergio Guazzotti is a Senior Global Marketing Director for ion chromatography and sample preparation at Thermo Fisher Scientific. Prior to this role, he was the Global Marketing Director for gas chromatography/gas chromatography-mass spectrometry also at Thermo Fisher Scientific. He joined the company in 2008 as Senior Global Strategic Marketing Manager for HPLC and was later appointed as Senior Integration Manager to assist the integration of Dionex Corporation into Thermo Fisher Scientific. Prior to joining Thermo Fisher Scientific, he was the Vice President of Engineering and Technical Services at Nanostream, Inc. Earlier in his career, he was a Professor of Analytical Chemistry at the University of California, San Diego. He holds a PhD degree in Chemistry from the University of California.
Abstract:
An accurate understanding of the contents of any pharmaceutical entity helps to ensure both drug efficacy and patient’s safety. Over several decades, there has been significant improvement in the analytical methods and techniques ensuring critical quality attribute analysis of the pharmaceutical products. The solutions offered by Dionex Ion Chromatography systems are widely adopted and are everyday gaining more traction because of the several technological advancements and benefits in these Dionex IC systems. These advancements include superior accuracy, high-throughput, improved reliability, and environmental safety concerns which significantly contribute towards the critical analysis of the drug entity of interest. IC primarily relies on suppressed as well as non-suppressed conductivity detections for ionic species in pharmaceutical samples. Dionex IC systems can accurately analyze multiple anions/cations in a single injection, thereby, accelerating the analysis throughput. The productivity can be further improved by converting the single channel system to a dual-channel system where two different samples can be concurrently analyzed. Most recent advancement, Consumables Device Monitor, can automatically identify and tracks the installation time, use, and performance metrics of all the installed IC consumables. This feature can reduce any associated downtime due to consumable installation errors and can even schedule preventive maintenances. Such smart capabilities can significantly improve the productivity as well as lessen the burden on the analysts’ time in a fast-paced pharmaceutical laboratory. All modern IC systems can make eluents automatically, allowing the consistent and reliable production of high purity IC eluent concentrations. The only routine reagent then needed is high-purity water. Consequently, the instrument pump seals and pistons only come into contact with deionized water instead of acids and bases which can precipitate. This extends the lifetime of pump seals and pistons, and significantly reduces the overall pump maintenance requirements. Dionex IC systems are constantly evolving with the changing times and needs. Recent IC systems are equipped with a tablet supporting 11 different languages with an intuitive interface. This tablet control enables direct local control of the system and its status. All these enhanced capabilities and advancements have only led to the successful adoption of IC for analyzing ionic species in pharmaceutical applications.
- Analytical and Bioanalytical Applications of Chromatography-HPLC | Biochemical Applications of Chromatography-HPLC | Chromatography-HPLC in Bio-Medical research | Chromatography-HPLC in Food Sciences Chromatography-HPLC in Pharmaceutical Analysis
Location: Barcelona, Spain
Session Introduction
Mladen Krajacic
University of Zagreb, Croatia
Title: Monolithic chromatographic supports employed in virus separation and purification
Biography:
Mladen Krajacic is a Full Professor at University of Zagreb where he completed his PhD in Virology. As a Head of the Laboratory and Principal Investigator in several research projects, he has been leading the molecular biology investigations on viruses, sub-viral agents (viroids, satellite RNAs) and non-cultivable bacteria. During the last decade, he has dedicated to chromatography on monolithic supports and its appliance in separation of viral and sub-viral ribonucleic acids, as well as virus particles. His results have been published in prominent scientific journals in which he has regularly been employed as a Reviewer. He was supervising a number of young research fellows who have received positions from well recognized institutions across the world.
Abstract:
The particular structure of monolithic chromatographic supports has been proved highly advantageous in analytic separation and purification of large biomolecules. Characterized by very high porosity, high binding capacity, and high flow rate based on convective mass transport, monoliths are particularly applicable in virus research. Monolith chromatography has hardly any limitation to be applied in processing of virus particles, huge macromolecular complexes, and viral genomes, especially when being distinct from nucleic acid forms present in the host cell. The majority of trials published so far, have exploited ion exchange carriers, although other chemistries are also applicable, like hydrophobic interaction when concentrating viruses from marine environment. According to papers published over the past decade, viruses of different sizes, structures and morphologies, even virus-like particles, have successfully been purified from tissue homogenates or cell lysates. Moreover, following virtual separation by overlapping chromatograms obtained from separate experiments, a real separation of three virus species, and a distant strain of one of them (four viral fractions in total) was accomplished from laboratory prepared mixture. One of the most recent achievements is a proof of principle that virus chromatographic feature could easily be modified without abolishing its structural stability, or its biological activity. As adenoviruses have been used in almost a quarter of human gene therapy trials, the experiment was conducted with an adenoviral vector. The deletion of just two negatively charged amino acids from the main structural protein was efficient in shortening chromatographic retention of the recombinant adenovirus. In this way, it would be possible to shift virus particles away from particular interfering substances present in the crude lysate. The concept might be followed to facilitate chromatography-approach purification by engineering modifications contributing to virus separability, besides those contributing to its therapeutic functionality.
Fotios Tsopelas
National Technical University of Athens, Greece
Title: Immobilized artificial membrane chromatography as a tool in medicinal chemistry and in environmental sciences
Biography:
Fotios Tsopelas is a Lecturer in the School of Chemical Engineering at National Technical University (NTUA), Greece. He studied Chemical Engineering in the NTUA (1999) and Pharmacy (2004) in the National and Kapodistrian University of Athens. He completed his PhD in 2007 in Environmental Analytical Chemistry at NTUA (scholarship from Onassis Foundation) and his Postdoctoral research was focused on biomimetic chromatography for novel drug design. He has more than 25 publications in peer-reviewed scientific journals and more than 40 contributions in international conferences. He has acted as a Referee in more than 20 international journals. He has participated as a member of scientific committee in two international conferences. He has coordinated five national and international funded research projects. His research interest is mainly focused on the development of biomimetic chromatographic approaches for the evaluation of pharmacokinetic properties of candidate drugs and ecotoxicity of emerging pollutants.
Abstract:
Pidgeon and his coworkers described for the first time in 1989, the immobilization of phosphatidylcholine to propylamino-silica skeleton and up to now immobilized artificial membrane (IAM) chromatography have been employed for simulation of the environment of cell membranes. In particular, IAM chromatography constitutes a valuable tool for medicinal chemists for prioritization of drug candidates in the early drug development stages. The retention outcome on IAM stationary phases encodes lipophilicity, electrostatic and other secondary interactions in contrary to traditional octanol-water partitioning. An increasing number of publications in recent years suggest that IAM indices, including isocratic logk(IAM) or extrapolated logkw(IAM) retention factors, hydrophobicity index CHI(IAM) which corresponds to the percentage of acetonitrile required for equal partitioning of the solute between mobile and stationary phase (i.e. logk=0) or the polarity parameter Δlogkw(IAM) can successfully model the passage of xenobiotics through biological membranes and barriers and predict pharmacokinetic properties, often in combination with additional descriptors. More recently, IAM chromatography is applied to estimate toxicological endpoints in regard to drug safety, such as the phospholipidosis potential, or in regard to chemicals risk hazard including the bio-concentration factor and aquatic organisms’ toxicity. The presentation will be devoted to applications of IAM chromatography to medicinal chemistry and environmental sciences. Examples referring to modeling of human oral absorption, blood-brain penetration, skin partition as well as bioconcentration factor and median toxicity (LC50) in aquatic organisms will be discussed. The combination of promising results in both medicinal chemistry and in environmental science with the speed, reproducibility and low analyte consumption suggest that a broader application of IAM chromatography in early drug discovery process and in ecotoxicity is expected in initial drug candidate selection and contribute to reduced risk hazard of chemicals.
Monika Šuleková
University of Veterinary Medicine and Pharmacy in Košice, Slovakia
Title: The study of naproxen desorption from the silica by RP-HPLC
Biography:
Monika Šuleková has completed her Graduation at the University of Pavol Josef Šafárik in Košice, Slovakia. During her university studies, she spent half a year at Friedrich-Schiller University in Jena, Germany where she studied Analytical Chemistry. Nowadays she works as a Teacher at the University of Veterinary Medicine and Pharmacy in Košice, Slovakia as well as a Researcher in the field of desorption of drugs from mesoporous silica modified by different functional groups, and in determination of synthetic dyes in pharmaceutical products by the RP-HPLC method.
Abstract:
Naproxen, a non-steroidal anti-inflammatory drug (NSAID) is widely used to moderate pain relief in the treatment of many diseases. Naproxen has analgesic and antipyretic properties. Mesoporous silica SBA-15 was prepared to evaluate its application as naproxen drug delivery system. The amount of naproxen released from the pores of mesoporous silica SBA-15 into the solutions was determined by the method of a reverse-phase high performance liquid chromatography (RP-HPLC). SBA-15 having 3-aminoprophyl-, methyl-, fenyl-and cyclohexyl-surface groups was successfully prepared by the grafting of SBA-15 with the corresponding alkoxysilanes. The release of the drug was performed in two different media, in a simulated body fluid (pH 7.40) and in a simulated gastric fluid (pH 2.06). The HPLC system Dionex Ultimate 3000 RS (Thermo Fisher Scientific, Germany) consisted of a quaternary pump, a degasser, an automated injector, a column oven and a diode array detector DAD. HPLC system was used, with stationary phase ODS Hypersil C18 column (150x4.6 mm, 3 μm). To determine the concentration of naproxen, the calibration curve has been established based on five solutions of different concentrations of naproxen. The linearity was determined by threefold repeating measurement of each concentration step. The mixture of acetonitrile and water (55:45, v/v) adjusted with ortho-phosphoric acid to pH 3 was selected as the best mobile phase. The flow rate was 1 mL/min and detection was carried out at a wavelength of 229 nm. During the chromatographic separation, the mobile phase was kept isocratic. The release of the drug was studied as a function of time and the results are shown in Figure.
Clydewyn M Anthony
The United States Pharmacopeial Convention (USP), USA
Title: Chiral HPLC resolution of a potentially serious global health crisis
Biography:
Clydewyn M Anthony is a Senior Scientific Liaison in the Chemical Medicines Division at The United States Pharmacopeial Convention (USP) and is currently responsible for the modernization of documentary standards for Over-The-Counter drug formulations. He completed his PhD in Analytical Chemistry at The Pennsylvania State University and BS in Chemistry in Hunter College at the City University of New York. Prior to joining USP in May 1999, he worked as a Research Chemist with Texaco Inc. where he was responsible for performing and overseeing the compositional analyses of motor oils, gasolines and all aftermarket petroleum related products on both the domestic and international markets. He also held the position of Criminalist with the New York Police Forensic Investigation Department, worked on thousands of narcotics and arson related cases, and testified as an Expert Witness on behalf of the New York City Police Department.
Abstract:
A few years ago there was a potentially serious health issue in Pakistan and Paraguay which spurred investigation and responsive action by both the United States Pharmacopeial Convention (USP) and The Food and Drug Administration (FDA). This crisis resulted in the deaths of adults and children who had ingested Dextromethorphan Cough Syrup. It was later determined and confirmed that toxic levels of the controlled substance, levomethorphan, an enantiomer of dextromethorphan, was found in the drug formulation and was responsible for the resulting deaths. USP has thus charged with developing a quantitative procedure for monitoring levomethorphan and simultaneously incorporating this method as a revision to the documentary standard within its compendium. At the time of the public health issue, the existing USP Dextromethorphan monograph did not include a quantitative procedure for the determination of its enantiomer, levomethorphan. Hence a chiral HPLC method was developed to bring the monograph up-to-date and simultaneously address obvious safety concerns associated with the enantiomer. The proposed HPLC method separates levomethorphan and dextromethorphanone (another impurity, dextromethorphan Related Compound C) from dextromethorphan; and allowed quantitation to satisfy acceptance criteria requirements for these impurities (0.10%). Hence, manufactured lots which test higher than the specified limit of levomethorphan can be rejected thus helping to prevent potential safety issues in the future. A complete overview of the issues encountered in the development of this chiral HPLC method along with the challenges associated with the implementation of a global procedure which utilizes a schedule 11 controlled substance as a public standard will be presented.