8^th World Congress on Chromatography September 13-14, 2018 Prague, Czech Republic | Panorama Hotel Prague | Milevská 7, 140 63 Praha

Biography:

Gilles Goetz is a Principal Scientist at Pfizer in Groton, Connecticut, USA. Gilles received his B.Sc. (1991) and Ph.D. (1995) at the University of Strasbourg in France. After post docs at the University of Hawaii (1996-97) and of Neuchatel (CH) (1998-99) studying marine and fungal natural products, he joined Monsanto in 2000. There he worked through mergers and acquisitions for Pharmacia and Pfizer successively in the Natural Product group, the HTS group (analytical support), and the Purification Group. In 2010 he transferred to the Expert Purification Group at Pfizer Groton and in 2011 to the Molecular Properties Group. He is part of the team influencing medicinal chemistry design through insights into molecular properties such as polarity, lipophilicity, shape, and conformation that will impact molecular behaviors like solubility, permeability, and efflux. They develop and use mainly chromatographic techniques (EPSA) to assess those properties, and work towards predicting molecular behaviors.

Abstract:

Applications of a new chromatographic method using SFC technology developed recently at Pfizer are described here. The EPSA method, as readout of polarity, correlates retention on a specific stationary phase with the exposed polarity of a molecule. Changes in retention can be interpreted by changes in polarity induced by the presence of Intra-molecular Hydrogen Bonding (IMHB): indeed, IMHBs tend to impact molecular conformation, inducing hidden polarity that results in a decrease in analyte retention on the EPSA support. We demonstrate here the impact of this method on multiple Beyond Rule of 5 projects (NS5A, Oxytocin Receptor, CXCR7 Modulator, others). Given that conformational changes (induced and/or stabilized by the formation of IMHB) increases potential for membrane permeability, we show here that EPSA, and the EPSA prediction model, have significant impact in peptide drug design.

Biography:

Mr. Abraham George is working as the Section Head of Analysis at ADNOC Refining Research Centre. He has 25 years of experience in the area of petroleum Inspection & Laboratory Analysis. He Graduated in Chemistry and obtained Master’s Degree in Business Administration from Mahatma Gandhi University, India. Worked in various capacities in managing laboratories in India, Saudi Arabia and in U.A.E and involved in Inspection and analysis of entire range of crude Oil, petroleum products and other materials. He is a certified Lead Auditor in ISO 9001:2008 QMS from Lloyds Register Quality Assurance.

Abstract:

Statement of the Problem: Petroleum product slop generated in products distribution terminals contains different products handled within the terminal, specifically unleaded Gasoline which contains MTBE (Methyl tertiary butyl ether) blended as additive. These slops are injected into the atmospheric residue stream feeding the refinery vacuum distillation unit as a recycling option. Due to this optional blending of MTBE containing slops to the Vacuum distillation (VD) feeds, there are concerns over possibility of MTBE carry over in the vacuum distillation products which might have an impact on the hydrocracking catalyst and the quality of the products specifically Naphtha. The objective of this case study is to determine the MTBE content in the vacuum distillation products like Light Vacuum Gas Oil & Heavy Vacuum Gas Oils (LVGO & HVGO). Since there are no standard test methods exists to determine the content MTBE in VD products. The purpose of this study is to develop a chromatographic method for identification and quantification of MTBE in heavy hydrocarbon matrices.

Methodology & Theoretical Orientation: Various heavy hydrocarbon matrices starting with Light Vacuum Gasoil, Heavy Vacuum Gasoil, and Straight Run Residue were selected as representative heavy hydrocarbon matrix. Temperature conditions from 90°C to 180^°C with an increment of 30°C were selected for study in GC-HS. Optimized GC Headspace parameters and GC parameters for all the matrices.

Findings: After the laboratory study using various heavy hydrocarbon matrices at various temperatures, it is observed that Gas Chromatography Headspace Technique can be used for the identification and quantification of MTBE. Also derived a Theoretical equation for the quantitation in specific matrix. Results obtained theoretically and practical measurements are well within the repeatability window of the gas chromatography headspace technique.

Biography:

Dawei Cao is a PhD candidate under the supervision of Prof. Shuming Peng (China Academy of Engineering Physics) and Prof. Zhengjun Zhang (Tsinghua University). He graduated from Amoy University in 2012. His current research concentrates  on the separation and analysis of hydrogen isotopes.

Abstract:

Hydrogen isotope separation is among the key technological problems in realizing the peaceful utilization of nuclear fusion energy, moreover, gas atmosphere in the process flow of ITER fuel cycle is more than complexity. Thus, making effective separation and analysis of hydrogen isotopic mixtures necessary and an urgent task to be addressed. As hydrogen isotopes share almost identical shape, size, and chemical properties, separating and analyzing of hydrogen isotopes is really not an easy task. In this letter, ultralow temperature separation of H₂/D₂ mixture through quantum sieving was experimentally examined on two metal-organic framework (MOF) materials, with an extreme two-dimensional confinement formed within the material of {[Fe(OH)(H₂bta)](H₂O)}_n experienced by hydrogen molecules, an extraordinary separation factor of H₂/D₂ as high as 41.4±0.4 at 20 K was finally experimentally obtained. Furthermore, MOF material CPL-1 ([Cu₂(pzdc)₂(pyz)]_n) was further tested as the stationary phase of gas chromatography for the analysis of H₂/HD/D₂ mixtures, with a large specific surface area and uniform pore size, CPL-1 showed a better adsorption of H₂/D₂ in capacity than that of MnCl₂@γ-Al₂O₃ and γ-Al₂O₃, and CPL-1 packed column showed more rapidly in signal detection, i.e., less retention time, than that of MnCl₂@γ-Al₂O₃ toward H₂/HD/D₂ under a condition of 77 K and carrier gas (Ne) flow rate of 3 ml/min. With a sampling volume of 0.25~2.0 ml, GC with CPL-1 packed column showed good linear respondence toward measurement of H₂/HD/D₂ mixtures with mean relative error less than 4 %, showing promising potential use of MOF material in hydrogen isotope chromatographic analysis.  

Biography:

With a background in analytical chemistry, I had the opportunity of developing my thesis in collaboration with an enterprise dedicated to the production of fluorinated substances. The aim of the researches was focused on the development of fast and green analytical methods, for the quality control and production processes to be implemented. Through my experience in development of analytical methods, it has allowed me to work on a variety of analytes such as inorganics, organics in liquid or solid state in different fields: industrial, environmental and forensic ones.

The experience acquired in the drug department since 2012, following a 2-years postdoctoral position, has been focused to: the development of the actual analytical methods for the routine analysis of major and minor components in heroin and cocaine illicit drugs by fast GC-MS, reporting caseworks for the tribunal of justice as well as the collaboration to obtain the ISO accreditation 17025 for the laboratories of the Service of Expertise in the drug department.

Abstract:

The present work is focus on the optimization and validation of the analytical method by fast-GC-MS for the determination of cocaine, and identification of minor alkaloids and most common cutting agents in powders seized by the law enforcement.

Optimization procedure was a deal between the sensibility, signal saturation and time analysis for the identification of minor alkaloids in the presence of a large amount of some substances as it occurs in some real cases. Injection temperature and volume, split ratio as well as the temperature ramp for the separation were the optimized instrumental variables.

The validation was performed using interlaboratory samples of cocaine. For this purpose, the accuracy profile procedure was applied in order to evaluate the capability of the method to quantify samples with a known accuracy and a fixed risk at 5%. The analytical method was accredited by the Swiss Accreditation Service (SAS) according to the UNE-EN ISO/IEC 17025:2005 guidelines.

The method is used as a routine analysis in the forensic laboratory and allows not only the quantification of cocaine but also the profiling analysis of the minor alkaloids in less than 6 min per run.

The profiling study provides information as an added value to the law enforcement, since it provides information about links among cocaine street samples using Pearson correlation coefficients, principal components analysis (PCA) and hierarchical cluster analysis (HCA).

Biography:

Lourdes Hernández has her expertise in the design of purification process for recombinant proteins. She has 10 years of experience in the field of Biotechnology and held positions within development and project management. She holds a Master in Science in Engineering for Biotechnology Process from Faculty of Chemical Engineering in the Higher Polytechnic Institute José Antonio Echeverría, Havana, Cuba.  Lourdes has involve in the evaluation and application of the new designs of chromatography supports for increase the productivity of the productive process of recombinant protein such as EPO and monoclonal antibodies.

Abstract:

Chromatographic techniques are employed in the purification step of hr-EPO production process in order to obtain a reliable product with high purity. Anion exchange chromatography supports have proved high efficient in removing contaminants such as DNA. For that reason the DNA removal was determined by spike studies, on three anion exchange chromatographic supports: gel, membrane and monolithic column; used in intermediate purification stage. This study showed that membrane and monolith columns have very good results in the removal of contaminants at this step. Log removal values (LRV) greater than 3.5 were obtained from DNA spike clearance studies. Monolithic column was determined as the best technological proposal, with more than 4 LRV and 7.72 mg DNA per mL of adsorbent. Scaling-up 8 fold of this step using monolithic column resulted in good process performance and DNA clearance. The results of this study may be used in the selection of commercially available chromatography supports for intermediate purification steps for other recombinant protein.

Biography:

Dr. Mohammed A. Al-Meetani has received his PhD Degree in applied analytical chemistry from Colorado School of Mines, Colorado, USA in 2003. His research encompasses various topics in the areas of pyrolysis mass spectrometry of the peptide and proteins, degradation of organic water pollutants using advanced oxidation processes, determination of human derived chemicals in ground and wastewater, and development of analytical methods for detection and determination of designer drugs of abuse. Dr. Meetani’s work has resulted over 40 articles in reputed journals and international conference proceedings. He has worked at different international universities and research institutes such as national renewable energy laboratory (NREL), CO, USA, University of Wyoming, Wy, USA, and Sam’s Nobel Foundation, OK, USA.

Abstract:

A statement of the Problem: the latest version of new designer substances (NDS) is called “bath salts” and they g spread in the drug of abuse market. Bath salts are a group of central nervous system stimulants that consists mainly of synthetic cathinone derivatives. They are chiral substances that exist as a racmic mixture. Objectives: Development and validation of sensitive and selective method for enantioseparation and quantitation of synthetic cathinones “bath salts” has been done by using GC-MS (SIM) with chemical ionization source in negative mode (NCI). Methodology:  Indirect chiral separation of thirty six synthetic cathinone compounds has been conducted by using optically pure chiral derivatizing agent (CDA) called (S)-(–)-N- (trifluoroacetyl)pyrrolidine-2-carbonyl chloride (L-TPC) which converts cathinone enantiomers into diastereoisomers that can be separated on achiral GC-MS columns. Ultra inert 60 m column was used. Slow heating rate (2 ^oC/min) on the GC oven has resulted an observed enhancement in enantiomer peak resolution. An internal standard, (+)-cathinone, was used for quantitation of synthetic cathinone. Conclusion & Significance:  Method validation in terms of linearities, limits of detection (LOD), limits of quantitation (LOQ), recoveries and reproducibilities have been obtained for fourteen selected compounds that ran simultaneously as a mixture after being spiked in urine and plasma. Unlike the Electron Impact ion source (EI), NCI showed higher sensitivity by three orders of magnitude by comparing with the previous results.. Moreover, signal intensity improvement observation after changing the CI reagent gas from methane to isobutane, argon or methane/ammonia (95:5) will be discussed.

Biography:

Tomasz Tuzimski is adjunct professor in Department of Physical Chemistry at Faculty of Pharmacy with Medical Analytics Division, Medical University of Lublin, Poland. Tomasz Tuzimski received MA degree and PhD degree (in 1995 and 2002, respectively), and Doctor of Sciences (habilitation) degree (in 2012) at the Faculty of Pharmacy with Medical Analytics Division, Medical University of Lublin. His scientific interest include the theory and application of liquid chromatography, extraction (QuEChERS) and detection techniques. He is authored or co-authored more than 62 scientific papers (IF = 100, H-index = 17). He is member of the editorial board of the Acta Chromatographica. He is quest editor of special sections on pesticide residues analysis in the JAOAC Int. Tomasz Tuzimski co-authored and co-edited with Professor Joseph Sherma the book entitled ‘High Performance Liquid Chromatography in Pesticide Residue Analysis’ (2015) and the book ‘Determination of Target Xenobiotics and Unknown Compounds Residue in Food, Environmental and Biological Samples’ (2018; CRC Press). Dr hab. Tomasz Tuzimski is promoter of one doctorate (2017) and research work of 6 masters of pharmacy and supervised the research work of 10 masters of pharmacy.

Abstract:

Bisphenols are a class of chemicals with two hydroxyphenyl functionalities, which include bisphenol A (BPA) and several analogues such as BPS, BPB, BPF, BADGE, BADGE • 2H₂O,  BADGE • 2HCl. As industrial chemical, BPA is widely used in the production of polycarbonate (PC) plastics (used in food contact materials, such as food containers, baby food and water bottles), epoxy resins (used as internal coating in canned food and beverage to prevent the food to get in contact with the metal wall and the deterioration of cans) and as an antioxidant in polyvinyl chloride (PVC) plastics in materials intended to come into contact with food (packaging cling films). Due to endocrine disruptor potential and estrogenic activity of the compound, the BPA release from packaging or storage containers into foods and beverages is a great public health concern. The release of BPA into the food depends on the type, pH and lipid content of food, temperature, and contact time. Due to their fat content, both breast and dietary milk could be polluted by many xenobiotics characterized by lipophilic properties. Milk and dairy products are widely consumed by infants, children, and many adults throughout the world, and occurrence of quantifiable amounts of BPA represents a matter of public health concern. European Commission (EU) has established a migration limit of 0.6 mg/kg for BPA in food or food simulant from plastic materials and articles intended to come in contact with foodstuffs (Regulation (EU) No. 10/2011) and has interdicted the BPA use in the fabrication of baby bottles (Regulation (EU) No.321/2011). Considering that many estrogenic effects caused by BPA occur at concentrations below the recommended safe daily exposure and that children are particularly vulnerable, a new risk assessment has been strongly recommended for consumer health protection. The aim of the paper was determination of xenobiotics (BPA and its analogues, pesticides, dyes) in natural and biological samples (e.g., breast milk) and food products.

Biography:

V. A.  Krylov, Doctor of Chemistry, Professor, Head of the Division of Analytical Chemistry of the Nizhny Novgorod State University. In 1980 – 2015 he was the head of the Laboratory of Analytical Chemistry of High Purity Substances at the Institute of the Chemistry of High Purity Substances of the Russian Academy of Sciences. The main direction of scientific research of professor Krylov is the development of the theory and applications of chromatography for the analysis of high purity substances, environmental objects and development of methods of the microextraction. The attained detection limits for molecular impurities constitute 10^–6 to 10^–11wt % and hit a record low. He is the author of more than 200 scientific papers, including reviews on the analytical chemistry of high purity volatile substances, air and liquid-liquid  microextractionpreconcentration.

Abstract:

Esters of o-phthalic acid are very dangerous for human health. Their occurrence in wines is connected with the inflow from the plasticized polymer seals, plastic piping, tanks and stoppers. In this study the  high sensitive gas chromatographic-mass spectrometric determination of phthalates in low alcoholic beverages (champagne, red and white wine) coupled ultrasound-assisted emulsification-microextraction was  developed. As extractants environmentally friendly hydrocarbons - n-heptane and hexane are proposed.The sources of possible systematic errors were investigated:   leaking of o-phthalates from chromatographic septum; contamination of phthalate in solvents; influence of macro components of wines(sugar, alcohol,anthocyanins); the hydrolysis of o-phthalates and others. For the first time it is shown that the impact of these factors can lead to an overestimation or underestimation of the actual concentration of impurities by 1-2 orders of magnitude. The methods of accounting or elimination of systematic errors are proposed. Purification of solvents by Rayleigh distillation method allows to obtain samples with impurity content lower than (1-4)∙10^-3mgL^-1. Containers for sampling and storage of samples to be analyzed should be made of borosilicate glass or quartz. The content of o-phthalates in wines was 0.03 - 1 mgL^-1. The largest concentrations are characteristic for diethyl-, di-n-butyl- and di(2-ethylhexyl) о-phthalates.

The limits of detection of esters of о-phthalic acid in low alcohol beverages achieved are at the level of 10^-6–10^-5 mgL^-1 and are highly competitive with the best world results. Therelative expanded uncertainty of the determination of toxicants is at the level of 13- 30%.

Biography:

Xiaolong Fu obtained his Ph. D. in physical chemistry in Institute of Chemistry, Chinese Academy of Sciences in 2015. Then, he joined Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics. He mainly focused on the novel microporous and mesoporous materials and applications in hydrogen isotopes seperations.

Abstract:

Hydrogen isotopes are most likely fuels of future nuclear fusion plants. And fast analysis of hydrogen isotopes is very important. Cryogenic gas chromatograph with capillary column is one of the best methods for analyzing hydrogen isotopes. Recently, significant progress has been made to shorten analysis time and realize on-line analysis by cryogenic gas chromatograph, with promising potential for application. However, due to the same chemical properties and the identical kinetic diameters, separation and quantitative analysis hydrogen isotopes is difficult by using their minute difference.

Herein, we reported a new method in preparation of metal-organic frameworks capillary column via sol-gel process. Metal-organic frameworks thin film was uniformly coated on the inner wall of the capillary column. And the hydrogen isotopes were separated within 1 min.

Biography:

Alicia Gómez López (representative investigator of this research team) has been part of the CNM Mycology Reference Laboratory since 2000. Since her incorporation as a PhD student, has participated in several research projects related to research in human fungal infection.

In 2007 she was in charge of creating a new research line into the Laboratory. This is a line of cutting-edge research in Medical Mycology, which seeks to define relationships between dose and therapeutic response, and also better explain the clinical significance of resistance, by evaluating parameters PK/PD of antifungals and their relationship with efficacy. New strategies using alternative models of infection are now on going in this field with interesting perspectives and applications.

This research is also evaluating the effect of the patient genetic background in treatment efficacy (pharmacogenetic).

This new line is nowadays working actively in the lab. Each year new staff is incorporating to advance in this research by means of competitive applications.

Thanks to these resources new methods have been developed and validated, contributing positivity to assist the national health system in fungal infection management.

Dr Gomez-Lopez has worked in the production of over 79 papers published in scientific journals in the field of mycology and antifungal (2100 times cited, h-index 29), as well as training of fellows, pre-doctoral students, laboratory technicians and other lab management activities.

A total of 50 abstracts have been accepted for poster presentation in national and international Conferences. She has also participated in two Conferences as invited speaker (Expert Sessions). 

As a result of activity of the group a technology-based company was created in 2009, Micología Molecular SL. This is a spin-off Of the ISCIII and its activities are focused in the development of new tools to detect fungal infections.

One patent have been obtained for the diagnosis of mycosis.

Abstract:

Background: The past three decades have seen a considerable expansion in antifungal drug research that led to the clinical development of antifungal agents with different pharmacologic properties. The new antifungal triazoles (fluconazole FCZ, voriconazole VCZ, itraconazole ICZ, posaconazole PCZ and isavuconazole ISvZ) are widely used for the management of invasive fungal infections (IFI). With the exception of fluconazole, these triazoles exhibit significant inter- and intrapatient pharmacokinetic variability and are associated to multiple drug interactions. Thus, unexpected blood concentrations often need to be evaluated in patients treated with them, to prevent treatment failure or toxicity.  A large number of recent studies suggested that the efficacy and tolerance of azoles can be increased through TDM. Measuring blood concentrations of these antifungals and their metabolites could be used for quick identification of patients with impaired metabolism, a suitable strategy to improve effectiveness of this type of treatment. So, to facilitate dosage adjustment, easy, accurate and precise TDM methods need to be routinely used.

Objective: The aim of the study was to describe systemic azoles pharmacokinetic in a collection of clinical samples using a validated HPLC-PDA assay. The method also allows the simultaneous quantification of triazoles and some of their major metabolites (voriconazole N-oxide VCZ N-oxide, and hidroxy-itraconazole OH-ICZ) in the same run.

Method: The proposed method consists in a simple high-pressure liquid chromatography assay using a stepwise gradient elution profile. It enables the simultaneous quantification of systemic azoles in 150μL of serum samples, after a first step of protein precipitation and direct injection of resulting supernatant. The analytical run enables the specific characterization of azoles by its UV profile. For the validation procedure (following international guidelines) linearity, accuracy and precision parameters were determined. We tested this method by monitoring azole serum concentrations in real clinical samples and using external quality controls. An additional description of the rate metabolite/parent drug is also determined to assess the relevance of metabolites on routinely azole TDM.

Results: The selectivity of the chromatographic procedure and PDA detection allowed good resolution. No significant interfering peaks were detected at similar retention times of the tested compounds. The chromatographic assay took 15 minutes per sample; the retention times were found to be: 7.30 ± 0.3, 9.50 ± 0.3, 11.6 ± 0.3, 11.7 ± 0.3, 12.6± 0.3 and 13.4 ± 0.3 minutes for VCZ N-oxide, VCZ, PCZ, OH-ICZ, ISvZ and ICZ, respectively. The validation procedure establishes that the method was linear between concentrations ranging from 0.25 and 16 mg/L for all components (analytical range). The correlation coefficient was higher than 0.9. Regarding the 115 samples received as part of an international quality control program, we found a high correlation between target and calculated concentration. A high percentage of the remaining clinical samples were received to assess VCZ and Noxide-VCZ (46% and 44% respectively). A great variability in concentration was observed among all the samples evaluated. We also found a high percentage of subtherapeutic samples (sbTh, samples in which azole did not reach the established concentration for efficacy). The mean VCZ Metabolic Rate (MR), established as the ratio between VCZ N-oxide /VCZ for each sample was estimated in 1.7-2, ranging between 0.09 and 25. In the case of ICZ, the mean MR was 1.3-2.   No metabolites have been described for PCZ, so no MR was calculated. Significant MR differences were observed between samples. Higher values were found in sbTh samples compared to those for which upTh concentrations were detected.

Conclusions: This method resulted very simple, fast, cheap and very useful for TDM application, to improve clinical management of antifungal therapy in critically ill patients. According to the results described here, we suggest a role of MR on azole TDM.

Biography:

Dr. Mohamed Abd El-Salam Ebiad Ass. Prof. Researcher of physical chemistry at Egyptian petroleum research institute. The last 3 years is a head of Gas chromatography lab, Analysis and Evaluation Department. He has active effort in the demonstrations of central lab for services. He has ~ 20 research article in different physical chemistry research area. He develop many Gas chromatographic applications in the lab such as PVT study, geochemistry, trace analysis for sulfur and inverse gas chromatography. He also participate in three research project using GC-MS. project for biomarker for Suez Gulf region as a data base for Egyptian crude oil, supported by EPRI. STDF project “Finger printing of some Egyptian crude oil via GC-MS in relation to their biomarker”. Gas analyzer MS (HIDDEN) in STDF project "The development of recent catalysts and membrane reactors for dry reforming of natural gas using CO₂".

Abstract:

The distribution of alkylated polycyclic aromatic compounds (PACs) is highly variable in hydrocarbon mixtures. This is because the concentrations are controlled by both the nature of the source organic matter and the conditions of diagenesis/thermal maturation. Different organic matter sources yield bitumens with varying amounts of PACs and different patterns of alkylation. Aromatic fractions separated from seven different Egyptian crude oils, having different geological origins, were analyzed by gas chromatography– mass spectrometry (GC/MS) especially for the generated alkylnaphthalenes and alkylphenanthrenes. Naphthalene (N), Methylnaphthalenes (MN), Dimethylnaphthalenes (DMN), Trimethylnaphthalenes (TMN) and Tetramethylnaphthalenes (TeMN) have been identified in the m/z (128, 142, 156,170 and 184) mass chromatograms. Phenanthrene (P), Methylphenanthrene (MP), dimethylphenanthrene (DMP), and trimethylphenanthrene (TMP) isomers have been identified in the m/z (178, 192, 206 and 220) mass chromatograms. Ratios depending on the differences in the thermal stability of the isomers were applied (eg. MPI, MPr, MNr, DMNr, TMNr2 ..etc.). The ratios of β-substituted to α-substituted isomers of both alkylnaphthalenes and alkylphenanthrenes revealed higher maturity of ND1 from Quassim formation in Nile Delta basin compared to other samples. WD1 oil samples from Faghur basin is characterized by a high abundance of 1,3,7- and 2,3,7-trimethylnaphthalenes (TMN) with (TMNr₂=1.154) and high Pristan/Phytan ratio (Pr/Ph=2.63) compared to WD2 from the same basin suggesting in-reservoir mixing of crude oils of different maturities.