Day 1 :
Keynote Forum
Malik Qaisar Hussain
Director Validation, Pharma Services, Pakistan
Keynote: Applications of core–shell particles in active pharmaceutical ingredients via liquid chromatography
Time : 10:00-10:40
Biography:
Malik Qaisar Hussain has 15 years’ experience in liquid chromatographic method development and validation, has strong scientific, analytical, statistical, managerial and training skills. Currently he is working as a Director validation for Pharma Services. Pharma Services, Pakistan provides services regarding the method development, calibration and validation of liquid chromatographic systems in Pakistan.
Abstract:
High performance liquid chromatography (HPLC) and ultrahigh performance liquid chromatography (UHPLC or UPLC) have been the most widely used tools for research and routine quality control of active pharmaceutical ingredients (API). The most important challenge in these techniques is fast and efficient separation. Both techniques are preferred due to their selectivity, high accuracy and remarkable precision. On the other hand, they have some limitations: In some cases, traditional HPLC uses high amounts of organic solvents with longer analysis time, and furthermore UHPLC has high back pressure and frictional heating. To overcome these limitations, scientists have developed new type of column particles. In general, two different silica types of column packing material based on their backbone have been used for HPLC and UHPLC. Stationary phases that have fully porous silica particles comply with the essential criteria of analysis, but these show all the limitations of HPLC. However, in recent years, core–shell silica particles (a combination of solid core and porous shell) have been increasingly used for highly efficient separation with reduced run times. Thus, core–shell technology provides the same efficient separations as the sub 2 μm particles that are used in UHPLC, while eliminating the disadvantages (potentially lower backpressure). The key factors for core–shell particles are size and thickness of porous shell layer, the latter of which can be explained using the Van Deemter equation. The columns packed with core–shell particles have been employed in a wide range of applications for analysis and quality control of pharmaceutical active substances
Keynote Forum
Malik Qaisar Hussain
Director Validation, Pharma Services, Pakistan
Keynote: Applications of core–shell particles in active pharmaceutical ingredients via liquid chromatography
Biography:
Malik Qaisar Hussain has 15 years’ experience in liquid chromatographic method development and validation, has strong scientific, analytical, statistical, managerial and training skills. Currently he is working as a Director validation for Pharma Services. Pharma Services, Pakistan provides services regarding the method development, calibration and validation of liquid chromatographic systems in Pakistan.
Abstract:
High performance liquid chromatography (HPLC) and ultrahigh performance liquid chromatography (UHPLC or UPLC) have been the most widely used tools for research and routine quality control of active pharmaceutical ingredients (API). The most important challenge in these techniques is fast and efficient separation. Both techniques are preferred due to their selectivity, high accuracy and remarkable precision. On the other hand, they have some limitations: In some cases, traditional HPLC uses high amounts of organic solvents with longer analysis time, and furthermore UHPLC has high back pressure and frictional heating. To overcome these limitations, scientists have developed new type of column particles. In general, two different silica types of column packing material based on their backbone have been used for HPLC and UHPLC. Stationary phases that have fully porous silica particles comply with the essential criteria of analysis, but these show all the limitations of HPLC. However, in recent years, core–shell silica particles (a combination of solid core and porous shell) have been increasingly used for highly efficient separation with reduced run times. Thus, core–shell technology provides the same efficient separations as the sub 2 μm particles that are used in UHPLC, while eliminating the disadvantages (potentially lower backpressure). The key factors for core–shell particles are size and thickness of porous shell layer, the latter of which can be explained using the Van Deemter equation. The columns packed with core–shell particles have been employed in a wide range of applications for analysis and quality control of pharmaceutical active substances.
Keynote Forum
Jenny Zhao
Professor, Lincoln University, New Zealand
Keynote: Micro Extraction and HPLC Quantification of Aucubin, Catalpol and Acteoside in Plantain
Time : 10:40-11:20
Biography:
Jenny Zhao, as a chromatography specialist, works in Lincoln University, New Zealand, her expertise has helped and supported wide range of research projects, which cover agriculture, food, wine and life science research area. In past years, she has established and developed many GC, HPLC, LC-MS methodologies, and published many research papers as a co-author with other scientists.
Â
Abstract:
Aucubin, Catapol and Acteoside (Verbascoside) are secondary metabolites found in plantain and other plants, which have antimicrobial activity and anti-inflammatory function for human and animals. This research had developed a fast and economical micro-extraction method, also developed a reliable HPLC analysis for separation and quantification of Aucubin, Catapol and Acteoside in plantain extract. The newly developed micro-extraction was using 2ml Eppendorf tube, saved a large of amount of organic solvent and time in extraction process, and also easier to handle. The method 1 of HPLC analysis for Aucubin and Catapol were detected at 204nm, and mobile phase contained 98% A and 2% B in isocratic. Sodium dihydrogen phosphate buffer as A, 100% Acetonitrile as B, the research found using buffer in mobile phase A enhanced the retention time stability compared with water as mobile phase A. The method 2 of HPLC analysis for Acteoside was completed by a 10 min isocratic run, mobile phase contained 80% C (5% acetic acid in water) and 20% B (same as above), detection at 330nm. Both separations performed on Agilent 1100 series consisted of quaternary pump and DAD detector, Prodigy column 250mmx4.6mm ODS 5um column (Phenomenex, USA) was used for separation. To complete quantification of three compounds effectively, a sequence set up in Chemstation software switched method 1 to 2 seamlessly, and allowed 30min column reconditioning between two runs by method 2 mobile phase.
Chair
Valentin A.Krylov
Nizhny Novgorod State University,Russia
Session Introduction
Mamta
Kurukshetra University, India
Title: Solvent-free synthesis and characterization of 6-chloro-3-alkyl/aryl/heteroaryl-1,2,4-triazolo[4,3-b]pyridazines
Biography:
My name is Mamta. I am research scholar at Kurukshetra University, Kurukshetra, India, and pursuing research under the kind supervision of Prof. Ranjana aggarwal. My research interest is to synthesize nitrogen containing heterocyclic compounds of biological significance. Compounds which I have synthesized during my Ph.D. evaluated for cytotoxicity and some of the compounds give promising activity.
Abstract:
The 1,2,4-triazole nucleus is an important five-membered heterocyclic scaffold, which is found large number of marketed drugs. Pyridazine ring has been known to be present in several natural products and drugs. A number of synthetic methods have been developed for the synthesis of 1,2,4-triazolo[4,3-b]pyridazine derivatives which involve the oxidation of hydrazones with various reagents such as lead tetraacetate, bromine, nitrobenzene, copper dichloride, mixture of Me4NBr and oxon etc. Unfortunately, most of these methods suffer from various disadvantages such as hazardous materials, poor yield and longer reaction time at higher reaction temperature. Utility of iodobenzene diacetate (IBD) in oxidative transformation is a valuable strategy for greener synthesis because of its easy availability, mild reaction condition and ease of handling. In view of these observations, solvent-free protocol synthesis was developed in the present study for the synthesis of 6-chloro-1,2,4-triazolo[4,3-b]pyridazines using iodobenzene diacetate (IBD) as an eco-friendly agent. Initially, a mixture of 3,6-dichloropyridazine 1 was refluxed with 1 equivalents of hydrazine hydrate in tert-butylalcohol which furnished 6-chloro-3-hydrazinopyridazine 2 after four hour. Further, 1 moles of benzaldehyde was homogenized with 1 equivalent of 2 the reaction mixture was grinded in pestle mortar at room temperature. The reaction was regularly monitored at short intervals by thin layer chromatography (tlc) which indicated the completion of reaction in 20 minutes and a new spot appeared. Then 1.1 equivalents of IBD was added in situ and the reaction mixture was grinded for another 1 hr. Formation of 3 was confirmed on the basis of tlc and spectral data. 1H NMR spectra of compounds 3 displayed pair of doublets for H-4 and H-5 of pyridazine ring at 7.1-8.4 ppm and 7.0-8.1 ppm, respectively with coupling constant 3J= ~ 9.2 Hz.
Athanasia Varvaresou
University of West Attica, Greece
Title: A hydrophilic interaction liquid chromatography method for the quantitation of acetyl hexapeptide-8 in cosmeceuticals.
Biography:
Athanasia Varvaresou is the Director of the Division of Aesthetics and Cosmetic Science of the Department of Biomedical Sciences in University of West Attica, Athens, Greece and Professor in Cosmetic Science. She is graduate from the School of Pharmacy, University of Athens. Her PhD is in synthesis and biological evaluation of xanthene derivatives used in cosmetics. She worked as a post-doctoral research fellow in the University of Athens from 1996 till 2002. She is a reviewer for scientific journals. Her research interests are: Development of anti-aging cosmetics, efficacy tests of cosmetics and synthesis and structure elucidation and analysis of bioactive compounds.
Abstract:
The incorporation of bioactive ingredients in the preparation of cosmetics (referred to as “cosmeceuticals”) is gaining popularity, over the past fifty years, so as to deliver a biologic activity in support of cosmetic claims to provide beneficial topical actions. Cosmeceuticals were made possible by the increased understanding of skin physiology. Peptide cosmeceuticals is a new and popular option to treat aging skin as secondary benefit of research on wound healing as far back as the 1930s, when yeast extracts have been used in medications for their enhancement of wound healing. However, the use of engineered proteins possessing biological activity is novel. There is a real need to set up analytical methods in order to quantitate the active compounds in cosmeceuticals. The aim of this work was on the use of hydrophilic interaction liquid chromatography method for the quantitation of acetyl hexapeptide-8 in cosmetic products. Acetyl hexapeptide-8 mimics the N-terminal end of the SNAP-25 protein. It competes with the natural protein for a position in the SNARE complex, which is essential for muscle contraction. The anti-wrinkle effects of acetyl hexapeptide-8 are similar to those of botulinum neurotoxin. Hydrophilic interaction liquid chromatography (HILIC) combines the characteristics of the 3 major methods in HPLC: reversed phase (RPC), normal phase (NPC) and ion chromatography (IC). The functional group of the Xbridge®-HILIC BEH analytical column used in this work consists of BEH particles containing a sufficient number of accessible silanols on the surface. Chromatographic separation was achieved on a BEH XBridge®-HILIC analytical column with a mobile phase that was composed of a 30% 20mM ammonium formate water solution in acetonitrile and pumped at a flow rate of 0.25 mL min-1. UV detection of acetyl hexapeptide-8 was achieved at 225 nm. Sample preparation was based on dilution of the cosmetic cream into the mobile phase prior to their injection into the HILIC-UV system. The proposed HILIC method has been evaluated over the linearity, precision, accuracy and specificity and proved to be convenient and effective for the determination of acetyl hexapeptide-8 in cosmetic creams.
AntÃa Lestido Cardama
University of Santiago de Compostela, Spain
Title: Identification of potential migrants present in polymeric coatings in food cans
Biography:
Antía Lestido is a PhD student in the Department of Analytical chemistry, Nutrition and Food Science in the Faculty of Pharmacy, University of Santiago de Compostela (Spain). Her studies are based on the estimation of the exposition to different chemical migrants present in food packaging using methodologies based on gas chromatography (GC) and liquid choromatography (LC).
Abstract:
Polymeric coatings are commonly used in metal food cans to protect food from corrosion. However, there is a risk that coatings used in cans release complex chemical mixture into foodstuff including monomers, oligomers, additives, impurities, reaction products, etc. It is important to develop analytical tools for the identification of these potential migrants in the food packaging with the ultimate objective of ensure the consumer safety. A total of twelve food cans that cover several types of food (fish, vegetables, fruit, etc.) were selected as study samples. In a first step, after an extraction with acetonitrile, a non-targeted screening by gas chromatography coupled to mass spectrometry (GC-MS) was performed for migrant identification. Then, in the second part, a targeted analysis was carried out for the simultaneous determination of thirteen compounds including bisphenols (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADEGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionisation (APCI) source. The separation of the analytes was achieved on a Phenosphere 80A ODS (150 * 3.2 mm, 3 µm) column and using a gradient of water and acetonitrile:methanol (50:50) as mobile phase. The screening reveals the presence of a great variety of compounds including plasticizers, photoinitiators, antioxidants, lubricants, etc. The developed method by LC-MS/MS turned out to be an excellent analytical tool for the confirmation of the presence of bisphenol related compounds in the can extracts being cyclo-di-BADGE the predominant compound detected. The study was financially supported by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref.No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE). Antía Lestido is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación Universitaria).
AntÃa Lestido Cardama
University of Santiago de Compostela, Spain
Title: Identification of potential migrants present in polymeric coatings in food cans
Biography:
Antía Lestido is a PhD student in the Department of Analytical chemistry, Nutrition and Food Science in the Faculty of Pharmacy, University of Santiago de Compostela (Spain). Her studies are based on the estimation of the exposition to different chemical migrants present in food packaging using methodologies based on gas chromatography (GC) and liquid choromatography (LC).
Abstract:
Polymeric coatings are commonly used in metal food cans to protect food from corrosion. However, there is a risk that coatings used in cans release complex chemical mixture into foodstuff including monomers, oligomers, additives, impurities, reaction products, etc. It is important to develop analytical tools for the identification of these potential migrants in the food packaging with the ultimate objective of ensure the consumer safety. A total of twelve food cans that cover several types of food (fish, vegetables, fruit, etc.) were selected as study samples. In a first step, after an extraction with acetonitrile, a non-targeted screening by gas chromatography coupled to mass spectrometry (GC-MS) was performed for migrant identification. Then, in the second part, a targeted analysis was carried out for the simultaneous determination of thirteen compounds including bisphenols (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADEGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionisation (APCI) source. The separation of the analytes was achieved on a Phenosphere 80A ODS (150 * 3.2 mm, 3 µm) column and using a gradient of water and acetonitrile:methanol (50:50) as mobile phase. The screening reveals the presence of a great variety of compounds including plasticizers, photoinitiators, antioxidants, lubricants, etc. The developed method by LC-MS/MS turned out to be an excellent analytical tool for the confirmation of the presence of bisphenol related compounds in the can extracts being cyclo-di-BADGE the predominant compound detected. The study was financially supported by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref.No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE). Antía Lestido is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación Universitaria).
AntÃa Lestido Cardama
University of Santiago de Compostela, Spain
Title: Identification of potential migrants present in polymeric coatings in food cans
Biography:
Antía Lestido is a PhD student in the Department of Analytical chemistry, Nutrition and Food Science in the Faculty of Pharmacy, University of Santiago de Compostela (Spain). Her studies are based on the estimation of the exposition to different chemical migrants present in food packaging using methodologies based on gas chromatography (GC) and liquid choromatography (LC).
Abstract:
Polymeric coatings are commonly used in metal food cans to protect food from corrosion. However, there is a risk that coatings used in cans release complex chemical mixture into foodstuff including monomers, oligomers, additives, impurities, reaction products, etc. It is important to develop analytical tools for the identification of these potential migrants in the food packaging with the ultimate objective of ensure the consumer safety. A total of twelve food cans that cover several types of food (fish, vegetables, fruit, etc.) were selected as study samples. In a first step, after an extraction with acetonitrile, a non-targeted screening by gas chromatography coupled to mass spectrometry (GC-MS) was performed for migrant identification. Then, in the second part, a targeted analysis was carried out for the simultaneous determination of thirteen compounds including bisphenols (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADEGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionisation (APCI) source. The separation of the analytes was achieved on a Phenosphere 80A ODS (150 * 3.2 mm, 3 µm) column and using a gradient of water and acetonitrile:methanol (50:50) as mobile phase. The screening reveals the presence of a great variety of compounds including plasticizers, photoinitiators, antioxidants, lubricants, etc. The developed method by LC-MS/MS turned out to be an excellent analytical tool for the confirmation of the presence of bisphenol related compounds in the can extracts being cyclo-di-BADGE the predominant compound detected. The study was financially supported by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref.No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE). Antía Lestido is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación Universitaria).
AntÃa Lestido Cardama
University of Santiago de Compostela, Spain
Title: Identification of potential migrants present in polymeric coatings in food cans
Biography:
Antía Lestido is a PhD student in the Department of Analytical chemistry, Nutrition and Food Science in the Faculty of Pharmacy, University of Santiago de Compostela (Spain). Her studies are based on the estimation of the exposition to different chemical migrants present in food packaging using methodologies based on gas chromatography (GC) and liquid choromatography (LC).
Abstract:
Polymeric coatings are commonly used in metal food cans to protect food from corrosion. However, there is a risk that coatings used in cans release complex chemical mixture into foodstuff including monomers, oligomers, additives, impurities, reaction products, etc. It is important to develop analytical tools for the identification of these potential migrants in the food packaging with the ultimate objective of ensure the consumer safety. A total of twelve food cans that cover several types of food (fish, vegetables, fruit, etc.) were selected as study samples. In a first step, after an extraction with acetonitrile, a non-targeted screening by gas chromatography coupled to mass spectrometry (GC-MS) was performed for migrant identification. Then, in the second part, a targeted analysis was carried out for the simultaneous determination of thirteen compounds including bisphenols (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADEGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionisation (APCI) source. The separation of the analytes was achieved on a Phenosphere 80A ODS (150 * 3.2 mm, 3 µm) column and using a gradient of water and acetonitrile:methanol (50:50) as mobile phase. The screening reveals the presence of a great variety of compounds including plasticizers, photoinitiators, antioxidants, lubricants, etc. The developed method by LC-MS/MS turned out to be an excellent analytical tool for the confirmation of the presence of bisphenol related compounds in the can extracts being cyclo-di-BADGE the predominant compound detected. The study was financially supported by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref.No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE). Antía Lestido is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación Universitaria).
AntÃa Lestido Cardama
University of Santiago de Compostela, Spain
Title: Identification of potential migrants present in polymeric coatings in food cans
Biography:
Antía Lestido is a PhD student in the Department of Analytical chemistry, Nutrition and Food Science in the Faculty of Pharmacy, University of Santiago de Compostela (Spain). Her studies are based on the estimation of the exposition to different chemical migrants present in food packaging using methodologies based on gas chromatography (GC) and liquid choromatography (LC).
Abstract:
Polymeric coatings are commonly used in metal food cans to protect food from corrosion. However, there is a risk that coatings used in cans release complex chemical mixture into foodstuff including monomers, oligomers, additives, impurities, reaction products, etc. It is important to develop analytical tools for the identification of these potential migrants in the food packaging with the ultimate objective of ensure the consumer safety. A total of twelve food cans that cover several types of food (fish, vegetables, fruit, etc.) were selected as study samples. In a first step, after an extraction with acetonitrile, a non-targeted screening by gas chromatography coupled to mass spectrometry (GC-MS) was performed for migrant identification. Then, in the second part, a targeted analysis was carried out for the simultaneous determination of thirteen compounds including bisphenols (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADEGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionisation (APCI) source. The separation of the analytes was achieved on a Phenosphere 80A ODS (150 * 3.2 mm, 3 µm) column and using a gradient of water and acetonitrile:methanol (50:50) as mobile phase. The screening reveals the presence of a great variety of compounds including plasticizers, photoinitiators, antioxidants, lubricants, etc. The developed method by LC-MS/MS turned out to be an excellent analytical tool for the confirmation of the presence of bisphenol related compounds in the can extracts being cyclo-di-BADGE the predominant compound detected. The study was financially supported by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref.No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE). Antía Lestido is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación Universitaria).
Patricia Vázquez Loureiro
University of Santiago de Compostela, Spain
Title: Identification of unknown compounds in PE and PP for food contact materials
Biography:
Patricia Vázquez Loureiro is a PhD Student in the Department of Analytical Chemistry, Nutrition and Food Science in the University of Santiago de Compostela. Her works are focus on packaging materials and food safety and she has experience in the analysis of compounds of interest in food products as well as in method developments or different extraction sample procedures. She has worked with both liquid and gas chromatography coupled to mass spectrometry (LC-MS/MS and GC- MS) and liquid chromatography with fluorescence detector to identify and quantify compounds of interest.
Abstract:
Packaging materials are complex mixtures and can contain unknown compounds due to unexpected reactions or degradation of substances present in the materials used for their manufacture. Polyethylene (PE) and polypropylene (PP) are polymers widely used for packaging applications, which may undergo changes during their manufacture. One of the challenges in the food packaging field is the identification of unknown compounds present in the final material and that could be originated during its processing. In the present work a non-targeted analysis for the identification of unknown compounds was applied. Different PE and PP were analyzed. Samples consisted of raw materials as well as the additives used in its manufacture. Each sample was analyzed by gas chromatography coupled to mass spectrometry (GC-MS) after solvent extraction to detect semi-volatile compounds and GC-MS coupled to Purge and Trap (GC-MS-P&T) in case of volatile compounds. To be analyzed by GC-MS, samples were previously extracted with hexane at 70ºC for 4 hours and with a mixture of Hexane: Ethanol (3:1 v/v) at 20ºC for 8 hours. Likewise, each sample was directly subjected to a slight heating (Purge) during which the volatiles present were dynamically dragged through a stream of Helium being retained in a trap. Subsequently the trap was subjected to rapid heating and the retained compounds were eluted to the chromatograph where they were analyzed. The presence of alkanes as more abundant components was confirmed by both techniques, as well as the presence of 2,4-di-tertbutylphenol as can be seen in Figure 1. This compound is a product of degradation of the antioxidants used in the processing of this material.
The study was financially supported by the “Ministerio de Economía y Competitividad”, "Fondo Europeo de Desarrollo Regional (FEDER) and by "Agencia Estatal de Investigación" ref. RTC-2017-6553-2. “NAPA” (MINECO/FEDER, UE)
SEEMA GARG
SPC Govt. College, India
Title: COST EFFECTIVE IVORY PAPER CHROMATOGRAPHY TECHNIQUE FOR QUALITATIVE ANALYSIS OF CHEMICAL SUBSTANCES
Biography:
Dr. Seema Garg is an Associate Professor in the Department of Chemistry, at Samrat Prithviraj Chauhan Government College, Ajmer, Rajasthan, India. She completed her PhD in Pharmaceutical Chemistry in 1993 from Gujarat University, India. She has a teaching experience of 22 years. In 2019, she was conferred with the honorary Excellence in Teaching award from her Institute. Dr. Garg has her expertise in pyrimidine synthesis and drug design. She recently patented her research titled “A process for preparation of herbal gelatine” which has wide ranging industrial applications and may prove to be pathbreaking in gelatine synthesis.
Abstract:
The technique of chromatography has undergone tremendous amount of modifications since its discovery. Almost any kind of a given chemical sample can now be separated using this technique. Paper chromatography is one of the widely utilized physiochemical separation method for both, inorganic and organic substances. Traditionally, Paper chromatography technique involved the use of upmarket filter papers of various types, deployed according to the need of the chemist. The focus of my current research is to demonstrate how a sheet of Ivory paper can be utilized for performing paper chromatography. Ivory paper has conventionally found its use in Charcoal and water colour paintings, but its use in chromatography largely remains unexplored. Ivory paper is known for its evenness and fineness of its grains. Ivory is very dense; its pores are close and compact. Ivory sheets of various thicknesses are easily available in the market at very low costs. The Absence of any coating on an Ivory sheet results in faster movement of solvent from the starting line and therefore helps in attaining an expeditious equilibrium and sharper separation of the solute from the solvent.
Moreover, it has better defined bands, better and faster staining efficiency, higher sensitivity and better handling (due to stronger sheets). Furthermore, the availability of Ivory sheets in varied thicknesses even makes it a good candidate for conducting quantitative analysis as well as paper electrophoresis.
Osarumwense Peter Osarodion
Ondo State University of Sciences and Technology, Nigeria.
Title: Anti-Inflammatory activity Of newly synthesized 7-chloro-2-methyl-4H-benzo [d] [1,3]-oxazin-4-one and 3-amino-7-chloro-2-methyl-quinazolin-4(3H)-one
Biography:
Abstract:
Introduction: Heterocyclic chemistry comprises at least half of all organic chemistry research worldwide in particular, heterocyclic structures form the basis of many pharmaceutical, agrochemical and veterinary products.
Methods: The condensation of Methyl-2-amino-4-Chlorobenzoate with acetic anhydride yielded the cyclic compound 2-methyl 7-Chloro-1, 3-benzo-oxazine-4-one (1) which further produce 3-Amino-2-Methyl 7-Chloro quinazolin-4(3H)-ones (2) via the reaction with hydrazine hydrate. The compounds synthesized were unequivocally confirmed by means of Infrared, Nuclear Magnetic Resonance (1H and 13C), Gas Chromatography-Mass spectrophotometry and Elemental analysis.
Results: Compound 1 and 2 has Anti-inflammatory activity of 96.78%, 95.71% and 97.62%, 95.35% at 10mg/kg and 20mg/Kg dose levels.
Discussion: Compound 1 has IR spectrum showed signals for carbonyl functional group at 1662 cm-1, C-O and C-H stretch vibrations at 1102 cm-1 and 2871 cm-1respectively. The 1H NMR spectrum showed three aromatic protons at δH 7.59, 7.16 and 6.40 and a vinyl methyl protons at δH 2.57..In the 13C NMR spectrum, the ester carbonyl resonated at δC 168.08, while the aromatic carbons resonated in the range δC 113.40 – 149.23. The resonances at δC 153.13 and δC 22.15 were due to the imine oxygenated carbon (C-1) and the methyl carbon respectively. Compound 2, had NMR data similar to1, except for an additional signal at δH 5.80 in the 1H NMR spectrum which was attributed to the amino protons (2H).
Conclusion: Compound 2 had a higher anti-inflammatory activity than Compound 1. The compounds synthesized had a higher anti-inflammatory activity than Indomethacin, a standard anti-inflammatory drug.
Xueqin Liu
Jiangsu ocean university, China
Title: Purification and characterization of Antioxidant Peptides from Shrimp Enzymatic Hydrolysis Products
Biography:
Liu Xueqin, Jiangsu Ocean University, Lianyungang City, Jiangsu Province, is a graduate student in the Key Laboratory of Marine Bioresources and Environment of Jiangsu Province. Under the guidance of the instructor, research on the activity of marine food microbial and microbial metabolites has been devoted for several years.
Abstract:
Marine biological antioxidant peptides have become a hotpots in multidisciplinary research such as modern biomedicine. In this study, the lyophilized powder of shrimp paste was used as raw material, and the protease produced by the protease-producing strain isolated from the shrimp paste raw material was hydrolyze. A total of 10g Shrimp powder was dissolved in 50 mL distilled water and the pH of the solution was adjusted to 6.0 using 1M HCl. Then, ST-1protease was added at a ratio of enzyme to substrate. The mixture was incubated at 50 ℃ with shaking. After 6 h incubation, the mixture was heated at 100 ℃ for 15 min to inactivate the ST-1protease. Alcohol precipitation: The solution was cooled to 40 ℃ and rota-evaporated to remove water. Anhydrous ethanol was then added and the solution was settled for 12 h. The solution was centrifuged at 8000 rpm for 15 min and the supernatant was dried under vacuum to obtain shrimp paste peptides (SPs), which was then separated and purified by a gel column G-25. The results of the antioxidant activity test showed that the component three exhibited high antioxidant activity; the component three was collected and separated by reverse high phase liquid phase (RP-HPLC) to obtain four components. The isolated antioxidant peptide exhibits high DPPH scavenging activity, relatively good hydroxide radical and superoxide anion scavenging activity. Antioxidant peptides have broad prospects for development in medical, cosmetic, cosmetic and food applications.
Dr L.Hetemi
Institute of biochemistry Skopje, north macedonia.
Title: Diabet type ll related with anemia
Biography:
She started working in Olive medical Laboratory and now she is currently working as a Resident Doctor in Biochemistry Institute Skopje, North Macedonia.
Abstract:
Introduction: The purpose of this study was to: follow-up patients with type II diabetes through testing of: glycated hemoglobin (HbA1c) derivatives, but the importance of the HPLC method during HbA1c testing in: diagnosis, monitoring, follow-up, access to type II diabetes therapy also obtained results from: diabetes mellitus, diabetes, patient insulin insertion, monotherapy, but also findings of abnormal HgB forms in diabetic patients, such as hemoglobinopathies, and during the research we found that the diagnostic orientation through a HbA1c test with HPLC is in some pathology, which was both preventive and diagnostic in other pathologies.
The research lasted over 1 year at the Olive medical & laboratory diagnostic center. Keis group pharmaceutical Kosovo.For the first time in our country we performed HbA1c with HPLC. The G8 HPLC system based on the principle of high performance liquid chromatography (HPLC), the G8 analyser uses a cation exchange column to separate haemoglobin components by their ionic charges. The various components of haemoglobin, are quickly separated into 6 fractions and assayed during a 1.6 minute cycle. The absorbance of the different haemoglobin components, separated in the column, is monitored by the detector. When the assay is completed, results for these haemoglobin fractions are printed as percentages together with the chromatogram.
The study was conducted on 150 patients, of which 80% were type ll diabetes, age 40-65 years, with HbA1c ranging from 6.9-11%, HbA from 6-8, HbF of over 1 % -8% (in 48% of cases was HbF positive), the control group was non-diabetic, suspect, dyslipidemia patients with no signs of type II diabetes, the reason for testing being because they had high insulin resistance, or moderate , some were cases of polycystic ovary syndrome etc, their age ranged from 40-65 years. In addition to the absolute accuracy of the HPLC method in testing HbA1c, in this study we found HbF positive of patients with type II diabetes, which is leading us to anemia, and the cause of this anemia is thought to be impairment of renal function, such as diabetic nephropathy - complication of type II diabetes, but a still unclear mechanism between abnormal HbF congenital and type II diabetes will to remain uninvolved as we were not able to test all the patients for Hb electrophoresis.
From these laboratory findings, HbF results in increased pathology: in addition to being an innate congenital form, its elevated level was also found in cases of pernicious anemia, hemolytic, thalassemia, thyrotoxicosis, venous thrombosis. LA1c as the labile form of glycated Hb,could be increase in case of presence of carbamylated Hb (urea, patients with kidney diseases) and acetylated Hb (alcohol abuses, liver diseases, etc), of course increase of blood sugar glucose. When blood glucose levels are high,glucose molecules attached to RBC,the longer hyperglycemia occurs,more the glucose binds to Hb,and higher the glycated Hb. So from this study we found approximately 35% of cases with LA1c positive, where diabetic nephropathy had already begun, which was confirmed by positive microalbuminuria, and consultations with patients with nephrologist. Abnormal forms of HbF lead in our country, and in these 150 cases there were no other abnormal forms of HbF, we conclude with the facts that HPLC can freely be called the gold standard diagnostic method, as it has proven to be the best method. Risk for pre-diabetic, where 20% of our patients, with HbA1c values between 6-6.4%, about 10% of our patients where with HbA1c values more than:6.5%,tested for the first time, that consider diabetic, about 25% where with adecuate control:with 6.6-7% values, and inadecuate control according ADA(Ameriacn Diabetic association criteria’s) with 7-8% values of HbA1c,about 45% of them.
Dr L.Hetemi
Institute of biochemistry Skopje, north macedonia.
Title: Diabet type ll related with anemia
Biography:
She started working in Olive medical Laboratory and now she is currently working as a Resident Doctor in Biochemistry Institute Skopje, North Macedonia.
Abstract:
Introduction: The purpose of this study was to: follow-up patients with type II diabetes through testing of: glycated hemoglobin (HbA1c) derivatives, but the importance of the HPLC method during HbA1c testing in: diagnosis, monitoring, follow-up, access to type II diabetes therapy also obtained results from: diabetes mellitus, diabetes, patient insulin insertion, monotherapy, but also findings of abnormal HgB forms in diabetic patients, such as hemoglobinopathies, and during the research we found that the diagnostic orientation through a HbA1c test with HPLC is in some pathology, which was both preventive and diagnostic in other pathologies.
The research lasted over 1 year at the Olive medical & laboratory diagnostic center. Keis group pharmaceutical Kosovo.For the first time in our country we performed HbA1c with HPLC. The G8 HPLC system based on the principle of high performance liquid chromatography (HPLC), the G8 analyser uses a cation exchange column to separate haemoglobin components by their ionic charges. The various components of haemoglobin, are quickly separated into 6 fractions and assayed during a 1.6 minute cycle. The absorbance of the different haemoglobin components, separated in the column, is monitored by the detector. When the assay is completed, results for these haemoglobin fractions are printed as percentages together with the chromatogram.
The study was conducted on 150 patients, of which 80% were type ll diabetes, age 40-65 years, with HbA1c ranging from 6.9-11%, HbA from 6-8, HbF of over 1 % -8% (in 48% of cases was HbF positive), the control group was non-diabetic, suspect, dyslipidemia patients with no signs of type II diabetes, the reason for testing being because they had high insulin resistance, or moderate , some were cases of polycystic ovary syndrome etc, their age ranged from 40-65 years. In addition to the absolute accuracy of the HPLC method in testing HbA1c, in this study we found HbF positive of patients with type II diabetes, which is leading us to anemia, and the cause of this anemia is thought to be impairment of renal function, such as diabetic nephropathy - complication of type II diabetes, but a still unclear mechanism between abnormal HbF congenital and type II diabetes will to remain uninvolved as we were not able to test all the patients for Hb electrophoresis.
From these laboratory findings, HbF results in increased pathology: in addition to being an innate congenital form, its elevated level was also found in cases of pernicious anemia, hemolytic, thalassemia, thyrotoxicosis, venous thrombosis. LA1c as the labile form of glycated Hb,could be increase in case of presence of carbamylated Hb (urea, patients with kidney diseases) and acetylated Hb (alcohol abuses, liver diseases, etc), of course increase of blood sugar glucose. When blood glucose levels are high,glucose molecules attached to RBC,the longer hyperglycemia occurs,more the glucose binds to Hb,and higher the glycated Hb. So from this study we found approximately 35% of cases with LA1c positive, where diabetic nephropathy had already begun, which was confirmed by positive microalbuminuria, and consultations with patients with nephrologist. Abnormal forms of HbF lead in our country, and in these 150 cases there were no other abnormal forms of HbF, we conclude with the facts that HPLC can freely be called the gold standard diagnostic method, as it has proven to be the best method. Risk for pre-diabetic, where 20% of our patients, with HbA1c values between 6-6.4%, about 10% of our patients where with HbA1c values more than:6.5%,tested for the first time, that consider diabetic, about 25% where with adecuate control:with 6.6-7% values, and inadecuate control according ADA(Ameriacn Diabetic association criteria’s) with 7-8% values of HbA1c,about 45% of them.
Dr L.Hetemi
Institute of biochemistry Skopje, north macedonia.
Title: Diabet type ll related with anemia
Biography:
She started working in Olive medical Laboratory and now she is currently working as a Resident Doctor in Biochemistry Institute Skopje, North Macedonia.
Abstract:
Introduction: The purpose of this study was to: follow-up patients with type II diabetes through testing of: glycated hemoglobin (HbA1c) derivatives, but the importance of the HPLC method during HbA1c testing in: diagnosis, monitoring, follow-up, access to type II diabetes therapy also obtained results from: diabetes mellitus, diabetes, patient insulin insertion, monotherapy, but also findings of abnormal HgB forms in diabetic patients, such as hemoglobinopathies, and during the research we found that the diagnostic orientation through a HbA1c test with HPLC is in some pathology, which was both preventive and diagnostic in other pathologies.
The research lasted over 1 year at the Olive medical & laboratory diagnostic center. Keis group pharmaceutical Kosovo.For the first time in our country we performed HbA1c with HPLC. The G8 HPLC system based on the principle of high performance liquid chromatography (HPLC), the G8 analyser uses a cation exchange column to separate haemoglobin components by their ionic charges. The various components of haemoglobin, are quickly separated into 6 fractions and assayed during a 1.6 minute cycle. The absorbance of the different haemoglobin components, separated in the column, is monitored by the detector. When the assay is completed, results for these haemoglobin fractions are printed as percentages together with the chromatogram.
The study was conducted on 150 patients, of which 80% were type ll diabetes, age 40-65 years, with HbA1c ranging from 6.9-11%, HbA from 6-8, HbF of over 1 % -8% (in 48% of cases was HbF positive), the control group was non-diabetic, suspect, dyslipidemia patients with no signs of type II diabetes, the reason for testing being because they had high insulin resistance, or moderate , some were cases of polycystic ovary syndrome etc, their age ranged from 40-65 years. In addition to the absolute accuracy of the HPLC method in testing HbA1c, in this study we found HbF positive of patients with type II diabetes, which is leading us to anemia, and the cause of this anemia is thought to be impairment of renal function, such as diabetic nephropathy - complication of type II diabetes, but a still unclear mechanism between abnormal HbF congenital and type II diabetes will to remain uninvolved as we were not able to test all the patients for Hb electrophoresis.
From these laboratory findings, HbF results in increased pathology: in addition to being an innate congenital form, its elevated level was also found in cases of pernicious anemia, hemolytic, thalassemia, thyrotoxicosis, venous thrombosis. LA1c as the labile form of glycated Hb,could be increase in case of presence of carbamylated Hb (urea, patients with kidney diseases) and acetylated Hb (alcohol abuses, liver diseases, etc), of course increase of blood sugar glucose. When blood glucose levels are high,glucose molecules attached to RBC,the longer hyperglycemia occurs,more the glucose binds to Hb,and higher the glycated Hb. So from this study we found approximately 35% of cases with LA1c positive, where diabetic nephropathy had already begun, which was confirmed by positive microalbuminuria, and consultations with patients with nephrologist. Abnormal forms of HbF lead in our country, and in these 150 cases there were no other abnormal forms of HbF, we conclude with the facts that HPLC can freely be called the gold standard diagnostic method, as it has proven to be the best method. Risk for pre-diabetic, where 20% of our patients, with HbA1c values between 6-6.4%, about 10% of our patients where with HbA1c values more than:6.5%,tested for the first time, that consider diabetic, about 25% where with adecuate control:with 6.6-7% values, and inadecuate control according ADA(Ameriacn Diabetic association criteria’s) with 7-8% values of HbA1c,about 45% of them.
Nabat Abdullayeva
Sumgait State University, Azerbaijan
Title: Chromatographic analysis of chloranilines in aqueous environments
Biography:
I am Nabat Abdullayeva.I s a graduate student. The title of the dissertation is "Gasochromatographic determination of pre-bromination of aniline and its chlorine derivatives in water".I am doing research on sampling wastewater from paints and pharmaceutical plants operating in Azerbaijan.
Abstract:
Statement of the Problem: Aniline and its chlorine derivatives of industrial importance are widely used in textile, cosmetics, medicines, food, paper, and plastic. Aniline, which is included in the dye class, mixes with pure water in the wastewater, and first of all, pollutes the water and changes its color. In addition to visual contamination it absorbs sun rays prevents the water depth by absorbing or reflecting sunlight. This prevents various microorganisms from developing and prevents photosynthesis of aquatic plants. As a result, there is a change in the composition of natural water, and the amount of oxygen is significantly reduced. Methodology & Theoretical Orientation: For these reasons, different methods have been proposed to etermine the aniline and chloraniline dervatives in water. The gasochromatographic methods for the determination of micro chloranilines in water were studied. Findings: Chromatographic properties of chloranilines. Chemical modifications of chloranilines and evaluation of their effectiveness. Conclusion & Significance: As a result of this study, quantitative analysis of aniline and its chlorine derivatives may be prepared in water. In this way, the aniline prevents the spread of aniline and its effects on mutagenic and carcinogenic substances such as chlorine derivatives.
Dr L.Hetemi
Institute of biochemistry Skopje, north macedonia.
Title: Diabet type ll related with anemia
Biography:
She started working in Olive medical Laboratory and now she is currently working as a Resident Doctor in Biochemistry Institute Skopje, North Macedonia.
Abstract:
Introduction: The purpose of this study was to: follow-up patients with type II diabetes through testing of: glycated hemoglobin (HbA1c) derivatives, but the importance of the HPLC method during HbA1c testing in: diagnosis, monitoring, follow-up, access to type II diabetes therapy also obtained results from: diabetes mellitus, diabetes, patient insulin insertion, monotherapy, but also findings of abnormal HgB forms in diabetic patients, such as hemoglobinopathies, and during the research we found that the diagnostic orientation through a HbA1c test with HPLC is in some pathology, which was both preventive and diagnostic in other pathologies.
The research lasted over 1 year at the Olive medical & laboratory diagnostic center. Keis group pharmaceutical Kosovo.For the first time in our country we performed HbA1c with HPLC. The G8 HPLC system based on the principle of high performance liquid chromatography (HPLC), the G8 analyser uses a cation exchange column to separate haemoglobin components by their ionic charges. The various components of haemoglobin, are quickly separated into 6 fractions and assayed during a 1.6 minute cycle. The absorbance of the different haemoglobin components, separated in the column, is monitored by the detector. When the assay is completed, results for these haemoglobin fractions are printed as percentages together with the chromatogram.
The study was conducted on 150 patients, of which 80% were type ll diabetes, age 40-65 years, with HbA1c ranging from 6.9-11%, HbA from 6-8, HbF of over 1 % -8% (in 48% of cases was HbF positive), the control group was non-diabetic, suspect, dyslipidemia patients with no signs of type II diabetes, the reason for testing being because they had high insulin resistance, or moderate , some were cases of polycystic ovary syndrome etc, their age ranged from 40-65 years. In addition to the absolute accuracy of the HPLC method in testing HbA1c, in this study we found HbF positive of patients with type II diabetes, which is leading us to anemia, and the cause of this anemia is thought to be impairment of renal function, such as diabetic nephropathy - complication of type II diabetes, but a still unclear mechanism between abnormal HbF congenital and type II diabetes will to remain uninvolved as we were not able to test all the patients for Hb electrophoresis.
From these laboratory findings, HbF results in increased pathology: in addition to being an innate congenital form, its elevated level was also found in cases of pernicious anemia, hemolytic, thalassemia, thyrotoxicosis, venous thrombosis. LA1c as the labile form of glycated Hb,could be increase in case of presence of carbamylated Hb (urea, patients with kidney diseases) and acetylated Hb (alcohol abuses, liver diseases, etc), of course increase of blood sugar glucose. When blood glucose levels are high,glucose molecules attached to RBC,the longer hyperglycemia occurs,more the glucose binds to Hb,and higher the glycated Hb. So from this study we found approximately 35% of cases with LA1c positive, where diabetic nephropathy had already begun, which was confirmed by positive microalbuminuria, and consultations with patients with nephrologist. Abnormal forms of HbF lead in our country, and in these 150 cases there were no other abnormal forms of HbF, we conclude with the facts that HPLC can freely be called the gold standard diagnostic method, as it has proven to be the best method. Risk for pre-diabetic, where 20% of our patients, with HbA1c values between 6-6.4%, about 10% of our patients where with HbA1c values more than:6.5%,tested for the first time, that consider diabetic, about 25% where with adecuate control:with 6.6-7% values, and inadecuate control according ADA(Ameriacn Diabetic association criteria’s) with 7-8% values of HbA1c,about 45% of them.
Letricia Barbosa-Pereira
University of Santiago de Compostela, Spain.
Title: Phenolic profile of several fruit industry byproducts determined by HPLC-DAD-MS/MS
Biography:
Letricia Barbosa-Pereira is a Postdoctoral researcher at the Department of Analytical Chemistry Nutrition and Food Science of the Faculty of Pharmacy of the University of Santiago de Compostela. Her expertise is focused in new approaches for the recovery, characterization and application of plant- based bioactive compounds as food ingredients/additives, development of new healthier food products using low-cost functional ingredients, development of functional foods with health benefits to provide the consumers healthy food choices and find new applications of bioactive in the health sector as nutraceuticals.
Abstract:
Fruit sector produces large amounts of wastes during juice extraction by pressing. These by-products are an important source of high amounts of dietary polyphenols recognized by their antioxidant properties and so their potential health benefits. Therefore, the bioconversion of fruit by-products into new functional and clean label ingredients/additives represents a sustainable approach with great potential of application for food, pharmaceutical and cosmetic sectors.
The aim of this work was the exhaustive characterization of different extracts yielded from three fruit by-products by the identification and quantification of the polyphenols using liquid chromatography.
Ethanolic extracts yielded from apple, lemon and orange by-products containing polyphenols were analyzed by liquid chromatography coupled to mass spectrometry (LC-MS/MS) operated in negative ESI (Electrospray System Ionization) mode. Separation was performed on a Kinetex® EVO C18 100 Å (150 x 3mm, 5µm size of particle) column using water and acetonitrile acidified with 0.1% formic acid as mobile phase. High resolution liquid chromatography with diode detector (HPLC-DAD) was used for the quantification of the main phenolic compounds.
More than 30 compounds were tentatively identified with different distribution among the extracts. Orange by-product was that with high number of polyphenols, while lemon extract was that with high concentrations of these molecules. The main compounds present in orange by-product were Naringenin-7-O-rutinoside, Hesperetin-7-O-rutinoside, Isosakuranetin-7-O-rutinoside. Lemon extract was characterized by the presence of Naringenin-7-O-rutinoside, Eriodyctiol-O-rutinoside, Hesperetin-7-O-rutinoside. On the other hand, apple by-product showed a different phenolic profile (e.g. Phlorizin, Naringenin-7-O-glucoside and Rosmarinic acid) compared to the citric extracts and also in lower concentrations. The results highlight that the origin of the extract affects its composition and therefore the characterization of these profiles is mandatory for food application. These fruits by-products may be a low-cost source of polyphenols that can be used as food ingredients/additives minimizing their environmental impact.
Biography:
Deanna Mulvihill has her expertise in evaluation and passion in improving the health and wellbeing. Her open and contextual evaluation model based on responsive constructivists creates new pathways for improving health care. She has built this model after years of experience inresearch, evaluation, teaching and administration both in hospital and education institutions. The foundation is based on fourth generation evaluation (Guba& Lincoln, 1989) which is a methodology that utilizes the previous generations of evaluation: measurement, description and judgment. It allows for value-pluralism. This approach is responsive to all stakeholders and has a different way offocusing.
Abstract:
Polycyclic aromatic hydrocarbons are priority pollutants due to the very high toxicity. Therefore, to determine them, it is necessary to use sensitive methods with preconcentration. In the present study, a novel method named electroflotation-assisted deemulsification liquid–liquid microextraction combined with GC-MS analysis has been proposed for the preconcentration and determination of polycyclic aromatic hydrocarbons in water samples. The advantage of electroflotation deemulsification is the ease of changing the gas flow and size of gas micro-bubbles. The formation of gas micro-bubbles occurs on platinum electrodes soldered into a glass concentrator. Hexane, toluene and o-xylene were used as extractants. Application of extract capillary collection have solved the problem of the light extractant sampling. Dispersion of the extractant was performed by ultrasound. The volume of microextract was 7-10 µl. The recovery of polycyclic aromatic hydrocarbons from water was 62-95%. A DB-5 (5% phenyl + 95% polydimethylsiloxane) fused-silica capillary column (30 m ×0.25 mm i.d. and 0.25-µm film thickness)was applied for separation of the analytes. The limits of detection and quantification of polycyclic aromatic hydrocarbons achieved were at the level of 10-5–10-6 mgL-1 and highly competitive with the best world results. 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)∙10-3 mgL-1. Containers for sampling and storage of samples to be analyzed should be made of borosilicate glass or quartz. The expanded uncertainty was calculated. It included precision, uncertainty of standards preparation, calibration, sample introduction, enrichment factor. The relative expanded uncertainty was at the level of 13-30%.
Muhammad Jehangir
Senior Manager Quality Control Novamed Group, Pakistan
Title: Pharmaceutical impurity analysis of raw materials and final product by using analytical techniques
Biography:
Muhammad Jehangir has 13 years diversified experience of Quality Control, Quality Assurance, Registration Affairs, Product development and Pharmaceutical manufacturing, Process Planning, Method development, Method validation, Statistical Methodology, Process & Cleaning Validation, and Equipment Validation. Certificate Courses on cGMP, cGLP, Process Validation, CTD Documents, ISO 9001:2015, 13485-2016, and 14001-2004, has strong scientific, analytical, statistical, managerial and training skills. Currently he is working as a Senior Manager Quality Control and validation for Novamed Pharmaceuticals. It is toll manufacturing oriented company, manufacturing of companies like Getz Pharma, ICI, SEARLE, Macter, Ray, and for Sanofi-Aventis. He is also looking after the Quality of Novamed Healthcare, the nutraceutical and cosmeceutical manufacturing plant.
Abstract:
The evaluation of pharmaceutical raw materials and finished products for impurities and degradation products is an essential part of the drug development and manufacturing testing process. Additionally, toxicological information must be obtained on any drug-related impurity that is present at a concentration of greater than 0.1% of that of the active pharmaceutical ingredient (API). In pharmaceutical QC and manufacturing, impurity analysis has traditionally been performed by HPLC with UV, PDA, or MS detection. As it is essential to detect and measure all of the impurities in the sample, it is necessary to have a high resolution separation process. This usually involves long analysis times resulting in low throughput. As candidate pharmaceutical compounds become more potent and are dosed at lower and lower levels, ever more sensitive assays are needed to detect and measure impurities. The low throughput of HPLC can become the rate-limiting step in product release testing or process evaluation. Since much of the process of impurity identification involves the coupling of LC to sophisticated MS, any reduction in analysis time will result in a more efficient use of these significant investments. Analytical technology advances such as UPLC and UPC offer significant improvements in throughput and sensitivity, with benefits to the process of product release and identification of drug-related impurities. The most characteristic feature of the development in the methodology of pharmaceutical and biomedical analysis during the past 25 years is that HPLC became undoubtedly the most important analytical method for identification and quantification of drugs, either in their active pharmaceutical ingredient or in their formulations during the process of their discovery, development and manufacturing.
Suhair M. S. Jambi
University of Jeddad, Saudi Arubia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..
Suhair M. S. Jambi
University of Jeddah, Saudi Arabia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..
Suhair M. S. Jambi
University of Jeddah, Saudi Arabia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..
Suhair M. S. Jambi
University of Jeddah, Saudi Arabia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..
Suhair M. S. Jambi
University of Jeddad, Saudi Arubia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..
Suhair M. S. Jambi
University of Jeddah, Saudi Arabia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..
Suhair M. S. Jambi
University of Jeddah, Saudi Arabia
Title: Structural of Pd(II) and Pt(II) complexes of N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea by mass and infrared spectroscopy
Biography:
Suhair Mansour Jambi, has completed her PhD at 2011 from King Abdulaziz university in Saudi Arabia in Jeddah. She is interested in modern technologies in the field of metallic complexes, the structure of metal complexes using modern methods, thiourea complexes and their use in the treatment of some microbes and some diseases such as cancer. She had published more than 13 papers in a reputed journal such as Z.Kristallogr.NCS, journal of Molecular Liquids, journal of Molecular Structure, journal of Sulfur Chemistry. Now she is work at the university of Jeddah..
Abstract:
An efficient synthesis of ligand N-phenyl-N′-(4′-methylthiazol-2′-yl)-thiourea via the reaction of 2-amino-4-methylthiazol and Phenylisothiocyanate under mild conditions has been developed. This reaction proceeded well at room temperature, to products in excellent yields for a wide range of substrate. The corresponding complexes of these ligand were synthesized by the reaction of the ligand with Pd(II), Pt(II) at molar ratio of 1:2. The structures of compiexes were identified by physic-chemical and spectroscopic techniqes (IR, Mass spectrometry). IR spectrum of the ligand displays two bands at 3340 cm-1 and 3165cm-1, attributable to υ(N1–H), υ(N2-H), respectively. The IR spectra of the complexes showed stretching frequency for the N2H group and the disappearance of the band of N1H. The disappearance or absence of the strong band at 650cm-1 in the free ligandis a strong evidence for the coordination of the nitrogen atoms of the thiazole ring in the metal complexes. The mass spectrum of the PdL2 complex revealed the highest peak at m/z = 602 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pd-106 isotope. The mass spectrum of the [PtL2ClH2O] complex revealed the highest two peak with low intensity at m/z = 692 and 693, based on atomic weight of Pt-195 and Pt-196, respectively, among the isotope cluster peaks assigned to a molecular ion of the complex. The mass spectrum of the [PtL12].4H2O complex revealed the highest peak at m/z = 691 corresponds to the molecular weight of the parent cationic species [M]+. This assign mentis based on the atomic weight of Pt-165 isotope among the isotope cluster peaks assigned to a molecular ion of the complex. This corresponds to the molecular weight of the non-aqueous cationic complexPtL2â”+..