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Employment of gas chromatography in the field of drug analysis III.
Šináklová, Barbora ; Kučera, Radim (advisor) ; Vrbatová, Ivana (referee)
Diploma thesis Employment of gas chromatography in the field of drug analysis III. Barbora Šináklová Charles Univerzity in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control The gas chromatography represents a sensitive analytic method. Effective and fast separation of complicated compounds and manipulation with small amounts of samples using a relatively simple equipment characterise the GC method in particular. Butan-1,3-diol is a substance used in chemical industry as a solvent and a carrier of aromatic substances, or for plastics and explosives production. It is added to antifreeze mixtures in radiatores. Another usage possibility constitute cosmetic products, the substance also occurs in pesticides. Because of its antimicrobial effects, butan-1,3-diol is added to cleansing articles. It extends the effect of certain syringe articles and increases the effect of dissolved effective substances. This method was used in this diploma thesis to determine the volume of butan-1,3-diol and the method was validated. The work was realized with gas chromatograph Shimadzu GC-2010 with flame- ionization detector. Hydrogen was chosen as the carrier gas. Supelcowax TM-10, Fused silica capillary column, 30 m × 0,53 mm × 0,5 µm was used. The inner standard...
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Identification of related compounds by GC-MS
Kušnír, Jaroslav ; Kučera, Radim (advisor) ; Vrbatová, Ivana (referee)
Identification of Related Substances Using GC-MS Thesis Jaroslav Kušnír Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control A molecular weight was researched for the purpose of identifying three foreign matters, which were found in 1,3-butanediol substance during GC/FID. GC/MS technique was used for researching molecular weight. Following techniques were used to ionize the samples - electron ionization, chemical ionization using methane and isobutene reagent gases. To acquire a more stable molecular ion, different derivative reactions were tried as for example acylation. Nevertheless result were not satisfiable. Chemical ionization using isobutene reagent gas was found to be the most effective for researching molecular weight of the foreign matters. Isobutene is more sensitive reagent gas than methane and therefore a more intensive ion (M+H)+ can be found in the mass spectrum, from which it is possible to define molecular weight. Apart from researching molecular foreign matters, the best conditions for using reagent gas isobutene in GC/MS were examined. From the measuring it was found that the best conditions are during 80 kPa pressure and increased voltage by 0.4 kV from the default setting of the detector. Molecular weight of...
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The employment of HPLC in chiral separation II.
Bartošová, Martina ; Kučera, Radim (advisor) ; Vrbatová, Ivana (referee)
Employment of HPLC in chiral separation II. Diploma thesis Martina Bartošová Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Heyrovského 1203, Hradec Králové. The need to obtain enantiomerically pure substance increases due to the permanent growing demands on quality, efficiency and safety of drugs. The importance of chiral separations, which are necessary in the area of drug production as well as drug analysis, raises as a consenquence of this trend. There are several methods, which are capable of chiral separations. The most favourable are chromatographic methods, where the high performance liquid chromatography (HPLC) occupies the leading position. This method is being constatntly developed. High efficiency and fast separation of enantiomers are the main driving forces. The main demands are stable chiral stationary phases (CSP), which are able to achieve baseline enantiomeric separation in the shortest time as possible. The chiral stationary phases have to prove high selectivity, efficiency and mechanic resistance. This phenomenon leads to the continual search for new options in the area of CSPs. New alternatives have been in chiral selectors, which are responsible for the nature of chiral separations, and also in...
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Analysis of selected polar compounds in HILIC mode
Brychová, Anna ; Kovaříková, Petra (advisor) ; Vrbatová, Ivana (referee)
Nowadays High Pressure Liquid Chromatography is the most important and the most frequently used separation technique that enables qualitative and quantitative analysis of the complex mixtures. One of its variants is Hydrophilic Interaction Liquid Chromatography. Lately this technique has experienced an increasing boom particularly, due to its ability to improve separation of very polar and hydrophilic compounds. The adeninribonucleotides (ATP, ADP, AMP, cAMP), creatine and phosphoceratine are among these highly polar compounds that are of great importance not only for human body. Number of analytical methods has been developed and published for the analysis of these compounds; however HPLC methods using the reverse phases have been dominated. The basic overview of these methods is a part of this diploma thesis. The experimental part of this thesis is focused on the development of chromatographic conditions suitable for the simultaneous analysis of ATP, ADP, AMP, cAMP, creatine and phosphocreatine in HILIC mode. The best separation was achieved on ZIC®-HILIC (150 x 2,1 mm; 3,5 μm; 200 Å) column using a binary mobile phase and gradient elution. The mobile phase consisted of the A component, (2 mM ammonium formate, pH 6,45) and the B component (90% of acetonitrile, 2 mM ammonioum formate) that were...
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The employment of separation methods in the field of drug analysis IV.
Ondrišíková, Lucie ; Kučera, Radim (advisor) ; Vrbatová, Ivana (referee)
Employment of separation methods in the field of drug analysis IV. Diploma thesis Lucie Ondrišíková Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové Nowadays, high performance liquid chromatography is one of the most progressive analytical methods, which is widely used in all areas of drug analysis. Currently, the majority of analysis is done using silica columns. Despite the positive properties (e.g. available in the widest selection of particle size, pore diameter and surface area; wide selection of types of reversed phases) these columns have some limitations - e.g. there are stable only at pH = 2.0 to 8.0 and the temperature must be lower than 60řC. For these reasons new materials for stationary phases are being developed and tested. Zirconia seems to be very perspective; it is stable at any pH and temperatures up to 200řC. The theoretical part of this thesis deals with both the physical and chemical properties of zirconia from a chromatographic point of view. This part describes characteristics of HPLC zirconia columns in comparison to silica columns as well. The experimental part focuses on studying and comparing the retention behavior of neutral, acid and alkaline substances on Zr-...
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Bioanalytical method development for the investigation of the role of pyridoxal isonicotinoyl hydrazone in isoniazid intoxication II.
Charvátová, Jana ; Vrbatová, Ivana (advisor) ; Pilařová, Pavla (referee)
Diploma thesis Abstract 52 Abstract Bioanalytical method development for the investigation of role of pyridoxal isonicotinoyl hydrazone in isoniazid intoxication II. Jana Charvátová Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Heyrovského 1203, 500 05 Hradec Králové Keywords: isoniazid, vitamin B6, hydrazone, hydrophilic interaction chromatography HPLC/UV method was developed for analysis of isoniazid - INH, its main (acetylisoniazid - AcINH) and putative metabolites (pyridoxal isonicotinoyl hydrazone - PIH, pyridoxal isonikotinoyl hydrazone 5-phosphate - PIH5P), vitamins B6 (pyridoxine - PN, pyridoxal - PL and pyridoxal 5-phosphate - PLP) using ZIC-pHILIC stationary phase. The following parameters were modified to assess their impact on the retention of these compounds: composition of mobile phase, percentage content of organic solvent, buffer concentration, pH, flow rate of mobile phase and column temperature. The best available separation of the compounds was achieved using 10mM ammonium formate (pH 3) and ACN (40:60, v/v), flow rate 0.10 ml/min and column temperature 25 řC. Developed method was transferred to HPLC/ESI/MS. Experiments revealed that all analytes gave the higher signal in positive mode and the most abundant ions...
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HPLC analysis of the clinically used drug - dexrazoxane
Pecuchová, Vladimíra ; Kovaříková, Petra (advisor) ; Vrbatová, Ivana (referee)
1. ABSTRACT High performance liquid chromatography (HPLC) is a progressive analytic method which belongs among the most frequently used separation techniques. Iron is an irreplaceable biogenous element, which is involved in many important biochemical processes in human body. However, under specific pathophysiological conditions its severe effects may occur. Anthracycline cytostatics belong to the frequently used drugs for the treatment of various hematologic malignity and solid tumors. Their most important toxic effect is cardiotoxicity. Anthracyclines are able to form complexes with iron that are very redox active. They produce by the cyclic mechanism the high amount of cytotoxic hydroxyl radicals. This mechanism is believed together with own redox ability of anthracyclines molecule to be responsible for the drugs cardiotoxicity. Dexrazoxane, bisdioxopiperazine derivative, is the only clinically used drug for the treatment of anthracycline induced cardiotoxicity. It is supposed, that dexrazoxane is bioactivated inside the cardiomyocytes to active metabolite - ADR-925. Iron chelating ability of ADR-925 is believed to be responsible for the cardioprotective effect of dexrazoxane. This work is aimed at development of the optimal mass spectrometry compatible chromatographic conditions for the separation of...
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Bioanalytical method development for the investigation of the role of pyridoxal isonicotinoyl hydrazone in isoniazid intoxication II.
Charvátová, Jana ; Vrbatová, Ivana (advisor) ; Pilařová, Pavla (referee)
Diploma thesis Abstract 52 Abstract Bioanalytical method development for the investigation of role of pyridoxal isonicotinoyl hydrazone in isoniazid intoxication II. Jana Charvátová Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Heyrovského 1203, 500 05 Hradec Králové Keywords: isoniazid, vitamin B6, hydrazone, hydrophilic interaction chromatography HPLC/UV method was developed for analysis of isoniazid - INH, its main (acetylisoniazid - AcINH) and putative metabolites (pyridoxal isonicotinoyl hydrazone - PIH, pyridoxal isonikotinoyl hydrazone 5-phosphate - PIH5P), vitamins B6 (pyridoxine - PN, pyridoxal - PL and pyridoxal 5-phosphate - PLP) using ZIC-pHILIC stationary phase. The following parameters were modified to assess their impact on the retention of these compounds: composition of mobile phase, percentage content of organic solvent, buffer concentration, pH, flow rate of mobile phase and column temperature. The best available separation of the compounds was achieved using 10mM ammonium formate (pH 3) and ACN (40:60, v/v), flow rate 0.10 ml/min and column temperature 25 řC. Developed method was transferred to HPLC/ESI/MS. Experiments revealed that all analytes gave the higher signal in positive mode and the most abundant ions...
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The employment of HPLC in chiral separation II.
Bartošová, Martina ; Kučera, Radim (advisor) ; Vrbatová, Ivana (referee)
Employment of HPLC in chiral separation II. Diploma thesis Martina Bartošová Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Heyrovského 1203, Hradec Králové. The need to obtain enantiomerically pure substance increases due to the permanent growing demands on quality, efficiency and safety of drugs. The importance of chiral separations, which are necessary in the area of drug production as well as drug analysis, raises as a consenquence of this trend. There are several methods, which are capable of chiral separations. The most favourable are chromatographic methods, where the high performance liquid chromatography (HPLC) occupies the leading position. This method is being constatntly developed. High efficiency and fast separation of enantiomers are the main driving forces. The main demands are stable chiral stationary phases (CSP), which are able to achieve baseline enantiomeric separation in the shortest time as possible. The chiral stationary phases have to prove high selectivity, efficiency and mechanic resistance. This phenomenon leads to the continual search for new options in the area of CSPs. New alternatives have been in chiral selectors, which are responsible for the nature of chiral separations, and also in...
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