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Development and validation of UHPLC-MS/MS method for determination of maraviroc in placental perfusion
Čapková Maxová, Eliška ; Nováková, Lucie (advisor) ; Kočová Vlčková, Hana (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of analytical chemistry Candidate: Eliška Čapková Maxová Supervisor: Assoc. Prof. PharmDr. Lucie Nováková, Ph.D. Title of Thesis: Development and validation of UHPLC-MS/MS method for the determination of maraviroc in placental perfusions The goal of this work was to develop fast and selective method for the determination of maraviroc in human placental perfusions. The ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) was used. BEH C18 column and gradient elution with the mobile phase A (water with 0.1% formic acid) and B (acetonitrile) at 0.35 mL/min flow-rate and 40 řC temperature were used for the separation. The mass spectrometry conditions were optimist and set up as follows: electrospray ionization in positive mode, capillary voltage 1.0 kV, cone voltage 35 V, extractor 3.0 V, RF lens 0.1 V, desolvatation gas flow 1000 L/h, temperature 450 žC, cone gas flow 100 l/h, ion source temperature 130 žC. Selected reaction monitoring (SRM) mode was used for quantitation. Liquid-liquid extraction (LLE) was chosen for sample preparation and was optimised. The best results were obtained when dichloromethane was used as the extraction agent (recovery >90%). The optimized method was fully validated in...
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Impacts of Selected Changes in Accounting Legislation on Reporting and Comparison of Data
NOVÁKOVÁ, Lucie
The thesis deals with the evaluation of changes in accounting legislation in relation to the informative ability of accounting. In particular, these changes are: - Canceling Reporting Item Separation Reporting alone - Changes in accounting for provisions - Accounting for activation and inventory of own activity - Categorization of entities and related obligations - Cancellation of extraordinary costs and revenues - Amendment to the regulations governing the auditor's audit of financial statements - Canceling the separate reporting of the Trade Margin item As the Czech Republic is a part of the European Union, it is impossible to ignore the effort to unify repor-ting, which is intended to improve the readability of financial statements for users from other countries. The work includes an evaluation of changes from the perspective of various authors and the professional public. Selected statements are verified on selected businesses. The ongoing small legislative adjustments do not fully meet the needs of current businesses, the concept of the new form of accounting, which is currently presented to the professional public for discussion, indicates the future direction of Czech ac-counting. An equally important part of the thesis is the analysis of the questionnaire, which seeks to gain the opinion of the professional public on the issue.
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Elizabeth Bishop: The Map of Her Life and Work
Nováková, Lucie ; Veselá, Pavla (advisor) ; Quinn, Justin (referee)
The aim of the thesis is straightforward: to provide readers with a glimpse into the life of Elizabeth Bishop but not to put emphasis on biographical details. The focus lies on her two most formative relationships with her fellow poets, namely Marianne Moore and Robert Lowell. The thesis aims to present five selected poems and to read them with acknowledging the mutual influences and, at the same time, it strives to provide specific instances of such influences. The first part of the thesis is dedicated to the relationship with Marianne Moore. The two poets met during Bishop's Vassar years and their friendship lasted until Moore's death in 1972. From the teacher - mentored paradigm, their friendship evolved into an affectionate companionship. The thesis introduces their relationship while using selected letters, interviews and, to illustrate the matters more clearly, two of Bishop's poems, "The Roosters" and "Invitation to Miss Marianne Moore." The first poem captures the breaking free from Moore's direct influence and additionally serves as a link to the second part of the thesis. The later poem is used to illustrate their reconciliation and to present the milestone that marks the shift of paradigms. The second part of the thesis presents Robert Lowell, who is the already mentioned link between...
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Evaluation of separation potential of stationary phases based on porous graphitic carbon
Guláš, Ondrej ; Nováková, Lucie (advisor) ; Šatínský, Dalibor (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Ondrej Guláš Supervisor: Assoc. Prof. PharmDr. Lucie Nováková, Ph.D. Title of Diploma Thesis: Evaluation of separation potential of stationary phases based on porous graphitic carbon. Stationary phases based on porous graphitic carbon (PGC) exhibit many interesting features. For example high mechanical resistance, stability across the entire pH range and excellent high temperature resistance. Moreover, they are significant due to their unique mechanism of retention. Despite all of these positive features and long existence on the market, their broader use in pharmaceutical analysis is still lacking. In our paper we have analyzed 11 groups of drugs, including active pharmaceutical ingredient and its potential impurities. Overall, 67 substances have been analyzed. Each separation on PGC has been optimized in order to achieve the best results. Changes in conditions of separation included testing of several mobile phases, gradient and isocratic elution and testing the effect of higher temperature. The use of gradient elution, with mobile phase consisting of acetonitrile and isopropanol in proportion 1:1 as organic modifier and 0,1% trifluoracetic acid as aqueous part has appeared as the most...
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Development of UHPLC method for separation of eight structurally related derivatives of vitamin E
Pružinská, Klára ; Nováková, Lucie (advisor) ; Pilařová, Veronika (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of analytical chemistry Candidate: Klára Pružinská Supervisor: Assoc. prof. PharmDr. Lucie Nováková, Ph.D. Title od the diploma thesis: Development of UHPLC method for separation of eight structurally related derivatives of vitamin E The aim of this diploma thesis was to develop UHLPC method for the separation of eight derivates of vitamin E. They include a group of tocopherols and tocotrienols. To achieve the aim ultra-high performance liquid chromatography was used. In process of optimalization the most important thing was the choice of stationary phase, consistence of mobile phase, flow speed, temperature of column and the time of separation. The Ascentis Express F5 Column (100 x 3.0 mm, 2.7 μm), Sigma-Aldrich was the best stationary phase because the separation of all eight derivatives on this column including two problematic pairs: β-T3 with γ-T3 and the pair β-T with γ-T was performed. The mobile phase was a mixture of a methanol with acetonitrile (1:1) and water in the ratio 75:25 with a flow rate 1 ml/min, isocratic elution and PDA and FLR detection. In PDA detection the wavelength was set 290 nm. In more sensitive FLR detection the emission wavelenght was 325 nm and the exciting wavelength of exciting was set on 280 nm....
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Influence of sample preparation method on occurence of matrix effects in UHPSFC-MS analysis of vitamin E
Vasilisková, Lucia ; Nováková, Lucie (advisor) ; Pilařová, Veronika (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Lucia Vasilisková Supervisor: doc. PharmDr. Lucie Nováková, Ph.D. Title of Diploma Thesis: Influence of sample preparation method on occurence of matrix effects in UHPSFC-MS analysis of vitamin E The goal of this thesis was to optimize the chromatographic method for the determination of 8 different isomers of vitamin E that would provide better analysis results than two existing methods; high speed (HS) and high resolution (HR). New Torus stationary phases (SP) were tested (diethylamine, 1-aminoantracene, 2-picolylamine and diol under conditions: CO2:MeOH 98:2, flow rate 2 ml/min, injection volume 2 µl, column temperature 40řC, BPR 12.9 MPa, make-up solvent 0.1% NH4OH in MeOH. The modifiers (ethanol, isopropanol and a 1:1 mixture of acetonitrile/methanol) were tested on the 2-PIC column. The effect of additives in the mobile phase was also compared (0.1% NH4OH, 10mM ammonium formate, 10mM ammonium acetate and 2% H2O). The next part of the thesis describes the development of the sample preparation method to reduce or eliminate the matrix effects. Dilution method was tested using solvents - H2O, 50% acetonitrile (ACN) and 75% ACN. Urine samples were 10, 20, 50 and 100 times diluted by the most...
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Matrix effects in LC-MS analysis: occurrence, evaluation, and their elimination
Svoboda, Pavel ; Nováková, Lucie (advisor) ; Švec, František (referee) ; Havliš, Jan (referee)
Abstract Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Pavel Svoboda Supervisor: Assoc. Prof. PharmDr. Lucie Nováková, Ph.D. Advisor: RNDr. Hana Vlčková, Ph.D. Title of Doctoral Thesis: Matrix effects in LC-MS analysis: occurrence, evaluation, and their elimination The dissertation thesis deals with the issue of matrix effects in analysis using liquid chromatography coupled to mass spectrometry (LC-MS). LC-MS represents a well-established, widely used, and powerful tool in the field of qualitative and quantitative analysis of a wide range of different compounds. Despite all the advantages offered by LC-MS such as sensitivity, selectivity, and robustness, it suffers from a major drawback represented by matrix effects. This undesirable phenomenon affects important parameters of LC-MS method such as accuracy, precision, linearity, limit of detection, and limit of quantification. Therefore, an evaluation of these effects should be involved in validation of every single LC-MS method and their source should be eliminated. The assessment is generally performed by qualitative and quantitative approaches such as post-extraction addition, post-column infusion, and comparison of slopes of calibration curves. The matrix effects can be reduced or...
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Development and optimization of sample preparation step for fast chromatographic analysis
Pilařová, Veronika ; Nováková, Lucie (advisor) ; Bednář, Petr (referee) ; Šatínský, Dalibor (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of analytical chemistry Candidate Mgr. Veronika Pilařová Supervisor Assoc. Prof. Lucie Nováková, Ph.D. Title of Doctoral Thesis Development and optimization of sample preparation step for fast chromatographic analysis. The aim of the dissertation thesis is the development of modern extraction methods for the sample purification and for the analytes isolation and preconcentration from various biological materials, including biological fluids (plasma, serum, vaginal lavages) and plant material. Modern approaches have a lots of advantages such as a lower consumption of sample and organic solvents, extraction speed-up, better sample purification, matrix removal and lower influence of matrix effects. Extracts from modern microextraction methods can be analyzed by separation methods including ultra-high performance liquid chromatography and supercritical flluid chromatography coupled with mass spectrometry. The separation methods enable fast high-throughput analysis with sensitive and selective detection. Individual projects show the possibilty of use of the modern approaches in the sample preparation field, where the microextraction by packed sorbent (MEPS), microextraction by solid phase extraction in pipette tips...
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