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HPLC Method Development and Validation for Determination of Active Substances and Impurity in Valetol Preparation
Maroušková, Alena ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
This work extends the graduation thesis which found optimal chromatographic conditions for a separation of paracetamol, caffeine and propyphenazon, and the impurity p-aminophenol in the pharmaceutical preparation Valetol by HPLC method. At first, the benzoic acid was found as a suitable internal standard for the quantification. Next, the analytical method validation was carried out, including the suitability test of the chromatographic system. Within the suitability test of the chromatographic system the following attributes were tested: column efficiency expressed as a number of theoretic plates N assymetry of chromatographic peaks expressed as factor T resolution of chromatographic peaks reproducibility expressed as a relative standard error Within the analytic method validation were tested: precision linearity accuracy selectivity robustness stability The robustness test confirmed the analysis sensitivity to the change in the character of the mobil phase. As a part of the robustness test two parameters of mobile phase were tested: pH and triethylamine concentration changes. It was confirmed that the change of pH of the mobile phase influences mostly the retention times of p-aminophenol and benzoic acid. The change of triethylamine amount in the mobile phase influences mostly...
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Novel stationary phases in HPLC for the analysis of biologically active compounds - determination of vitamine E
Plíšek, Jiří ; Solich, Petr (advisor) ; Šatínský, Dalibor (referee)
Bc. Jiří Plíšek, 2008 Application of technology new stationary phases in HPLC analysis of biologically active compounds - determination of vitamin E (Abstract) The aim of my graduation thesis was to find the acceptable stationary phase for pretreatment of biological material [blood plasma] and isolation of vitamin E (α-tocopherol) by SPE technique and subsequent determination by HPLC analysis by using the developed method. LLE was then altered by SPE. I used vitamin A (retinol) as standard for my own work, because there is a possibility that the simultaneous determination of both vitamins for the laboratory GMK FN HK will be an advantageous combination. The main emphasis was put on vitamin E. Sample preparation - optimized SPE procedure: Blood samples were drawn from the peripheral vein after twelve hours of overnight fast. The samples were then centrifuged (1600×g, 10 min, 4řC) and plasma was separated. Then 250 μl of plasma was added and deproteinized by absolute ethanol (625 μl, 10 min, 4řC). After centrifugation (1600×g, 15 min, 4řC), the supernatant was separated and applied on the SPE column. Before application of the sample, the SPE column was activated by 1 ml methanol and then washed by 1 ml of purified water. After application of the sample the precipitate was diluted in 625 μl of absolute...
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Application of nanofibrous sorbents for on-line extraction in liquid chromatography
Háková, Martina ; Šatínský, Dalibor (advisor) ; Česla, Petr (referee) ; Urban, Jiří (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Háková Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: doc. PharmDr. Lucie Chocholoušová Havlíková, Ph.D. Title of Doctoral Thesis: Application of nanofibrous sorbents for on-line extraction in liquid chromatography A compilation of ten publications is presented in this dissertation thesis. It is focused on the application of nano and microfibrous polymers as a new extracting material in analytical chemistry. This work was based on close cooperation with the Institute for Nanomaterials, Advanced Technologies and Innovation and the Department of Nonwovens and Nanofibrous Materials at the Technical University of Liberec, where the author took part in designing and preparation of these materials. The first part deals with model studies, based on using polyamide, polystyrene and polycaprolactone nanofibers as sorbents for solid phase extraction in classical off-line mode or in on-line column switching system. It solves practical aspects such as orientation and the formation of the fibers in the extraction system, optimization of fabrication factors affecting applicability of the nanomaterials, suitable solvent systems, stability testing and reusability of the microcolumns. The...
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Effect of flow rate on the kinetic and the possibility of evaluating different reactions in the SIA system
Mrákotová, Vladěna ; Sklenářová, Hana (advisor) ; Šatínský, Dalibor (referee)
2 ABSTRACT Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of analytical chemistry Candidate: Vladěna Mrákotová Supervisor: Doc. PharmDr. Hana Sklenářová, Ph.D. Title of diploma thesis: Effect of flow rate on the kinetic and the possibility of evaluating different reactions in the SIA system The diploma thesis dealt with testing the effect of mixing and flow rate on the kinetic and the possibility of evaluating different reactions in the SIA system with spectrophotometric detection. Absorbance was measured for two kinds of chemical reactions with different reaction speed. For faster running reaction color change of bromothymol blue (BTB) with sodium hydroxide (NaOH) by the change in pH was evaluated by the increase in absorbance of blue form/decrease in absorbance of yellow form of BTB. The effect of flow rate and method of mixing (different sequence aspirations, different mixing ratio of working solution) was tested. The same parameters were also tested for slowly running two-step reaction of nitrites (D) with a diazo-coupling reagent (DKC). Furthermore, stop-flow technique was applied to see the effect of stopping the flow at certain parts of the flow system. The "sandwich" technique was tested too. The obtained results were evaluated using peak heights and peak areas. In...
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Optimization of neonicotinoids extraction using nanofibers in sequential injection analysis systém
Zouharová, Monika ; Horstkotte Šrámková, Ivana (advisor) ; Šatínský, Dalibor (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Monika Zouharová Supervisor: PharmDr. Ivana Horstkotte Šrámková, Ph.D. Title: Optimization of neonicotinoids extraction using nanofibers in sequential injection analysis system In this diploma thesis, we tested the use of various nanofibers as sorbents for solid phase extraction of neonicotinoids connected with sequential injection analysis system. Seven types of nanofibers were tested, specifically polyamide (PA6), polycaprolactone (PCL), polyimide (PID) and polydopamine coated polyamide (PA6)coated, polycaprolactone (PCL)coated, polyimide (PID)coated and a combination of polyimide and polycaprolactone (PID/PCL)coated. These nanofibers were produced by electrospinning. The studied nanofibers were placed in the 3D printed holder, which was connected into sequential injection analysis system. UV spectrophotometry was used as a detection method. The substances to analyse were neonicotinoid insectisides. The retention of these analytes was examinated with all seven types of nanofibers. Retention of the analytes on the tested nanofibers depending on their chemical structures and physical-chemical properties was studied in these measurements. The most experiments were performed with polydopamine coated...
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Modification of nanofibres for extraction in liquid chromatography
Valachovič, Adam ; Šatínský, Dalibor (advisor) ; Chocholouš, Petr (referee)
Department: Department of Analytical Chemistry Candidate: Adam Valachovič Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Modification of nanofibers for extraction in liquid chromatography The diploma thesis demonstrates the influence of modifications of polymer nanofibers on their extraction properties for extraction in liquid chromatography. Nanofibers represent a potential sorbent for extraction methods due to their large surface area, which leads to increased capacity of extraction. Another advantage of nanofibers is the possibility to modify their surface resulting in various nanofibers with different extraction properties. In this thesis, the modifications were performed by coating polypropylene nanofibers with a polydopamine layer. The polymerization solution was pumped through a column, in which the nanofibers were placed, using a peristaltic pump connected to the column by a system of tubes. An on-line SPE HPLC method was developed to determine the extraction properties of the modified nanofibers. Chlorogenic acid was chosen as the model analyte, because its extraction is affected by the polydopamine layer. The key parameters of the coating process were optimized, including the weight of the nanofibers, the concentration of dopamine in the polymerization...
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Nano-fibers as a modern extraction sorbents for extraction of samples in chromatographic analysis
Raabová, Hedvika ; Šatínský, Dalibor (advisor) ; Ševčík, Juraj (referee) ; Ventura, Karel (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Training workplace Department of Analytical Chemistry Doctoral degree program Pharmaceutical Analysis Candidate Mgr. Hedvika Raabová Supervisor prof. RNDr. Dalibor Šatínský, Ph.D. Advisor assoc. prof. PharmDr. Lucie Chocholoušová Havlíková, Ph. D. Title of Doctoral Thesis Nanofibers as modern extraction sorbents for sample extraction in chromatographic analysis Extraction techniques represent one of the most common approaches to sample handling. The analytes of interest can be isolated easily even from complex matrices, especially by solid-phase extraction (SPE). Therefore, this technique became very popular and routinely used in laboratories. The variety of commercially available sorbents has made this method even more attractive. Nevertheless, the new sorbent materials are still looked for because of the broadening spectrum of analyzed substances and the increasing demands on selectivity and extraction efficiency. Nanomaterials have been increasingly associated with these properties over the last ten years. Therefore, they are receiving more and more attention related to extraction procedures. The dissertation thesis is focused on the application of nanofibrous polymers as innovative sorbents for solid-phase extraction. First, the...
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HPLC method development and validation for analysis of anthocyanins content in black currant cultivars
Bobríková, Michaela ; Šatínský, Dalibor (advisor) ; Matysová, Ludmila (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical chemistry Candidate: Michaela Bobríková Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: Mgr. Barbora Šmídová Title of diploma thesis: HPLC method development and validation for analysis of anthocyanins content in black currant cultivars. A high performance liquid chromatography method with diode array detection was used and validated to determine delphinidin-3-glucoside, delphinidin-3-rutinoside, cyanidin-3-glucoside and cyanidin-3-rutinoside in black currant cultivars and black currant juices. The method used gradient elution with methanol and 2 % formic acid. Supelco Analytical, Ascentis Express C18 column with particle size 2.7 µm, 15 cm x 4.6 mm was used for separation. The analysis was performed using a temperature 50řC and a flow rate 0.8 ml/min. For detection, the wavelength of 520 nm was chosen.
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