|
|
Monitoring of liberation tests.
Beran, Marek ; Sklenářová, Hana (advisor) ; Matysová, Ludmila (referee)
Charles University Faculty of Pharmacy in Hradci Králové Department of Analytical Chemistry Candidate: Marek Beran Supervisor: Doc. PharmDr. Hana Sklenářová, Ph.D. Consultant: Ing. Daniela Šmejkalová, Ph.D Title of Diploma Thesis: Monitoring of liberation tests The diploma thesis is focused on the development of an automated method for the monitoring of the dissolution profile of clotrimazole from topical dosage forms. The dissolution profile of formulations containing the antifungal agent clotrimazole are compared. Commercially available formulations Canesten and Clotrimazol AL in the form of creams, are compared with a new formulation called Delcore from Contipro a.s., which contains a complex matrix. Theoretical part addresses mycotic infections with focus on superficial mycoses and products available on the Czech market for the treatment of those infections. Furthermore, there is a description of selected non-separation flow methods. The analysis was carried out in a sequential injection analysis system coupled with three attached Franz dissolution cells with a membrane on which the sample was applied. The Franz cells were placed in a water bath at 32 řC. Phosphate buffer with pH 7.4 was chosen as the dissolution medium as it partially imitates the conditions of the human environment. Detection...
|
|
|
Development of UHPLC method for determination of salicylic acid, methylsalicylate and ethylsalicylate in pharmaceutical formulations
Kosáčková, Nikola ; Matysová, Ludmila (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Nikola Kosáčková Supervisor: doc. PharmDr. Ludmila Matysová, Ph.D. Title of diploma thesis: Development of UHPLC method for determination of salicylic acid, methylsalicylate and ethylsalicylate in pharmaceutical formulations New chromatografic method for determination of salicylic acid, methylsalicylate and ethylsalicylate by using ultra-high performance liquid chromatography was developed. Analysis was carried out using the Kinetex® 1.7 µm XB-C18 100 Å, 50 x 2.1 mm column. The mobile phase was composed of aqueous solution of 1% acetic acid (pH 2.6) and methanol, and the flow rate was 0.4 ml/min. Separation was achieved using gradient elutions. An UV detector at the wavelength of 240 nm was used. Propylparaben was chosen as the internal standard. The total analysis time did not exceed 7 minutes. This method was used for the determination of releasing of salicylic acid and methylsalicylate from matrices consisting of polyester of D,L-lactic acid, glycolic acid and 8% dipentaerythritol (8D) and their dissolution media, which have been prepared at the Department of Pharmaceutical Technology at the FaF UK. Key words: Ultra-High Performance Liquid Chromatography, salicylic acid, methylsalicylate,...
|
|
|
Development and validation of UHPLC method for determination of miconazole, econazole and its impurities in solid dispersions
Arnoltová, Kristýna ; Matysová, Ludmila (advisor) ; Kujovská Krčmová, Lenka (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Kristýna Arnoltová Supervisor: doc. PharmDr. Ludmila Matysová, Ph.D. Title of the diploma thesis: Development and validation of UHPLC method for determination of miconazole, econazole and its impurities in solid dispersions The aim of the submitted thesis was to create a new analytical method for the determination of miconazole, econazole and its three impurities. Ultra-high performance liquid chromatography (UHPLC) was used. A KinetexTM XB C18 column, 1.7 μm particle size, 50 x 2.1 mm was used for the separation. The mobile phase was composed of the acetate buffer pH 7.8 in a mixture with methanol (80:20) and of acetonitrile with methanol (60:40), in a total ratio of 60:40. A gradient elution was used. Flow rate was set to 0.6 ml / min. Butylparaben was chosen as the internal standard. All substances were detected at a wavelength of 225nm. Total analysis time was 9 minutes. After optimization of the separation conditions, the method was partially validated and used for practical measurements to determine the content of miconazole in solid dispersions.
|
|
|
Stability testing of thiomersal stock solution by HPLC
Unverdorbenová, Veronika ; Matysová, Ludmila (advisor) ; Sklenářová, Hana (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Veronika Unverdorbenová Supervisor: doc. PharmDr. Ludmila Matysová, Ph.D. Title of the diploma thesis: Testing the stability of spare thiomersal solution by HPLC method. The aim of this thesis is testing the stability of thiomersal and subsequently establish conditions of storing the thiomersal solution. Reversed-Phase High Performance Liquid Chromatography was used for observing the concentrations of thiomersal in samples kept in different conditions. Tested samples were aqueous solutions of thiomersal with pH 6,85 and 7,5. These samples were stored in dark glass and plastic containers. Due to the non- photostability of thiomersal, the samples were stored in the dark. The temperature was laboratory and 4 řC. The samples were observed for the period of 90 days. Following the analysis, the most convenient conditions for storing the thiomersal solution is lowered temperature around 4 řC a pH 7,5. Under these storage conditions there were no substantial differences in the stability of thiomersal in the samples stored in plastic or glass containers. These samples were stable for the period of three months.
|
|
|
The use of supercritical fluid chromatography in pharmaceutical analysis
Babičová, Barbora ; Khalikova, Maria (advisor) ; Matysová, Ludmila (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Barbora Babičová Supervisor: Mgr. Maria Khalikova, CSc. Consultant: doc. PharmDr. Lucie Nováková, Ph.D. Title of the Diploma Thesis: The use of supercritical fluid chromatography in pharmaceutical analysis Keywords: enzalutamide, ticagrelor, supercritical fluid chromatography, method validation Enzalutamide is a new drug for the treatment of metastatic form of prostate cancer. Ticagrelor is a drug with antiplatelet activity. The optimization of UHPSFC/UV methods for analysis of both active substances enzalutamide, and ticagrelor, and their respective impurities is described in diploma thesis. In the case of enzalutamide, there were 4 impurities analysed using following conditions: Viridis BEH 2-EP column (3.0 x 100 mm, 1.7 µm) with a column temperature of 40 řC. The mobile phase used was methanol with 10 mM ammonium formate and gradient elution using 0-40 % of organic mobile phase modifier over 3 minutes with a flow rate of 1.5 ml/min. The UV detection was proceed at 270 nm. The total analysis time was 4.5 minutes. Separation of ticagrelor and its 2 impurities was made using Acquity UPLC HSS C18 SB column (3.0 x 100 mm, 1.8 µm). The mobile phase was composed of methanol and acetonitrile (1:1,...
|
|
|
Separation of tocopherols using HPLC technique
Hutníková, Michaela ; Kujovská Krčmová, Lenka (advisor) ; Matysová, Ludmila (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Michaela Hutníková Supervisor: assoc. prof. RNDr. Lenka Kujovská Krčmová Ph.D. Title of diploma thesis: Separation of tocopherols using HPLC technique Vitamin E represents eight related compounds α, β, γ, δ-tocopherols (saturated phytyl side chain) and α, β, γ, δ-tocotrienols (unsaturated phytyl side chain). α-tocopherol was the most studied isomer in the past and its anti-inflammation and proliferative effect was described. Therefore most of cancer prevention trials have been focused on α-tocopherol. Present research studies have described the important role of γ and δ-tocopherols in cell proliferation, anti-inflammation and tumor burden. Also it has been demonstrated that γ-tocopherol inhibits colon, prostate, mammary and lung tumor genesis in animal models, suggesting to have a high potential in the prevention of human cancer. In this study the novel sensitive method for analysis of α, β, γ, δ-tocopherols was developed using the High Performance Liquid Chromatography (HPLC) technique. All the measurements were carried out on the chromatographic system HPLC Prominence LC 20, Shimadzu (Kyoto, Japan). During the method development core-shell columns-Kinetex (Torrance, USA) with different...
|
|
|
HPLC in nutraceuticals analysis of chlorogenic acids
Majorová, Michaela ; Šatínský, Dalibor (advisor) ; Matysová, Ludmila (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Michaela Majorová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: HPLC in nutraceuticals analysis of chlorogenic acids A new UHPLC method was developed and validated for determination of chlorogenic acids and their di-substituted derivates in nutraceuticals and the developed method was used for determination of chlorogenic acids in nutraceuticals Kilostop (Astina Pharm, a.s.), Zelená káva Extra (Medicura natural), Maxivitalis Zelená káva (Simply You Pharmaceuticals), Vieste Zelená káva Premium (Volt Retail), Zelená káva bylinný extrakt (Topvet), Zelená káva (VITO LIFE) a Kyselina chlorogenová (VITO LIFE). The analysis was performed on the Ascentis Express® RP-Amide (100 x 2.1 mm; 2.7 µm) column using gradient elution program with mobile phase consisted of mixture of acetonitrile and 5% aqueous solution of formic acid at flow rate of 0.9 ml/min, the PDA detector wavelenght was set at 325 nm and the column temperature was 30řC. Keywords: UHPLC, chlorogenic acid, green coffee extract, RP-Amide column, nutraceuticals
|
|
|
Comparison of interactions of equol and desmethylangolensin with iron and copper
Němcová, Hana ; Karlíčková, Jana (advisor) ; Matysová, Ludmila (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Botany Candidate: Hana Němcová Supervisor: PharmDr. Jana Karlíčková, Ph.D. Title of Thesis: Comparison of interactions of equol and desmethylangolensin with iron and copper Iron and copper are essential trace elements, which are important for our body. Both elements have a significant effect on the correct function of organs and make part of many enzymes. They are able to accept or donate electrons - conversion between oxidized (Fe3+, Cu2+) and reduced (Fe2+, Cu+) forms. If these metals are excess in organism, they are accumulated in the cells and mediate the creation of free radicals, that destroy cell structures. This deficiency is treated with chelators, which facilitate the excretion of metals from the body. Isoflavonoids are polyfenolic substances, which can have antioxidant effects and they are involved in the scavening of free radicals. Isoflavonoids can have also a pro-oxidative effect, because they are able to reduce metal ions. In this study were tested interactions (chelation and reduction) between the metabolites of isoflavonoids (equol and desmethylangolensin) and ions of iron and copper. Both metabolites only weakly chelate metal ions, but they significantly reduce cupric ions. KEYWORDS: Iron,...
|
|
|
Development and validation of HPLC methods for determination of preservatives in pharmaceutical formulations
Harmáčková, Barbora ; Matysová, Ludmila (advisor) ; Chocholoušová Havlíková, Lucie (referee)
5 ABSTRACT Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Barbora Harmáčková, DiS. Supervisor: doc. PharmDr. Ludmila Matysová, Ph.D. Title of the diploma thesis: Development and validation of HPLC methods for determination volume of preservatives in pharmaceutical formulations This diploma thesis is focused on the development and validation of methods for determination of preservative content in medicinal products, especially thiomersal and benzalkonium chloride. The development was based on the HPLC methods used for benzalkonium chloride a mixture of methanol and 7.5 mM potassium phosphate in a ratio of 68:32 and for a thiomersal mixture of methanol and phosphate buffer in a ratio of 65: 35: 0.9. The development of the methods for both mentioned substances consisted mainly in optimizing the composition of the mobile phase and the temperature conditions of the analysis. In particular, the length of the analysis and the resolution and symmetry of the peaks of the substances being determined were monitored. In the final version of the HPLC method for benzalkonium chloride an isocratic elution with the mobile phase of MetOH: K3PO4 (pH 3, 7.5 mM) in a ratio of 73: 27 was chosen at 50 ř C. In the final version for thiomersal, an HPLC method with the same...
|
|
|
Development and validation of UHPLC method for determination of terbinafine and its impurities
Firleyová, Michaela ; Matysová, Ludmila (advisor) ; Kujovská Krčmová, Lenka (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Michaela Firleyová Supervisor: doc. PharmDr. Ludmila Matysová, Ph.D. Title of diploma thesis: Development and validation of UHPLC method for determination of terbinafine and its impurities A new analytical method for the determination of terbinafine and its degradation products - β-terbinafine, Z-terbinafine and 4-methylterbinafine - was developed by using ultra-high performance liquid chromatography. The best separation of the analytes was achieved with a KinetexTM 1.7 μm - Biphenyl 100A column (50 mm x 2.1 mm). The selected mobile phase was composed of the buffer pH 5.0, made up of the citrate and the phosphate buffer, and methanol (25:75, v/v). Propylparaben as the internal standard was detected at the wavelength of 254 nm, whereas the terbinafine and its three degradation products at 222 nm. The retention time of the terbinafine was 4.2 min, the total analysis time was within 6 minutes. After finding the optimal conditions the method was validated.
|
guest ::
