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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...
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Column switching chromatography for mycotoxines determination in Czech beer samples
Lhotská, Ivona ; Ramos, María Carolina Fernández (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Ivona Lhotská Supervisor, consultant: María Carolina Fernández Ramos, Ph.D, Doc. RNDr. Dalibor Šatínský, Ph.D. Title of Diploma Thesis: Column switching chromatography for mycotoxines determination in Czech beer samples A new fast and sensitive method of high performance liquid chromatography for simultaneous determination of mycotoxins ochratoxin A and citrinin using column- switching system for on-line sample pretreatment was developed. 100 µl of beer was injected directly into the chromatographic system. Isolation of analytes was performed on guard column Ascentis Express RP-C18 (5 x 4.6 mm, 2.7 µm) washing out with methanol - water solution of acetic acid 0.5% (30:70, v/v), at a flow rate 2 ml/min; time of valve switch was set on 2 minutes. The separation was performed on Ascentis Express Phenyl-Hexyl column (100 x 4.6 mm, 2.7 µm) with mobile phase of composition acetonitril - water solution of acetic acid 0.5% at a flow rate 1 ml/min. A gradient was increasing up to 75:25 linearly in time 3 - 5.5 min. The temperature 50řC was set up for column separation. Wavelengths of fluorimetric detection were set at Ex 335 nm, Em 497 nm. Analysis of one sample including on-line pretreatment was...
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Development of GC Metod for the Determination of Vitamine E Acetate in Nutritive Supplements
Kymlová, Helena ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Helena Kymlová Consultant: Doc. RNDr. Dalibor Šatínský, PhD. Title of Thesis: Development of GC metod for the determination of vitamine E acetate in nutritive supplements A GC method was developed for the determination of content of vitamine E acetate in nutritive supplements. The method was optimised and validated. The column Capillary GC, Equity Columns, Equity TM - 5 poly (5 % bifenyl / 95 % dimethylpolysiloxan); 0,32 mm ID x 30 m; 1,0 mm dr was used for the analysis. Helium was used as a carrier. Split was 1 : 100. Flame-ionization detector was used for detection. Optimal conditions for analysis: temperature of column 340 řC, temperature of injection 340 řC, temperature of detector 320 řC, flow-rate 2 ml/min. Fenoxycarb was chosen as an internal standard. The method was used for an analysis of vitamine E acetate in nutritive supplements Geladrink Forte pulverized drink - pineapple and Chondrotin MSM 2600. Determined concentration of vitamine E acetate was re-counted to the content of vitamine E declared by producer.
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Forced degradation studies of dimethindene maleate using HPLC
Pannyová, Anna ; Chocholoušová Havlíková, Lucie (advisor) ; Kujovská Krčmová, Lenka (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Student: Anna Pannyová Supervisor: PharmDr. Lucie Havlíková, Ph.D. Title of diploma thesis: Forced degradation studies of dimethindene maleate using HPLC The aims of this thesis were to perform forced degradation of dimethindene maleate and to optimize the chromatographic conditions for the determination of dimethindene maleate and its related compounds. The stress testing was conducted with drug product/drug in order to exam its stability. Decomposition of the product can lead to loss of the content of the active substance, loss of their pharmacological activity or forming of degradation products. Dimethindene maleate is an antihistamine drug. He affects H1 histamine receptors. Nowadays, high performance liquid chromatography (HPLC) is one of the most used separation techniques for the determination of the drug stability. The stability of dimethindene maleate was investigated using stress testing (forced degradation studies). Dimethindene was stable in aqueous and acid solution as well as under heating (70řC). Significant degradation was observed when the drug was subjected to basic and oxidation stress conditions; this led to the formation of two degradation products DP1 and DP2 (described using...
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Dispersive Solid-Phase Extraction for the Analysis of Chosen Substances in Zingiber officinale
Urbanová, Martina ; Chocholoušová Havlíková, Lucie (advisor) ; Matysová, Ludmila (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Urbanová Consultant: PharmDr. Lucie Chocholoušová Havlíková, Ph.D. Thesis Title: Dispersive Solid-Phase Extraction for the Analysis of Chosen Substances in Zingiber officinale The thesis was focused on the development of optimal extraction method for the analysis of chosen substances contained in Zingiber officinale. Some representative samples containing extracts of Zingiber officinale were chosen. This method was based on the diploma thesis of Martina Urbanová [1]. To get a higher preconcentration factor, dispersive solid-phase extraction (dSPE) was tested for the sample pretreatment. Then, a method of supported liquid extraction (SLE) was examined as another methodology for the sample preparation. Chosen substances, 6-gingerol, 8-gingerol, 6-shogaol and 10-gingerol, were found in almost all samples. Among syrups, the largest amount of substances was contained in the Kitl syrup (preparation with cold water). Among teas, the highest number of substances was contained in Fruit-herbal tea flavored with ginger and lemon. 6-Shogaol was not found in rhizome samples, however, it has been found in the samples of teas and syrups. During the optimization of this method, various...
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HPLC method devolopment for betacarotene determination in nutraceuticals
Hlaváčková, Markéta ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Markéta Hlaváčková Consultant: Doc. RNDr. Dalibor Šatínský, Ph.D. Diploma Thesis Title: Development of HPLC Method for the Determination of Betacarotene in Nutritional Supplements A new HPLC method was optimized and developed for the determination of betacarotene contents in nutritional supplements Betakaroten Farmax, GS Betakaroten FORTE (GreenSwan pharmaceuticals), Walmark Betakaroten, Bioaktivní karoten (Pharma Nord Denmark), Beta karoten Max, BETAVID + LUTEIN (Naturvita), Karovit (Vitabalans Oy), SELZINK PLUS (PRO.MED.CS), Pupalkový olej (Aromatica). The method is based on using Ascentis Express C18 column (30 x 4.6 mm; 2.7 µm) and UV detection at 450 nm. There was used isocratic elution of the mobile phase 100% methanol at a flow-rate of 1.5 ml/min. Column oven temperature was set at 60 řC during the measurement. The retention time of betacarotene under the optimized and validated conditions was 2.185 min. Keywords: betacarotene, HPLC, Betakaroten Farmax, GS Betakaroten FORTE (GreenSwan pharmaceuticals), Walmark Betakaroten, Bioaktivní karoten (Pharma Nord Denmark), Beta karoten Max, BETAVID + LUTEIN (Naturvita), Karovit (Vitabalans Oy), SELZINK PLUS (PRO.MED.CS), Pupalkový olej...
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Study of influence of mobile phase composition on selectivity and retention of the analytes on HILIC stationary phases
Štětková, Kateřina ; Kočová Vlčková, Hana (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Kateřina Štětková Supervisor: RNDr. Hana Vlčková, Ph.D. Title of Diploma thesis: Study of influence of mobile phase composition on selectivity and retention of the analytes on HILIC stationary phases This graduation thesis deals with an influence of concentration of ACN, pH and buffer concentration in mobile phase on retention of selected analytes and on selectivity of Atlantis HILIC Silica column (3 μm, 2,1 mm x 100 mm) and Luna NH2 column (3 μm, 2,0 mm x 100 mm). A set of 35 analytes including neutral, basic and acidic compounds were chosen for this study. Detection was performed by PDA detector at the wave-length of 245 nm. Measurements were carried out using isocratic flow 0.4 ml.min-1 of mobile phase ACN/water (buffer). The column temperature was set up to 30 řC, auto sampler temperature to 4 řC and injection volume to 2 µl. For easier evaluation of results, measured data are presented in charts and tables. These were used to evaluation of columns in terms of selectivity and retention of the individual groups of analytes. The typical HILIC behavior, an increasing retention of analytes with increasing ACN concentration in mobile phase, was observed for Atlantis HILIC Silica column....
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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,...
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