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The Development and Validation of HPLC Methods for Determination of Ketoprofen in Pharmaceutical Preparations
Bajcurová, Lucie ; Matysová, Ludmila (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Lucie Bajcurová Consultant: PharmDr. Ludmila Matysová, Ph.D. Title of Thesis: The Development and Validation of HPLC Methods for Determination of Ketoprofen in Pharmaceutical Preparations The already developed method for determination of ketoprofen in the pharmaceutical preparation "PRONTOFLEX" - a 10% skin spray has been validated. The precision expressed as relative standard deviation was 1.43 %. The accuracy expressed as recovery was 101.52 %. The correlation coefficient R was more than 0.999. The method for determination of ketoprofen in the pharmaceutical preparation "Ketonal" - a 5% cream has been further developed. The already developed method has been validated. The chromatographic separation was performed on a SUPELCO Discovery C18 column (150 mm x 4.6 mm, 5 µm). The mobile phase consisted of a mixture of acetonitrile, water and a phosphate buffer pH 3.5 (39:59:2, v/v/v). At a mobile phase flow rate of 1.5 ml/min, injection volume of 5 μl and UV detection at a wavelength of 233 nm, the total time of analysis was less than 10 minutes. Ethylparaben was used as an internal standard. The precision expressed as relative standard deviation was 0.64 %. The accuracy expressed as...
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Determination of vitamine C and dehydroascorbic acid using UHPLC-MS method
Proroková, Zuzana ; Nováková, Lucie (advisor) ; Chocholoušová Havlíková, Lucie (referee)
A coupling of Ultra High Performance liquid chromatography with mass spectrometry provides a technique, which is rapid and sensitive. This thesis is focused on the use of UHPLC-MS for the determination of ascorbic acid (AA) and dehydroascorbic acid (DHA). AA is a small polar molecule that acts as an antioxidant. After oxidation AA creates DHA. AA/DHA ratio is an indicator of a redox state of organism. For the determination of AA and DHA several methods have been developed, which usually do not allow the simultaneous analysis, but require multistep subtraction procedure. The optimization of UHPLC-MS method for the determination of AA and DHA include the choice of mobile and stationary phase and mass spectrometry detector set- up. The choice of appropriate conditions depended mainly on retention time and the detector response. The effect of stationary phase, concentration, pH, composition of mobile phase on retention of AA and DHA was observed. Effect of mobile phase on stability of AA and DHA was observed as well. BEH Shield RP C18, BEH HILIC and BEH Amide column were compared. The best results were achieved on column BEH Shield RP C18. Measurements with 0.1%, 0.05%, 0.01% formic acid, 0.1%, 0.05%, 0.01% acetic acid, ammonium formate at pH 3.5 and amonium acetate at pH 4.4 and 6.8 as a water...
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The metod development for determination of diazodinitrofenol explosive
Ihnát, Lukáš ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Consultant: Doc. RNDr. Dalibor Šatínský, PhD. Diploma Thesis Title: The method development for determination of diazodinitrofenol explosive A new HPLC method for determination of diazodinitrophenol alongside with sodium picramate was developed and optimized. Column Ascentis® Express C18 10cm x 3mm; 2.7µm particles was select as most suitable one. Detection of compounds was performed at 220 nm using UV detector. Mobile phase consist of mixture 0.085% H3PO4 and acetonitrile in ratio 70/30. Flow rate was determined at 0.8 ml/min. Column oven temperature was set to 50řC. Retention times under these condition was tDDNP=1.324 min a tPikNa=4.012 min. Keywords: determination, diaziodinitrophenol, sodium picraminate, HPLC, chromatography, dinol, DDNP
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Vývoj imunochromatografického stanovení pro testování reálných vzorků obsahujících TNT
Kosařová, Lucie ; Chocholouš, Petr (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical chemistry Candidate: Lucie Kosařová Supervisor: PharmDr. Petr Chocholouš, Ph.D. Title of diploma thesis: Development of lateral flow immunoassay for testing real samples containing TNT Obtaining results very fast is requested more often these days. This is particularly true for dangerous and potentially dangerous compounds. One of these compounds is 2,4,6,-trinitrotoluene (TNT), which was tested in this research. TNT has been extensively used as a military explosive and is still one of the most widely used explosives. Its advantages, such as low manufacturing costs, safety of handling and fairly good explosive power can be tempting for abuse by terrorists. In addition, TNT is a well known pollutant because of its toxicity and low biodegradability. It can contaminate surface and ground waters, soils and sediments, thus causing environmental and health problems. According to these facts there is a requirement to detect this nitroaromatic compound in minimal concentrations very fast and outside the laboratory. These demands could be met by the lateral flow test. In this research lateral flow immunoassay (LFIA) based on colloidal gold nanoparticle labels was developed for detection of TNT in real samples. The...
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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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