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Analysis of Historical Pharmaceutical Preparations Containing Alkaloids, Sulphonamide, Derivatives of Barbituric Acid, and Derivative of Pyrazolone
Kudláček, Karel ; Nesměrák, Karel (advisor) ; Bosáková, Zuzana (referee)
Pharmaceutical preparations of quinine (injection solutions), sulfanilamide, aminophenazone, barbital (tablets), caffeine, phenobarbital (dragee), and theophylline (suppositories) about seventy years old were analyzed using RP-HPLC. Samples were quantified by HPLC-UV and UV-spectrophotometry. Products of degradation were identified using HPLC-UV and HPLC-MS. Conditions of separation were optimized. The samples of quinine injection solutions consist of 92% or 87% of declared quinine content. Quinotoxine has been identified as the product of quinine degradation. The quantification of theophylline in suppositories and caffeine in dragee did not show any degradation after more than 67 years from their manufacturing. Decrase of potent amount (decrase about 8-22 %) were found in drugs containing sulfanilamide, barbital, phenobarbital and aminophenazone. Products of degradation of these pharmaceuticals were not found.
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Porphyrazine film for use in electrochemical sensor
Merhoutová, Jana ; Nesměrák, Karel (advisor) ; Ludvík, Jiří (referee)
Porphyrazine film for use in electrochemical sensor Abstract: A water soluble N,N',N'',N'''-tetramethyltetra-3,4-pyridinoporphyrazine complex containing cobalt cation (II) as a central atom was used like a mediator for preparation of electrochemical sensor. Such effects on a sensor function like an electrode carrier material, the manner of porphyrazine deposition, pH and thickness of the layer, were studied by cyclic voltammetry method. The sensor was tested for hydrogen detection in water buffer solution consequently.
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Determination of dissociation exponents of selected polyaza derivatives
Hajduová, Jana ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
Title: Determination of dissociation exponents of selected polyaza derivatives Annotation: The aim of this thesis is extimation of dissociation exponets of seclected polyaza derivatives by acid-base titration with potentiometric registration of titration curve. The titration curve was processed using Hyperquad 2006 software. The satisfactory agreement of determined values of dissociation exponents with literature data was found. Key words: dissociation exponent, potentiometric titration, polyaza compounds
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The comparison of methods for determination of ascorbic acid in medical formulations
Kohoutová, Petra ; Nesměrák, Karel (advisor) ; Červený, Václav (referee)
The aim of this thesis is to compare and assess chosen analytical methods for ascorbic acid determination in pharmaceuticals with respect to their correctness, accuracy, time and finance exigencies. Four methods were chosen alkalimetric titration with visual and instrumental indication, iodometry and spectrophotometry. Pills, capsules and injection solution were chosen as samples of pharmaceuticals. The obtained results as to accuracy of the declared value (or range permitted under Pharmacopoeia) agreed by all titration methods, spectrophotometric determination showed overestimated results. All used methods were approximately equally accurate. As time seems to be most optimal acidobasic titration with visual indication, while demanding in terms of time was spectrophotometry. If we consider methods on financial intensity all titration methods were quite equal.
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Flow injection analysis of selected glycosaminoglycans with spectrofluorimetric detection
Tichá, Renata ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
The thesis is focused on a determination of heparin and chondroitin sulfate, using flow injection analysis with spectrofluorimetric detection. The determination is based on the interaction of negatively charged heparin, chondroitin sulfate resp., with a cationic dye (azure B or phenosafranine) which is manifested by the decrease in fluorescence intensity of the dye in its emission maximum. The optimal conditions for the determination in static mode were found, and calibration dependencies were measured. The conditions of FIA were optimized and following parameters were established: the volume of dispensed sample of 100 ml, the length of the reaction coil 60 cm, the flow rate 0.7 ml min-1 , the concentration of azure B 1.6×10-5 mol dm-3 , the concentration of phenosafranine 3.5×10-5 mol dm-3 . For the determination of heparin using azure B it was found: LOD = 0.023 IU ml-1 , LOQ = 0.186 IU ml-1 , and linear dynamic range 0.19-1.43 IU ml-1 . For the determination of heparin using phenosafranine it was found: LOD = 0.102 IU ml-1 , LOQ = 0.192 IU ml-1 , and linear dynamic range 0.19-1.79 IU ml-1 . For the determination of chondroitin sulfate using azure B it was found: LOD = 0.58 mg dm-3 , LOQ = 2.37 mg dm-3 , and linear dynamic range 2.37-8.32 mg dm-3 . The developed determination was applied to the...
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