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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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Analysis of the degradation products of the active substances in historical pharmaceutical relicts from 18th and 20th century.
Čambal, Peter ; Nesměrák, Karel (advisor) ; Kubíčková, Anna (referee)
Historical pharmaceutical preparations analyzed in this thesis were a senna extract more than 200 years old, an ointment "Naso-Merfen" 75 years old, and an ointment "Sulfathiazol" 42 years old. The active substances in the analyzed samples were sennosides A and B (senna extract), ephedrine and menthol (the ointment "Naso-Merfen"), and sulfathiazole (the ointment "Sulfathiazol"). The senna extract was analyzed by RP-HPLC and HPLC-MS. Separation conditions were optimized, especially for separation of the sennoside A and B enantiomers. The active substances were not detected in the sample. One degradation product and substances characteristic for senna were identified. Their presence in the historical and contemporary sample was compared. Detailed ESI− -MSn fragmentation mechanisms of sennoside A and B have been proposed. The sample of the ointment "Naso-Merfen" was analyzed by HILIC-UV, HPLC-MS, GC-MS, and AAS. Separation conditions were optimized. The active substances were quantified. Degradation products of the active substances were not detected in the sample. The sample of the ointment "Sulfathiazol" was analyzed by RP-HPLC and HPLC-MS. Separation conditions were optimized. The active substance was quantified. Degradation products of the active substance were not detected. The authenticity of...
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Analysis of the composition and degradation of pharmaceutical substances and pharmaceutical preparations from the 18th and 20th centuries
Kudláček, Karel
The dissertation focused on the analysis of twenty historical remains of pharmaceutical substances and pharmaceutical preparations dating to the 18th and 20th century by liquid and gas chromatography with UV-spectrometric or mass spectrometric detection. The analytical approach was chosen with regards to the age and pharmaceutical forms of the analyzed historical remain. The authenticity of the sample was verified by identifying the active ingredients, their possible degradation products and other excipients by tandem mass spectrometry. The fragmentation of some analytes was also studied by tandem mass spectrometry. The stability of historical pharmaceutical preparations from the 20th century was assessed on the basis of a decrease in the concentration of active substances compared to the content declared by the manufacturer or, in case of historical pharmaceutical remains from the 18th century, on the basis of active substance concentrations determined in the historical residue and current reference material. A multi-analytical approach combining five analytical methods, the results of which complement each other, was used to analyze the historical remains of ointments. While the active substances identified in ipecacuanha were found to be partially degraded, they were completely degraded in senna...
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Analysis of the composition and degradation of pharmaceutical substances and pharmaceutical preparations from the 18th and 20th centuries
Kudláček, Karel ; Nesměrák, Karel (advisor) ; Bosáková, Zuzana (referee) ; Gabriel, Jiří (referee)
The dissertation focused on the analysis of twenty historical remains of pharmaceutical substances and pharmaceutical preparations dating to the 18th and 20th century by liquid and gas chromatography with UV-spectrometric or mass spectrometric detection. The analytical approach was chosen with regards to the age and pharmaceutical forms of the analyzed historical remain. The authenticity of the sample was verified by identifying the active ingredients, their possible degradation products and other excipients by tandem mass spectrometry. The fragmentation of some analytes was also studied by tandem mass spectrometry. The stability of historical pharmaceutical preparations from the 20th century was assessed on the basis of a decrease in the concentration of active substances compared to the content declared by the manufacturer or, in case of historical pharmaceutical remains from the 18th century, on the basis of active substance concentrations determined in the historical residue and current reference material. A multi-analytical approach combining five analytical methods, the results of which complement each other, was used to analyze the historical remains of ointments. While the active substances identified in ipecacuanha were found to be partially degraded, they were completely degraded in senna...
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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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