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Analysis of phenobarbital in historical residues of pharmaceuticals in various dosage forms
Belianský, Michal ; Nesměrák, Karel (advisor) ; Kozlík, Petr (referee)
Belianský M.: Analysis of phenobarbital in historical residues of pharmaceuticals in various dosage forms. Master Thesis. Prague, Charles University, Faculty of Science 2022. Abstract: The work analysed four historical pharmaceutical residue samples up to 60 years old. All of the samples analysed contained phenobarbital, but in different dosage forms. The dosage forms of the selected historical pharmaceuticals were tablets, dragees, suppositories, and solution. The HPLC method with UV or mass detection was used for the analysis. Separation of the analytes took place in the SupelcosilTM LC-18 column using binary gradient elution. No degradation product was identified in three of the four historical designs analysed, while other substances not declared in the pharmacopoeias were identified. Two phenobarbital degradation products, feneturide and 3-aminopentanoic acid, were identified in the oldest sample, solution. The concentration of phenobarbital in this preparation decreased by 12.5% compared to the original content declared. Finally, analytes of historical pharmaceutical remains have been selected, quantified, and compared with the declared content. Key words: degradation, HPLC, mass spectrometry, phenobarbital
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Analysis of Nicotine or Opium Alkaloids in Historical Pharmaceutical Relics from 18th Century
Belianský, Michal ; Nesměrák, Karel (advisor) ; Kubíčková, Anna (referee)
Belianský M.: Analysis of Nicotine or Opium Alkaloids in Historical Pharmaceutical Relics from 18th Century. Bachelor Thesis. Prague, Charles University, Faculty of Science 2020. Abstract: Two samples of historical relics of pharmaceuticals dated to the 18th century were analyzed; the first sample contained tobacco, the second laudanum, i.e., a preparation containing opium. HPLC with UV or mass detection was used for analysis. Separation of the alkaloids was performed on X Bridge® BEH C18 column using binary gradient elution. By comparison with a modern tobacco sample and on the basis of data from the literature, the presence of nicotine degradation products, especially 6-hydroxy-N-methylmyosmine, was found in the historical sample. Because the nicotine content in the historical sample was very low, it was not possible to quantify it. The analysis of opium analytes in the second historical relics revealed the main opium alkaloids (cotarnine, morphine, meconin, papaverine, and noscapine) as well as their degradation products. Main alkaloids were also quantified. The ratio of noscapine to cotarnine was determined, which according to the literature is an indicator of the age of opium pharmaceuticals. Key words: degradation, HPLC, mass spectrometry, nicotine alkaloids, opium alkaloids
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