Structural Elucidation of Unknown Oxidative Degradation Products of Mycophenolate Mofetil Using LC-MSn
| Autor: | Jelena Golubović, Ana Protić, Mila Laušević, Marina Radišić, Mira Zečević, Biljana Otašević |
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| Rok vydání: | 2016 |
| Předmět: |
chemistry.chemical_classification
Chromatography 010401 analytical chemistry Organic Chemistry Clinical Biochemistry Mycophenolate 01 natural sciences Biochemistry Aldehyde 6. Clean water Mycophenolic acid 010406 physical chemistry 0104 chemical sciences Analytical Chemistry Adduct chemistry.chemical_compound chemistry Liquid chromatography–mass spectrometry medicine Ammonium Hydrogen peroxide Ammonium acetate medicine.drug Nuclear chemistry |
| Zdroj: | Chromatographia |
| ISSN: | 1612-1112 0009-5893 |
| Popis: | Unknown degradation products of mycophenolate mofetil formed under oxidative stress conditions have been characterized via LC-MSn, using an RP-LC column (50 mm length, 2.1 mm i.d., 1.9 A mu m). The mobile phase consisted of 26 % acetonitrile and 74 % 9 mM ammonium acetate pH 5.87, the column temperature was set at 40 A degrees C, and the flow rate of the mobile phase was 400 A mu L min(-1). Four degradation products formed under the influence of 15 % hydrogen peroxide after an hour. Two of the degradation products had previously been identified as mycophenolic acid (m/z 321) and the N-oxide of mycophenolate mofetil (m/z 450). The other two unknown degradation products, denoted DP I (m/z 319) and DP II (m/z 466), were investigated in depth in order to identify their structures. The fragmentation patterns of DP I and DP II were established, analyzed, and compared to the fragmentation patterns of mycophenolate mofetil and the N-oxide of mycophenolate mofetil, which aided the elucidation of the structures of the unknown degradation products. The unknown degradation product DP I (m/z 319.2) was proposed to be an oxidized unsaturated mycophenolate aldehyde which also appeared as an ammonium adduct ion at m/z 336.3. The second unknown degradation product, DP II (m/z 466.3), was characterized as a doubly oxidized derivative of mycophenolate mofetil. A possible degradation pathway of mycophenolate mofetil under the influence of an oxidizing agent was also proposed. |
| Databáze: | OpenAIRE |
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