Isolation and characterization of novel degradation products of Doxofylline using HPLC, FTIR, LCMS and NMR
| Autor: | Ch. Krishnam Raju, Sameer G. Navalgund, Avadhesh Kumar Pandey, Arunima Pola, Kaushik Ghosh, P Sanath Kumar Goud, S Gururaj, Mrunal A. Jaywant |
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| Rok vydání: | 2017 |
| Předmět: |
Magnetic Resonance Spectroscopy
Clinical Biochemistry Pharmaceutical Science Computer Science::Computational Geometry 01 natural sciences High-performance liquid chromatography Analytical Chemistry chemistry.chemical_compound Theophylline Spectroscopy Fourier Transform Infrared Drug Discovery Fourier transform infrared spectroscopy Chromatography High Pressure Liquid Astrophysics::Galaxy Astrophysics Spectroscopy Doxofylline Preparative hplc Chromatography 010405 organic chemistry Elution 010401 analytical chemistry 0104 chemical sciences chemistry Forced degradation Degradation (geology) Astrophysics::Earth and Planetary Astrophysics Enantiomer |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 140:1-10 |
| ISSN: | 0731-7085 |
| DOI: | 10.1016/j.jpba.2017.02.044 |
| Popis: | Forced degradation of Doxofylline (DFL) in different stress (base and peroxide) conditions gave rise to two potential unknown impurities. These unknown degradation products DFL DEG-I and DFL DEG-II were evaluated using a new-reverse-phase high performance liquid chromatography (HPLC), where it was eluted at 0.44 and 1.09 relative retention times to DFL peak. DFL DEG-I and DFL DEG-II were isolated using preparative HPLC from degradation mixtures. The structure of DFL DEG-I and DFL DEG-II were elucidated using high resolution MS, multi-dimensional NMR and FTIR spectroscopic techniques, and characterized. The stereochemistry of the enantiomers in DFL DEG-II has further been investigated using computational techniques. To the best of our knowledge, DFL DEG-I and DFL DEG-II are novel impurities and not reported elsewhere. |
| Databáze: | OpenAIRE |
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