Isolation and characterization of novel degradation products of Doxofylline using HPLC, FTIR, LCMS and NMR


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Abstract

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.Graphical abstractHighlightsForced degradation of Doxofylline in ultra-violet (light) condition.Forced degradation of Doxofylline in Basic condition.Isolation and characterization of 2 novel degradation products.Structural elucidation using MS-qTOF, 1D/2D NMR, IR.

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