A new compound Imp-F was obtained and the structures were elucidated by using spectral data (NMR, MS, and IR); the potential process-related impurities were speculated in the apremilast drug; LC conditions were optimized and an effective HPLC method for the quantitative determination of the potential process-related impurities in apremilast was developed.
High-performance liquid chromatography analysis of vonoprazan fumarate, a novel proton pump inhibitor drug revealed six impurities. These were identified by liquid chromatography with mass spectrometry. Further, the structures of the impurities were confirmed by synthesis followed by characterization by mass spectrometry, NMR spectroscopy, and infrared spectroscopy. On the basis of these data and knowledge of the synthetic scheme of vonoprazan fumarate, the previously unknown impurity was identified as 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3-yl]-N-methyldimethylamine, which is a new compound. The possible mechanisms by which these impurities were formed were also discussed. A high-performance liquid chromatography method was optimized in order to separate, selectively detect, and quantify all process-related impurities of vonoprazan fumarate. The presented method has been validated in terms of linearity, limits of detection, and quantification, and response factors and, therefore, is highly suitable for routine analysis of vonoprazan fumarate related substances as well as stability studies.
Palbociclib is the first U.S. Food and Drug Administration-approved cyclin-dependent kinase inhibitor indicated in combination with letrozole for the treatment of breast cancer. Development of a selective method for the determination of any impurities contained in this drug is significantly important to ensure the quality and safety of palbociclib. In this study, a reliable reversed-phase HPLC method for the separation and determination of eight potential impurities was developed and validated. The structures of two new compounds and six other process-related impurities were characterized and confirmed by MS, NMR, and IR. Based on spectral analysis and available knowledge of the synthetic route of palbociclib, these two new compounds were designated as 6-acetyl-8-cyclopentyl-5-methyl-2-{[3-(piperazin-1-yl)pyridin-2yl]amino}pyrido [2,3-d]pyrimidin-7(8H)-one and 6-acetyl-8-cyclopentyl-5-methyl-2-{[5-(4-t-butyloxycarbonyl-)-(piperazin-1-yl)pyridin-2yl]amino}pyrido [2,3-d]pyrimidin-7(8H)-one. The developed method was validated for accuracy, precision, linearity, sensitivity, robustness, and solution stability.
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