Forced degradation studies are widely used in the pharmaceutical industry to investigate the degradation pathways of drugs to indicate their stability.  Forced degradation reactions are often monitored by stability-indicating assays using liquid chromatography-mass spectrometry (LC-MS), which enables the quantitation of reactants, intermediates, and degradation products and aids in the identification of unknown species.  A stability-indicating assay for the new-to-the-market cancer drug, palbociclib, has been developed and will be presented.   Additionally, we have developed a simple instrument for online monitoring of forced degradation reactions that can be adapted to any commercial LC-MS equipment.  The system allows automated, continuous sampling of reaction mixtures by low flow rate vacuum aspiration followed by continuous, computer-controlled injections for online LC-MS analysis.  The stability of the automated sampling and injection system was excellent, with 3% relative standard deviation in peak area over a 24-h period.  The automated LC-MS method was used to examine the forced degradation of a common antiseptic, chlorhexidine, for 24 h with 15-min temporal resolution.

Development of liquid chromatography-mass spectrometry methods for forced degradation studies

251st National Meeting (2016)

The official archive and repository for all ACS Meetings & Expositions abstracts and select posters or presentations.