An automated workstation for forced degradation of active pharmaceutical ingredients

Abstract

This article describes a system capable of performing and analysing multiple degradation experiments on drug substances as part of the process of developing stability indicating separations methods. Qualitative data are generated on the significant primary degradation processes of the drug of interest. Ten samples are refluxed with stirring in a single heating block. The robot arm is equipped with a sampling device capable of removing aliquots, during the reflux experiment, and transferring them to an HPLC injector. On-line analysis using fast HPLC with diode array and electrospray mass spectrometric detection allows identification of degradants. The methods described offer a significant time savings compared to the previously applied manual approach, and also provide data from multiple time points for each reaction. This increased knowledge about the progress of the reaction aids us in focussing efficiently on the primary degradation processes. © 2002 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 91: 884–892, 2002