An automated workstation for forced degradation of active pharmaceutical ingredients

✍ Scribed by Jonathan L. Sims; John K. Roberts; Adrian G. Bateman; Judith A. Carreira; Martin J. Hardy

• Publisher: John Wiley and Sons
• Year: 2002
• Tongue: English
• Weight: 176 KB
• Volume: 91
• Category: Article
• ISSN: 0022-3549
• DOI: 10.1002/jps.10055

✦ Synopsis

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 signi®cant primary degradation processes of the drug of interest. Ten samples are re¯uxed with stirring in a single heating block. The robot arm is equipped with a sampling device capable of removing aliquots, during the re¯ux experiment, and transferring them to an HPLC injector. On-line analysis using fast HPLC with diode array and electrospray mass spectrometric detection allows identi®cation of degradants. The methods described offer a signi®cant 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 ef®ciently on the primary degradation processes.