The Use of Complimentary Stationary Phases and 2-Dimensional HPLC for the Separation of the Synthesis and Degradants of Tipredane (INN)

摘要

The article describes how stationary phase characterisation can be successfully employed to identify RP-LC columns of complimentary chromatographic selectivity for use in a 2-dimensional LC 'heart cutting technique' to separate a complex mixture of a pharmaceutically relevant steroid and its degradants/synthetic impurities including the intractable separation of two C17 diastereoisomers (epimers). The separation mechanism of the C17 epimers appears to be controlled by the spacial orientation of the bonded ligands which preferentially restricts access of one of the epimers into the RR The technique has been able to detect as low as 0.1 % w/w of the unwanted C17 epimer.