Summary
In the determination of ephedrine using reversed-phase, ion-pair liquid chromatography, a chromatographically pure sample was observed to give three peaks under certain mobile phase conditions. The mobile phases which produced maximum peak splitting were determined for ephedrine and a number of other sympathomimetic drugs.
A proposal that peak splitting was the result of the composite interplay of two discrete chromatographic mechanisms, was investigated. The results of analysis by GC/MS confirmed that each peak was due to ephedrine, however, only one of the three split peaks was found to contain ion pairs. It is postulated that peak splitting is a physical phenomenon on reversed-phase columns and the separation of these drugs by ion-pair HPLC is based on a mixed rather than a single mechanism.
This study has also shown that errors can arise in ion-pair HPLC when multiple peaks are assumed to indicate heterogeneity. Interconvertible species of the same solute can give rise to these peaks.
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Low, G.K.C., Duffield, A.M. & Haddad, P.R. Peak-splitting in reversed-phase, ion-pair high-performance liquid chromatography of sympathomimetic drugs and its probable mechanism. Chromatographia 15, 289–296 (1982). https://doi.org/10.1007/BF02265679
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DOI: https://doi.org/10.1007/BF02265679