Hebatallah A Wagdy and Hassan Y Aboul-Enein
This investigation describes the liquid chromatographic behavior in reserved phase mode for the separation of sitagliptin using two halogenated stationary phases namely pentabromobenzyl (PBr) and pentafluorophenyl (PFP) columns as well as the separation mechanism involved.
The optimized separation was achieved using a mobile phase composed of acetonitrile: water: triethylamine: acetic acid (80:20:0.2:0.1; v/v), at a flow rate 1.0 mL/min, at temperature 25°C. The detection wavelength was 268 nm. The quantitative analysis of sitagliptin in bulk and pharmaceutical tablet formulations was performed and validated on PBr column since this column eluted the analyte under study at a shorter retention time than PFP column.
Furthermore, this study led to better understanding of the mechanism of action involved in these newly developed halogenated stationary phases regarding the studied analyte and mobile phase/column parameters. It was found that both columns showed π aromatic- π aromatic, π aromatic- π aliphatic, π aromatic- π cationic interactions, in addition to hydrogen bonding in case of PFP column.
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