Isolation, identification and characterization of degradant impurities in Tolterodine tartrate formulation

• Simple and short gradient LC methods were developed for the detection, isolation and identification of impurities.
• LC–MS compatible HPLC and UPLC methods were developed for the identification all degradants.
• Degradation conditions were optimized to enhance the targeted impurities to maximum extent.
• Single preparative HPLC method was developed for the isolation of all degradants.
• The two unknown impurities were unambiguously characterized by using NMR and mass spectroscopy.

During the stability study of Tolterodine tartrate drug product, two unknown impurities (Impurities I and II) were detected by ultra performance liquid chromatography (UPLC). Both impurities were isolated by preparative liquid chromatography and were subjected to mass and NMR spectral studies. Based on the spectral data, the Impurities I and II were characterized as N-(3-(2-hydroxy-5-methylphenyl)-3-phenylpropyl)-N,N-diisopropyl hydroxyl ammonium trifluoro acetate and 3-(2-hydroxy-5-methylphenyl)-N-isopropyl-3-phenylpropane-1-amine oxide respectively.

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