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  • Title: Characterization of the trace-level impurities in the bulk drug citalopram by high-performance liquid chromatography/tandem multistage mass spectrometry.
    Author: Sun C, Xu H, Pan Y, Shen Z, Wang D.
    Journal: Rapid Commun Mass Spectrom; 2007; 21(17):2889-94. PubMed ID: 17663502.
    Abstract:
    Five trace impurities were detected in the bulk drug citalopram using high-performance liquid chromatography with UV detection. A simple and sensitive method suitable for liquid chromatography tandem multistage mass spectrometry (HPLC/MS(n)) analysis was developed. Using this method, the fragmentation behavior of citalopram and the impurities was investigated. Four impurities were rapidly characterized, and an unknown impurity was elucidated as 3-(3-dimethylaminopropyl)-N-(1-(3-dimethylaminopropyl)-1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl)-3-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-carboxamide on the basis of the MS(n) and exact mass evidence, and the proposed structure was further confirmed by nuclear magnetic resonance (NMR) experiments after preparative isolation.
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