Isolation and Characterization of Zolmitriptan Unknown Impurity by Chromatographic and Mass Spectroscopy

Author(s): G.P. Narasimha Reddy*, T. Srinivasulu Reddy, Vijay Kumar. R and P. Raghuram

Abstract: One unknown impurity in Zolmitriptan film coated tablet was detected during the stability studies by a simple High Performance liquid chromatographic method whose percentage area was ranged from 0.30 to 0.50 % in different stability batches. This unknown product was analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) to determine its molecular weight. Comparison of fragmentation pattern of the protonated species of unknown impurity and Zolmitriptan allow us to proposed possible structure for impurity and its fragments. A detailed study was done to characterize the impurity and it was further synthesized, subsequently characterized and was co injected with the sample and was found to be co-eluting with the impurity in the sample. Impurity was subsequently isolated using preparative scale chromatography and its structure was confirmed using MS/MS derived structural information combined with 1H proton, 13C-NMR and IR analysis. Based on the spectral data impurity was characterized as (4-4-[[3-[2-(Dimethyloxidoamino) ethyl]-1H-indol-5-yl] methyl-2-oxazolidinone).

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