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The application of LC-NMR and LC-MS for the separation and rapid structure elucidation of an unknown in 5-aminosalicylic acid

UNCORRECTED PROOF Thiswork has demonstrated the usefulness of combining liquid chromatography- nuclear magnetic resonance spectroscopy (LC- NMR) and liquid chromatography- mass spectrometry (LC- MS) methodologies for a rapid identification of an unknown impurity (N1) in the drug 5-aminosalycilic acid. Complementary information obtained from the two methods has revealed plenty of structural information and led to the fast on-line structure determination of N1 prior to its isolation and purification. The analysis of LC-NMR and LC- MS spectra revealed that N1 and 5-aminosalycilic acid are structurally closely related compounds. The structure of N1was later confirmed by high-resolutionNMRspectroscopy of the isolated compound and the atom assignment was made. The approach described here has potential for 5-aminosalycilic acid impurity profiling and monitoring the production process.

5-Aminosalicylic acid; Impurity; Liquid chromatography– nuclear magnetic resonance spectroscopy; Liquid chromatography– mass spectrometry

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