title: The application of LC-NMR and LC-MS for the separation and rapid structure elucidation of an unknown impurity in 5-aminosalicylic acid.
abstract: This work 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 N1 was later confirmed by high-resolution NMR spectroscopy 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.
authors.affiliation: Department of Analytical Chemistry, Faculty of Natural Sciences, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia. pnovak@chem.pmf.hr
authors.forename: Predrag
authors.initials: P
authors.lastname: Novak
authors.forename: Predrag
authors.initials: P
authors.lastname: Tepes
authors.forename: Ines
authors.initials: I
authors.lastname: Fistrić
authors.forename: Igor
authors.initials: I
authors.lastname: Bratos
authors.forename: Vesna
authors.initials: V
authors.lastname: Gabelica
mesh_terms: D002853:Chromatography, Liquid; D004121:Dimethyl Sulfoxide; D004340:Drug Contamination; D007202:Indicators and Reagents; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D019804:Mesalamine / Q000737:chemistry*; D011786:Quality Control; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D007202:Indicators and Reagents; D019804:Mesalamine; D004121:Dimethyl Sulfoxide