LC-NMR and LC-MS identification of an impurity in a novel antifungal drug icofungipen.
Successful use of LC-NMR and LC-MS for rapid identification of an impurity in a novel antifungal drug icofungipen has been demonstrated. Complementary information obtained from the two methods made it possible to determine the structure of A1 prior to its isolation and purification. Stop-flow LC-NMR ((1)H and DQFCOSY), LC-MS and LC-MS/MS spectra have shown that A1 is structurally related to icofungipen. It was later isolated and prepared synthetically and its structure was corroborated by high-resolution NMR spectroscopy.
Novak
Predrag
P
Department of Chemistry, University of Zagreb, Croatia. pnovak@chem.pmf.hr
Tepes
Predrag
P
Ilijas
Marina
M
Fistrić
Ines
I
Bratos
Igor
I
Avdagić
Amir
A
Hamersak
Zdenko
Z
Marković
Vesna Gabelica
VG
Dumić
Miljenko
M
D000935:Antifungal Agents / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D003515:Cycloleucine / Q000031:analogs & derivatives* / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*
D000935:Antifungal Agents; D003515:Cycloleucine; C114614:2-amino-4-methylenecyclopentane-1-carboxylic acid