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J Pharm Biomed Anal. 2013 Oct;84:69-76. doi: 10.1016/j.jpba.2013.05.043. Epub 2013 Jun 6.

Characterization of the components of meleumycin by liquid chromatography with photo-diode array detection and electrospray ionization tandem mass spectrometry.

Author information

1
Department of Antibiotics, National Institutes for Food and Drug Control, Beijing 100050, PR China.

Abstract

Reversed-phase liquid chromatography coupled with photo-diode array (PDA) detection and electrospray ionization tandem mass spectrometry (ESI-MS/MS) was used to characterize the components of meleumycin, a 16-membered macrolide antibiotic produced by fermentation. In total 31 components were characterized in commercial samples, including 12 impurities that had never been reported before and 12 others that were partially characterized. The structures of these unknown compounds were deduced by comparison of their fragmentation patterns with those of known components. Their ultraviolet spectra and chromatographic behavior were used to confirm the proposed structures: e.g. λmax shift from 232 nm to 282 nm would indicate the presence of an α-, β-, γ-, δ-unsaturated ketone instead of a normal α-, β-, γ-, δ-unsaturated alcohol in the 16-membered ring of the examined components. Compared to other methods, this LC/MS(n) method is particularly advantageous to characterize minor components at trace levels in multi-components antibiotics, in terms of sensitivity and efficiency.

KEYWORDS:

Component identification; Liquid chromatography–mass spectrometry; Macrolide antibiotic; Meleumycin; Photo-diode array detection

PMID:
23807001
DOI:
10.1016/j.jpba.2013.05.043
[Indexed for MEDLINE]

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