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Structure elucidation of four related substances in gramicidin with liquid chromatography/mass spectrometry
C Govaerts1, J Orwa, A Van Schepdael
1Katholieke Universiteit Leuven, Faculteit Farmaceutische Wetenschappen, Laboratorium voor Farmaceutische Chemie en Analyse van Geneesmiddelen, E. Van Evenstraat 4, B-3000 Leuven, Belgium.
Abstract:
A selective reversed phase liquid chromatography/mass spectrometry (LC/MS(n)) method is described for the identification of related substances in commercial gramicidin samples. Mass spectral data are acquired on an LCQ ion trap mass spectrometer equipped with an electrospray interface operated in the positive and the negative ion mode. The LCQ is ideally suited for identification of related substances because it provides on-line LC/MS(n) capability. Compared with UV detection the main advantage of this hyphenated LC/MS(n) technique is the efficient identification of novel related substances without time-consuming isolation and purification procedures. Using this method four novel related substances were separated and identified in a commercial sample.