title: Accurate mass measurement at enhanced mass-resolution on a triple quadrupole mass-spectrometer for the identification of a reaction impurity and collisionally-induced fragment ions of cabergoline.
abstract: In this study, accurate mass measurements were made by electrospray ionization (ESI) on a triple quadrupole mass spectrometer operating in enhanced mass-resolution mode (peak width = 0.1 u FWMH), to give qualitative information relating to the pharmaceutical, cabergoline. Accurate mass determinations by ESI-MS were performed on a protonated impurity formed during cabergoline storage. The accurate mass measurement resulted in only one proposed elemental composition for the impurity, using reasonable elemental limits and mass tolerance for the calculation. This information was sufficient to propose a structure for the impurity where ESI-MS/MS proved consistent. The difference between the accurate mass measurement and the exact mass calculated for the proposed structure was 0.8 mmu, with a standard deviation of 0.7 mmu for replicate accurate mass determinations. Accurate mass determinations in ESI-MS/MS provided information on cabergoline fragment ions formed through collisionally-induced dissociation. Since the potential formation of isobaric ions exists for two major cabergoline fragment ions, accurate mass measurement allowed for the determination of the most probable fragment ion structures. The differences between the accurate mass measurements and exact masses calculated for the proposed fragment ions were 1.9 and 2.1 mmu, with standard deviations of 0.4 and 0.8 mmu, respectively, for replicate determinations.
authors.affiliation: Thermo Finnigan, 265 Davidson Avenue, Suite 101, Somerset, NJ 08873, USA. gary.paul@thermo.com
authors.forename: Gary
authors.initials: G
authors.lastname: Paul
authors.forename: Witold
authors.initials: W
authors.lastname: Winnik
authors.forename: Nicola
authors.initials: N
authors.lastname: Hughes
authors.forename: Hans
authors.initials: H
authors.lastname: Schweingruber
authors.forename: Rexford
authors.initials: R
authors.lastname: Heller
authors.forename: Alan
authors.initials: A
authors.lastname: Schoen
mesh_terms: D000077465:Cabergoline; D004340:Drug Contamination; D004873:Ergolines / Q000737:chemistry* / Q000378:metabolism*; D007477:Ions / Q000737:chemistry; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000737:chemistry / Q000378:metabolism; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D004873:Ergolines; D007477:Ions; D004364:Pharmaceutical Preparations; D000077465:Cabergoline