title: Reliable and sensitive method for determination of microcystins in complicated matrices by frit-fast atom bombardment liquid chromatography/mass spectrometry.
abstract: A reliable and sensitive method for determination of hepatotoxic microcystins in complicated matrices by frit-fast atom bombardment liquid chromatography/mass spectrometry (Frit-FAB LC/MS) is described. Immonium ions of constituent amino acids, which were obtained together with molecular ion species by FAB mass spectral analysis of standard microcystins RR, YR, LR, and [D-Asp3] and [Dha7]microcystins LR using flow injection system composed of Frit-FAB probe, showed potential for reliable identification of microcystins by Frit-FAB LC/MS. Frit-FAB LC/MS using a microbore column provided not only the baseline separation of standard microcystins RR, YR, and LR but 200-fold higher sensitivity than that using conventional column. Furthermore, when a selected ion monitoring (SIM) technique was used, the detection limits of microcystins RR, YR, and LR were 300, 350, and 400 pg, respectively, at a signal-to-noise ratio of 5:1, and calibration curves of each microcystin showed a linear relationship from 2 ng to 50 ng. Finally, identification and quantitative analyses of microcystins in water samples were carried out.
authors.affiliation: Aichi Prefectural Institute of Public Health, Nagoya, Japan.
authors.forename: F
authors.initials: F
authors.lastname: Kondo
authors.forename: Y
authors.initials: Y
authors.lastname: Ikai
authors.forename: H
authors.initials: H
authors.lastname: Oka
authors.forename: H
authors.initials: H
authors.lastname: Matsumoto
authors.forename: S
authors.initials: S
authors.lastname: Yamada
authors.forename: N
authors.initials: N
authors.lastname: Ishikawa
authors.forename: K
authors.initials: K
authors.lastname: Tsuji
authors.forename: K
authors.initials: K
authors.lastname: Harada
authors.forename: T
authors.initials: T
authors.lastname: Shimada
authors.forename: M
authors.initials: M
authors.lastname: Oshikata
mesh_terms: D002853:Chromatography, Liquid; D000458:Cyanobacteria / Q000737:chemistry; D017022:Flow Injection Analysis; D005618:Fresh Water / Q000032:analysis; D008387:Marine Toxins; D052998:Microcystins; D010456:Peptides, Cyclic / Q000032:analysis*; D010749:Phosphoprotein Phosphatases / Q000037:antagonists & inhibitors*; D016339:Spectrometry, Mass, Fast Atom Bombardment
chemical_list: D008387:Marine Toxins; D052998:Microcystins; D010456:Peptides, Cyclic; C078588:microcystin; C063855:microcystin RR; D010749:Phosphoprotein Phosphatases; C057862:cyanoginosin LR