RRC ID 28750
Author Sano T, Takagi H, Nagano K, Nishikawa M, Kaya K.
Title Accurate LC-MS analyses for microcystins using per-15N-labeled microcystins.
Journal Anal Bioanal Chem
Abstract Per-(15)N-labeled microcystins were prepared for use as surrogates for accurate liquid chromatography-mass spectrometry analysis. Two strains of Microcystis aeruginosa were cultured in (15)NO(3)-containing TS-15 medium. To change from the incorporation of (14)N to (15)N into all cell components, cells of Microcystis aeruginosa were precultured in Na(15)NO(3)-containing medium for more than 6 months. After mass cultivation of the strains, cells of each strain were harvested and lyophilized. Microcystin variants were extracted from the lyophilized cells and per-(15)N-labeled microcystin variants were purified using high-performance liquid chromatography and high-performance thin-layer chromatography. The structures of per-(15)N-labeled microcystin variants were confirmed by their mass spectrometry spectra and NMR spectra. When per-(15)N-labeled microcystins were used as surrogates for quantitative analysis of these toxins in cyanobacterial cells, excellent accuracy (98-106%) was obtained, with the m/z of M(+), [M+1](+), and [M+2](+) of both microcystins and the per-(15)N-labeled microcystins as surrogates being completely separated. In conclusion, per-(15)N-labeled microcystins are excellent surrogates for microcystin analysis using liquid chromatography-mass spectrometry.
Volume 399(7)
Pages 2511-6
Published 2011-3
DOI 10.1007/s00216-010-4639-y
PMID 21221535
MeSH Chromatography, High Pressure Liquid / methods Chromatography, Thin Layer / methods Mass Spectrometry Microcystins / chemistry* Microcystins / isolation & purification* Microcystis / chemistry* Microcystis / metabolism Nitrogen Isotopes / metabolism Nuclear Magnetic Resonance, Biomolecular
IF 3.286
Times Cited 11
Algae NIES-107