H. Siren et al., Separation, purity testing and identification of cyanobacterial hepatotoxins with capillary electrophoresis and electrospray mass spectrometry, J CHROMAT A, 839(1-2), 1999, pp. 203-215
Capillary zone electrophoretic and micellar electrokinetic chromatographic
methods with UV detection were investigated for separation and identificati
on of some microcystins isolated from cyanobacterial Anabaena 90 strains in
Finland. The low-sensitivity purity tests with full scan UV-Vis spectra we
re done with a CZE method. All the test compounds, [D-Asp(3),Dha(7)]MCYST-L
R, MCYST-LR, MCYST-YR, [Dha(7)]MCYST-LR, MCYST-RR, [Dha(7)]MCYST-RR, [D-Asp
(3),Dha(7)]MCYST-RR, [D-Asp(3)]MCYST-LR and [D-Asp(3)]MCYST-RR (where MCYST
stands for microcystin) isolated with a preparative HPLC method, could be
separated from each other in a MECC method. The detection limits of the mic
rocystins were below ppm level. The repeatability of the MECC technique was
tested by comparing the absolute migration times with the indices calculat
ed with "in-laboratory" designed programs operating in MATLAB Mathworks Inc
. The identification and the high-sensitivity purity tests of the isolated
microcystins were made with an off-line electrospray mass spectrometer. Ide
ntification could be done for MCYST-YR, MCYST-LR, MCYST-RR, [Dha(7)]MCYST-R
R, [Dha(7)]MCYST-RR, [D-Asp(3)]MCYST-LR, [D-Asp(3)]MCYST-RR, [D-Asp(3), Dha
(7)]MCYST-LR and [D-Asp(3), Dha(7)]MCYST-RR on the basis of their [M+H](+)
or [M+2H](2+) ions in the MS mode and by using the protonated molecule as p
recursor in the MS-MS mode. (C) 1999 Elsevier Science B.V. All rights reser
ved.