Liquid chromatography with electrospray ion-trap mass spectrometry for the determination of anatoxins in cyanobacteria and drinking water
Article first published online: 12 FEB 2003
Copyright © 2003 John Wiley & Sons, Ltd.
Rapid Communications in Mass Spectrometry
Volume 17, Issue 6, pages 583–588, 30 March 2003
How to Cite
Furey, A., Crowley, J., Lehane, M. and James, K. J. (2003), Liquid chromatography with electrospray ion-trap mass spectrometry for the determination of anatoxins in cyanobacteria and drinking water. Rapid Commun. Mass Spectrom., 17: 583–588. doi: 10.1002/rcm.932
- Issue published online: 12 FEB 2003
- Article first published online: 12 FEB 2003
- Manuscript Revised: 20 DEC 2002
- Manuscript Accepted: 20 DEC 2002
- Manuscript Received: 6 SEP 2002
Anatoxin-a (AN) and homoanatoxin-a (HMAN) are potent neurotoxins produced by a number of cyanobacterial species. A new, sensitive liquid chromatography/multiple tandem mass spectrometry (LC/MSn) method has been developed for the determination of these neurotoxins. The LC system was coupled, via an electrospray ionisation (ESI) source, to an ion-trap mass spectrometer in positive ion mode. The [M+H]+ ions at m/z 166 (anatoxin-a) and m/z 180 (homoanatoxin-a) were used as the precursor ions for multiple MS experiments. MS2MS4 spectra displayed major fragment ions at m/z 149 (AN), 163 (HMAN), assigned to [MNH3+H]+; m/z 131 (AN), 145 (HMAN), assigned to [MNH3H2O+H]+, and m/z 91 [C7H7]+. Although the chromatographic separation of these neurotoxins is problematic, reversed-phase LC, using a C18 Luna column, proved successful. Calibration data for anatoxin-a using spiked water samples (10 mL) in LC/MSn modes were: LC/MS (25–1000 μg/L), r2 = 0.998; LC/MS2 (5–1000(μg/L), r2 = 0.9993; LC/MS3 (2.5–1000 μg/L), r2 = 0.9997. Reproducibility data (% RSD, N = 3) for each LC/MSn mode ranged between 2.0 at 500 μg/L and 7.0 at 10 μg/L. The detection limit (S/N = 3) for AN was better than 0.03 ng (on-column) for LC/MS3 which corresponded to 0.6 μg/L. Copyright © 2003 John Wiley & Sons, Ltd.