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Liquid chromatography with electrospray ion‐trap mass spectrometry for the determination of anatoxins in cyanobacteria and drinking water
Author(s) -
Furey Ambrose,
Crowley Janet,
Lehane Mary,
James Kevin J.
Publication year - 2003
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.932
Subject(s) - chemistry , chromatography , mass spectrometry , electrospray , tandem mass spectrometry , electrospray ionization , ion trap , detection limit , selected reaction monitoring , analytical chemistry (journal) , ion , liquid chromatography–mass spectrometry , organic chemistry
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/MS n ) 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. MS 2 MS 4 spectra displayed major fragment ions at m/z 149 (AN), 163 (HMAN), assigned to [MNH 3 +H] + ; m/z 131 (AN), 145 (HMAN), assigned to [MNH 3 H 2 O+H] + , and m/z 91 [C 7 H 7 ] + . Although the chromatographic separation of these neurotoxins is problematic, reversed‐phase LC, using a C 18 Luna column, proved successful. Calibration data for anatoxin‐a using spiked water samples (10 mL) in LC/MS n modes were: LC/MS (25–1000 μg/L), r 2 = 0.998; LC/MS 2 (5–1000(μg/L), r 2 = 0.9993; LC/MS 3 (2.5–1000 μg/L), r 2 = 0.9997. Reproducibility data (% RSD, N = 3) for each LC/MS n 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/MS 3 which corresponded to 0.6 μg/L. Copyright © 2003 John Wiley & Sons, Ltd.