Screening for multiple classes of marine biotoxins by liquid chromatography-high-resolution mass spectrometry |
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Authors: | Blay Pearl Hui Joseph P M Chang James Melanson Jeremy E |
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Institution: | (1) National Research Council of Canada, Institute for Marine Biosciences, 1411 Oxford Street, Halifax, NS, B3H 3Z1, Canada;(2) Thermo Fisher Scientific, 355 River Oaks Parkway, San Jose, CA 95134, USA; |
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Abstract: | Marine biotoxins pose a significant food safety risk when bioaccumulated in shellfish, and adequate testing for biotoxins
in shellfish is required to ensure public safety and long-term viability of commercial shellfish markets. This report describes
the use of a benchtop Orbitrap system for liquid chromatography–mass spectrometry (LC-MS) screening of multiple classes of
biotoxins commonly found in shellfish. Lipophilic toxins such as dinophysistoxins, pectenotoxins, and azaspiracids were separated
by reversed phase LC in less than 7 min prior to MS data acquisition at 2 Hz with alternating positive and negative scans.
This approach resulted in mass accuracy for analytes detected in positive mode (gymnodimine, 13-desmethyl spirolide C, pectenotoxin-2,
and azaspiracid-1, -2, and -3) of less than 1 ppm, while those analytes detected in negative mode (yessotoxin, okadaic acid,
and dinophysistoxin-1 and -2) exhibited mass errors between 2 and 4 ppm. Hydrophilic toxins such as domoic acid, saxitoxin,
and gonyautoxins were separated by hydrophilic interaction LC (HILIC) in less than 4 min, and MS data was collected at 1 Hz
in positive mode, yielding mass accuracy of less than 1 ppm error at a resolving power of 100,000 for the analytes studied
(m/z 300–500). Data were processed by extracting 5 ppm mass windows centered around the calculated masses of the analytes. Limits
of detection (LOD) for the lipophilic toxins ranged from 0.041 to 0.10 μg/L (parts per billion) for the positive ions, 1.6–5.1 μg/L
for those detected in negative mode, while the domoic acid and paralytic shellfish toxins yielded LODs ranging from 3.4 to
14 μg/L. Toxins were detected in mussel tissue extracts free of interference in all cases. |
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