Emerging Lyngbya wollei toxins: A new high resolution mass spectrometry method to elucidate a potential environmental threat |
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| Affiliation: | 1. University of South Carolina, Department of Chemistry and Biochemistry, 631 Sumter Street Columbia, SC 29208, United States;2. University of South Carolina, Center for Interactions of Climate Change on Oceans and Human Health, 921 Assembly St Suit 401, Columbia, SC 29208, United States;1. Cawthron Institute, Private Bag 2, Nelson 7010, New Zealand;2. AgResearch Ltd, Ruakura Research Centre, Private Bag 3123, Hamilton, New Zealand;3. AquaBio Consultants Ltd, PO Box 560, Auckland 1140, New Zealand;4. National Research Council Canada, Measurement Science and Standards, Biotoxin Metrology, 1411 Oxford Street, Halifax, Nova Scotia B3H 3Z1, Canada;5. South Australian Research & Development Institute, GPO Box 397, Adelaide, South Australia, Australia;1. School of Natural Sciences, Bangor University, Bangor, Gwynedd, LL57 2UW, United Kingdom;2. Department of Human Health, Physical Rehabilitation and Vital Activity, Ternopil V. Hnatiuk National Pedagogical University, Ternopil, Ukraine;3. Department of Marine Biology, Institute of Biological Sciences, University of Rostock, Rostock, Germany;4. UK National Crystallographic Service, Chemistry, Faculty of Natural and Environmental Sciences, University of Southampton, England, SO17 1BJ, United Kingdom;5. Department of Environmental Medicine, Poznan University of Medical Sciences, Poznań, Poland;1. Aquatic Ecosystems Protection Research Division, Environment Canada, 105 McGill Street, 7th Floor, Montreal, QC, Canada H2Y 2E7;2. Measurement Science and Standards, National Research Council of Canada, 1411 Oxford Street, Halifax, NS, Canada B3H 3Z1;1. Department of Chemistry, Université de Montréal, 2900 Edouard Montpetit, H3C 3J7, Montréal, QC, Canada;2. Environment and Climate Change Canada, 105 rue McGill, H2Y 2E7, Montréal, QC, Canada;3. BlueLeaf Inc., 310 Chapleau Street, J2B 5E9, Drummondville, QC, Canada;1. Department of Biological Sciences, National University of Singapore, 10 Science Drive 4, 117555, Singapore;2. St. John’s Island National Marine Laboratory (SJINML), Tropical Marine Science Institute (TMSI), National University of Singapore, 18 Kent Ridge Road, 119227, Singapore;1. U.S. Geological Survey, Organic Geochemistry Research Laboratory, Kansas Water Science Center, Lawrence, KS 66049, USA;2. U.S. Geological Survey, Kansas Water Science Center, Lawrence, KS 66049, USA;3. U.S. Environmental Protection Agency, Office of Research and Development, NHEERL, Chapel Hill, NC 27599, USA;4. U.S. Environmental Protection Agency, Office of Wetlands, Oceans, and Watersheds, Ariel Rios Bldg., 1200 Pennsylvania Ave., N.W., Mail Code 4503T, Washington, DC 20460, USA |
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| Abstract: | Mass spectrometric methods for the quantitative and qualitative analyses of algal biotoxins are often complicated by co-eluting compounds that present analytically as interferences. This issue is particularly critical for organic polyamines, where co-eluting materials can suppress the formation of cations during electrospray ionization. Here we present an extraction procedure designed specifically to overcome matrix-derived ion suppression of algal toxins in samples of Lyngbya wollei, a filamentous benthic algae known to produce several saxitoxin analogues. Lyngbya wollei samples were collected from a large, persistent harmful algal bloom in Lake Wateree, SC. Six known Lyngbya wollei-specific toxins (LWT1–6) were successfully resolved and quantified against saxitoxin using hydrophilic interaction liquid chromatography coupled with triple quadrupole and quadrupole time-of-flight mass spectrometry. The parent ions [M2+ – H+]+ were observed for LWTs 1–6 and the [M]2+ ion was observed for LWT5. High resolution mass spectra and unique fragmentation ions were obtained for LWTs 1–6. A dilution factor of 50 resulted in a linear calibration of saxitoxin in the algae matrix. Ion suppression was resolved by sample dilution, which led to linear, positive correlations between peak area and mass of the extracted sample (R2 > 0.96). Optimized sample extraction method and instrument parameters are presented. |
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| Keywords: | Cyanobacteria Saxitoxin Benthic Filamentous Quantification Liquid chromatography |
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