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Open AccessArticle

A Data-Independent Methodology for the Structural Characterization of Microcystins and Anabaenopeptins Leading to the Identification of Four New Congeners

1
Environment and Climate Change Canada, Aquatic Contaminants Research Division, Montréal, QC H2Y 2E5, Canada
2
NSERC-Industrial Chair on Drinking Water, CGM Department, École Polytechnique de Montréal, Montréal, QC H3T 1J4, Canada
3
Department of Chemistry, Université de Montréal, Montréal, QC H3T 1J4, Canada
*
Author to whom correspondence should be addressed.
Toxins 2019, 11(11), 619; https://doi.org/10.3390/toxins11110619
Received: 30 September 2019 / Revised: 17 October 2019 / Accepted: 23 October 2019 / Published: 26 October 2019
Toxin-producing cyanobacteria are responsible for the presence of hundreds of bioactive compounds in aquatic environments undergoing increasing eutrophication. The identification of cyanotoxins is still emerging, due to the great diversity of potential congeners, yet high-resolution mass spectrometry (HRMS) has the potential to deepen this knowledge in aquatic environments. In this study, high-throughput and sensitive on-line solid-phase extraction ultra-high performance liquid chromatography (SPE-UHPLC) coupled to HRMS was applied to a data-independent acquisition (DIA) workflow for the suspect screening of cyanopeptides, including microcystin and anabaenopeptin toxin classes. The unambiguous characterization of 11 uncommon cyanopeptides was possible using a characterization workflow through extensive analysis of fragmentation patterns. This method also allowed the characterization of four unknown cyanotoxins ([Leu1, Ser7] MC-HtyR, [Asp3]MC-RHar, AP731, and AP803). The quantification of 17 common cyanotoxins along with the semi-quantification of the characterized uncommon cyanopeptides resulted with the identification of 23 different cyanotoxins in 12 lakes in Canada, United Kingdom and France. The concentrations of the compounds varied between 39 and 41,000 ng L−1. To our knowledge, this is the first DIA method applied for the suspect screening of two families of cyanopeptides simultaneously. Moreover, this study shows the great diversity of cyanotoxins in lake water cyanobacterial blooms, a growing concern in aquatic systems. View Full-Text
Keywords: cyanotoxins; cyanobacteria; microcystins; anabaenopeptins; LC-HRMS; data-independent acquisition; suspect screening; non-target screening; structural characterization cyanotoxins; cyanobacteria; microcystins; anabaenopeptins; LC-HRMS; data-independent acquisition; suspect screening; non-target screening; structural characterization
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Roy-Lachapelle, A.; Solliec, M.; Sauvé, S.; Gagnon, C. A Data-Independent Methodology for the Structural Characterization of Microcystins and Anabaenopeptins Leading to the Identification of Four New Congeners. Toxins 2019, 11, 619.

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