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

Dhb Microcystins Discovered in USA Using an Online Concentration LC–MS/MS Platform

Department of Chemistry, Wayne State University, Detroit, MI 48202, USA
Author to whom correspondence should be addressed.
Toxins 2019, 11(11), 653;
Received: 4 October 2019 / Revised: 1 November 2019 / Accepted: 3 November 2019 / Published: 10 November 2019
Based on current structural and statistical calculations, thousands of microcystins (MCs) can exist; yet, to date, only 246 MCs were identified and only 12 commercial MC standards are available. Standard mass spectrometry workflows for known and unknown MCs need to be developed and validated for basic and applied harmful algal bloom research to advance. Our investigation focuses on samples taken in the spring of 2018 from an impoundment fed by Oser and Bischoff Reservoirs, Indiana, United States of America (USA). The dominant cyanobacterium found during sampling was Planktothrix agardhii. The goal of our study was to identify and quantify the MCs in the impoundment sample using chemical derivatization and mass spectrometry. Modifying these techniques to use online concentration liquid chromatography tandem mass spectrometry (LC–MS/MS), two untargeted MCs have been identified, [d-Asp3, Dhb7]-MC-LR and [Dhb7]-MC-YR. [Dhb7]-MC-YR is not yet reported in the literature to date, and this was the first reported incidence of Dhb MCs in the United States. Furthermore, it was discovered that the commercially available [d-Asp3]-MC-RR standard was [d-Asp3, Dhb7]-MC-RR. This study highlights a workflow utilizing online concentration LC–MS/MS, high-resolution MS (HRMS), and chemical derivatization to identify isobaric MCs. View Full-Text
Keywords: microcystins; cyanotoxins; (2S,3S,4E,6E,8S,9S)-3-amino-9-methoxy-2,6,8-trimethyl-10-phenyldeca-4,6-dienoic acid (Adda)-ELISA; LC–MS/MS; HRMS microcystins; cyanotoxins; (2S,3S,4E,6E,8S,9S)-3-amino-9-methoxy-2,6,8-trimethyl-10-phenyldeca-4,6-dienoic acid (Adda)-ELISA; LC–MS/MS; HRMS
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Birbeck, J.A.; Peraino, N.J.; O’Neill, G.M.; Coady, J.; Westrick, J.A. Dhb Microcystins Discovered in USA Using an Online Concentration LC–MS/MS Platform. Toxins 2019, 11, 653.

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