LC-MS/MS Method Development for the Discovery and Identification of Amphidinols Produced by Amphidinium

Marvin Wellkamp; Francisco García-Camacho; Lorena M Durán-Riveroll; Jan Tebben; Urban Tillmann; Bernd Krock

doi:10.3390/md18100497

LC-MS/MS Method Development for the Discovery and Identification of Amphidinols Produced by Amphidinium

Mar Drugs. 2020 Sep 29;18(10):497. doi: 10.3390/md18100497.

Authors

Marvin Wellkamp¹, Francisco García-Camacho², Lorena M Durán-Riveroll³, Jan Tebben⁴, Urban Tillmann⁴, Bernd Krock⁴

Affiliations

¹ Alfred-Wegener-Institut für Polar und Meeresforschung, 27570 Bremerhaven, Germany.
² Chemical Engineering Department, University of Almería, La Cañada, 04120 Almeria, Spain.
³ CONACyT-Departamento de Biotecnología Marina, Centro de Investigación Científica y de Educación Superior de Ensenada, Ensenada 22860, Mexico.
⁴ Section Ecological Chemistry, Alfred Wegener Institute, Helmholtz Centre for Polar and Marine Research, 27570 Bremerhaven, Germany.

Abstract

Amphidinols are polyketides produced by dinoflagellates suspected of causing fish kills. Here, we demonstrate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the identification and quantification of amphidinols (AM). Novel AM were detected by neutral loss (NL) scan and then quantified together with known AM by selection reaction monitoring (SRM). With the new method, AM were detected in four of eight analyzed strains with a maximum of 3680 fg toxin content per cell. In total, sixteen novel AM were detected by NL scan and characterized via their fragmentation patterns. Of these, two substances are glycosylated forms. This is the first detection of glycosylated AM.

Keywords: dinoflagellate; glycosylation; harmful algae; ichthyotoxin; phycotoxin.

MeSH terms

Chromatography, Liquid / methods*
Dinoflagellida / metabolism*
Polyketides / analysis*
Polyketides / isolation & purification
Tandem Mass Spectrometry / methods*

Substances

Polyketides