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Simultaneous Detection of 14 Microcystin Congeners from Tissue Samples Using UPLC- ESI-MS/MS and Two Different Deuterated Synthetic Microcystins as Internal Standards

1
Human and Environmental Toxicology, University of Konstanz, 78457 Konstanz, Germany
2
Cawthron Institute, 7010 Nelson, New Zealand
3
Toxicology of Contaminants Unit, French Agency for Food, Environmental and Occupational Health and Safety, ANSES, 35306 Fougères, France
4
Dr. Feurstein Medical Hemp GmbH, HANAFSAN, Hauptstr. 19A, 6840 Götzis, Austria
5
Organic and Bioorganic Chemistry, University of Konstanz, 78457 Konstanz, Germany
*
Author to whom correspondence should be addressed.
Toxins 2019, 11(7), 388; https://doi.org/10.3390/toxins11070388
Received: 5 June 2019 / Revised: 21 June 2019 / Accepted: 28 June 2019 / Published: 2 July 2019
(This article belongs to the Section Marine and Freshwater Toxins)
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Abstract

Cyanobacterial microcystins (MCs), potent serine/threonine-phosphatase inhibitors, pose an increasing threat to humans. Current detection methods are optimised for water matrices with only a few MC congeners simultaneously detected. However, as MC congeners are known to differ in their toxicity, methods are needed that simultaneously quantify the congeners present, thus allowing for summary hazard and risk assessment. Moreover, detection of MCs should be expanded to complex matrices, e.g., blood and tissue samples, to verify in situ MC concentrations, thus providing for improved exposure assessment and hazard interpretation. To achieve this, we applied two synthetic deuterated MC standards and optimised the tissue extraction protocol for the simultaneous detection of 14 MC congeners in a single ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) run. This procedure was validated using plasma and liver homogenates of mice (male and female) spiked with deuterated MC standards. For proof of concept, tissue and plasma samples from mice i.p. injected with MC-LR and MC-LF were analysed. While MC-LF was detected in all tissue samples of both sexes, detection of MC-LR was restricted to liver samples of male mice, suggesting different toxicokinetics in males, e.g., transport, conjugation or protein binding. Thus, deconjugation/-proteinisation steps should be employed to improve detection of bound MC. View Full-Text
Keywords: cyanobacterial toxin; deuterated MC standards; microcystin; blood; liver tissue; UPLC-MS/MS; quantification cyanobacterial toxin; deuterated MC standards; microcystin; blood; liver tissue; UPLC-MS/MS; quantification
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Altaner, S.; Puddick, J.; Fessard, V.; Feurstein, D.; Zemskov, I.; Wittmann, V.; Dietrich, D.R. Simultaneous Detection of 14 Microcystin Congeners from Tissue Samples Using UPLC- ESI-MS/MS and Two Different Deuterated Synthetic Microcystins as Internal Standards. Toxins 2019, 11, 388.

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