Screening for cyanobacterial hepatotoxins, microcystins and nodularin in environmental water samples by reversed-phase liquid chromatography- electrospray ionisation mass spectrometry

Lisa Spoof, Pia Vesterkvist, Tore Lindholm, Jussi Meriluoto*

*Corresponding author for this work

Research output: Contribution to journalArticleScientificpeer-review

164 Citations (Scopus)

Abstract

Water samples taken from 93 freshwater and brackish water locations in Åland (SW Finland) in 2001 were analysed for biomass-bound microcystins and nodularin, cyanobacterial peptide hepatotoxins, by liquid chromatography-mass spectrometry (LC-MS) in selected ion recording (SIR) and multiple reaction monitoring modes, HPLC-UV, and enzyme-linked immunosorbent assay (ELISA). The extracted toxins were separated on a short C18 column with a gradient of acetonitrile and 0.5% formic acid, and quantified on a Micromass Quattro Micro triple-quadrupole mass spectrometer with an electrospray ion source operated in the positive SIR or scan mode. An injection of 50 pg of microcystin-LR, m/z 995.5, on column gave a signal-to-noise ratio of 17 (peak-to-peak) at the chosen SIR conditions. In-source or MS-MS fragmentation to m/z 135.1, a fragment common to most microcystins and nodularin, was used for confirmatory purposes. Microcystins with a total toxin concentration equal to or higher than 0.2 μg l-1 were confirmed by all three methods in water samples from 14 locations. The highest toxin concentration in a water sample was 42 μg l-1. The most common toxins found were microcystins RR, LR and YR with different degrees of demethylation (non-, mono- or didemethylated). Parallel results achieved with ELISA and HPLC-UV were generally in good agreement with the LC-MS SIR results.

Original languageEnglish
Pages (from-to)105-119
Number of pages15
JournalJournal of Chromatography A
Volume1020
Issue number1
DOIs
Publication statusPublished - 5 Dec 2003
MoE publication typeA1 Journal article-refereed

Keywords

  • Bacteria
  • Environmental analysis
  • Hepatotoxins
  • Microcystins
  • Nodularin
  • Toxins
  • Water analysis

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