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Project Code [2002-PHD2-30]

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Project title

The Development of Liquid Chromatography-Mass Spectrometry (LC-MS) Methods for the Determination of Microcystins in Irish Freshwaters, Cyanobacteria and Drinking Water.

Primary Funding Agency

Environmental Protection Agency

Co-Funding Organisation(s)

n/a

Lead Organisation

Cork Institute of Technology (CIT)

Lead Applicant

Ambrose Furey

Project Abstract

Microcystins toxic cyclic heptapeptides and nodularin-R a toxic cyclic pentapeptide were determined using liquidchromatography (LC) with detection using photo-diode array ultra-violet (PDA-UV) and protein phosphatase (PP)assay. Positive fractions were analysed for toxins using collision-induced dissociation (CID) and tandem MS/MSexperiments which were carried out simultaneously using electrospray ion-trap instrumentation. Reversed-phase liquidchromatography (LC) using an acetonitrile/water gradient was used for the LC-MS2 determination of six microcystinsstandards and nodularin. The molecular related ion species [M+H]([M +2H]2 in the case of MC-RR) were used asthe precursor ions for MS2 experiments. Optimum calibration and reproducibility data were obtained for MC-LR usingLC-MS2; 0.1i-5.0 lg/ml r2 i? 0:992 (n i? 3); % RSD 6 7.3 at 0.25 lg MC-LR/ml (n i? 3). The detection limit (S=N i? 3)was better than 0.1 ng. Water samples for microcystin analysis were first screened using protein phosphatase (PP) assaysand positives were concentrated using C-18 solid-phase extraction. The developed method was applied to examine alake in Ireland contaminated by Microcystis sp. and MC-LR and MC-LA were identified.

Grant Approved

�75,000.00

Research Hub

Healthy Environment

Research Theme

Impacts on Aquatic Ecosystems & Human Health (including Drinking Water)

Start Date

01/10/2002

Initial Projected Completion Date

n/a