Chromatography

Liquid chromatography tandem mass spectrometry (LC-MS) was carried out with a Shimadzu Prominence HPLC system and SCIEX 6500 mass spectrometer. An aliquot of 10 µl of each sample was injected onto an Luna 3 µm Phenyl-hexyl 100 x 2.0 mm column at 50^oC for gradient separation. Mobile phases were: A, ddH₂O with 0.1% Formic Acid; and B, Acetonitrile with 0.1% Formic Acid. Gradient schedule starts at 10% B and is linearly increased to 95% B at 3 minutes, then held at 95% B until 3.2 minutes, and then returned to 10% B at 3.4 at minutes and re-equilibration until 5 minutes. Time per sample injection was 5 minutes with a flow rate is 500 µL/min.

Extraction Protocols:

Extraction protocols for sample processing are dependent on the matrices involved. Please see extraction methods section for more specific instructions.

References

Method derived from the following

[1] Liquid Chromatography/Mass Spectrometry of Domoic Acid and Lipophilic Shellfish Toxins with Selected Reaction Monitoring and Optional Confirmation by Library Searching of Product Ion SpectraPearse Mccarron, elliott Wright, and Michael a. QuilliaMNational Research Council of Canada, Biotoxin Metrology, Measurement Science and Standards, 1411 Oxford St, Halifax, Nova Scotia B3H 3Z1, Canada

Resources

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