Liquid chromatography/mass spectrometry of domoic acid and lipophilic shellfish toxins with selected reaction monitoring and optional confirmation by library searching of product ion spectra

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DOIResolve DOI: http://doi.org/10.5740/jaoacint.SGEMcCarron
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TypeArticle
Journal titleJournal of AOAC International
ISSN1060-3271
Volume97
Issue2
Pages316324; # of pages: 9
SubjectMass spectrometers; Mass spectrometry; Metabolites; Molluscs; Shellfish; Certified reference materials; Diarrhetic shellfish poisoning; Hybrid triple quadrupole-linear ion trap mass spectrometer; Information-dependent acquisitions; Liquid chromatography/mass spectrometry; Product ion spectra; Selected reaction monitoring; Spectral libraries; Toxic materials; domoic acid; drug derivative; kainic acid; lipid; marine toxin; animal; article; chemistry; food analysis; liquid chromatography; mass spectrometry; methodology; molecular library; reproducibility; shellfish; Animals; Chromatography, Liquid; Food Analysis; Kainic Acid; Lipids; Marine Toxins; Mass Spectrometry; Reproducibility of Results; Shellfish; Small Molecule Libraries
AbstractLC/MS methodology for the analysis of domoic acid and lipophilic toxins in shellfish was developed using a hybrid triple quadrupole linear ion trap mass spectrometer. For routine quantitation a scheduled selected reaction monitoring (SRM) method for the analysis of domoic acid, okadaic acid, dinophysistoxins, azaspiracids, pectenotoxins, yessotoxins, gymnodimines, spirolides, and pinnatoxins was developed and validated. The method performed well in terms of LOD, linearity, precision, and trueness. Taking advantage of the high instrument sensitivity, matrix effects were mitigated by reducing the amount of sample introduced to the mass spectrometer. Optionally, samples can be analyzed using information dependent acquisition (IDA) methods, either in positive or negative mode, which can provide an extra level of confirmation by matching the full product ion spectra acquired for a sample with those from a specially constructed spectral library. Methods were applied to the analysis of a new certified reference material and Canadian mussels (Mytilus edulis) implicated in a 2011 diarrhetic shellfish poisoning (DSP) incident. The scheduled SRM method enabled the screening and quantitation of multiple phycotoxins. As DSP had not previously been observed in this area of Canada, positive identification of putative toxins was accomplished using the IDA and spectral search method. Analysis of the 2011 toxic mussel samples revealed the presence of high levels of dinophysistoxin-1, which explained the DSP symptoms, as well as pectenotoxins, yessotoxins, and variety of cyclic imines. © 2014 Publishing Technology.
Publication date
LanguageEnglish
AffiliationNational Research Council Canada (NRC-CNRC); Measurement Science and Standards (MSS-SME)
Peer reviewedYes
NPARC number21272136
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Record identifier6312ac31-c2d7-4ce3-99f3-7e376f242881
Record created2014-07-23
Record modified2016-05-09
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