Determination of azaspiracids in shellfish using liquid chromatography/tandem electrospray mass spectrometry

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Abstract
Azaspiracid (AZA1), a recently discovered marine toxin, is responsible for the new human toxic syndrome, azaspiracid poisoning (AZP), which is caused by the consumption of contaminated shellfish. A new, sensitive liquid chromatography/mass spectrometry (LC/MS) method has been developed for the determination of AZA1 and its analogues, 8‐methylazaspiracid (AZA2) and 22‐demethylazaspiracid (AZA3). Separation of these toxins was achieved using reversed‐phase LC and coupled, via an electrospray ionisation (ESI) source, to an ion‐trap mass spectrometer. Spectra showed the protonated molecules, [M + H]+, and their major product ions, due to the sequential loss of two water molecules, [M + H − H2O]+, [M + H − 2H2O]+, in addition to fragment ions that are characteristic of these cyclic polyethers. A highly specific and sensitive LC/MS3 analytical method was developed and, using shellfish extracts containing AZA1, the detection limit (S/N = 3) was 4 pg on‐column, corresponding to 0.8 ng/mL. Using the protocol presented here, this is equivalent to 0.37 ng/g shellfish tissue and good linear calibrations were obtained for AZA1 in shellfish extracts (average r2 = 0.9988). Good reproducibility was achieved with % RSD values (N = 5) ranging from 1.5% (0.75 µg/mL) to 4.2% (0.05 µg/mL). An efficient procedure for the extraction of toxins from shellfish aided the development of a rapid protocol for the determination of the three predominant azaspiracids. Copyright © 2002 John Wiley & Sons, Ltd.
Funding Information
  • Enterprise Ireland
  • The Higher Education Authority, Ireland

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