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Determination of azaspiracids in shellfish using liquid chromatography/tandem electrospray mass spectrometry
Author(s) -
Furey Ambrose,
BrañaMagdalena Ana,
Lehane Mary,
Moroney Cian,
James Kevin J.,
Satake Masayuki,
Yasumoto Takeshi
Publication year - 2002
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.560
Subject(s) - chemistry , chromatography , marine toxin , mass spectrometry , shellfish , electrospray , tandem mass spectrometry , detection limit , ion trap , extraction (chemistry) , liquid chromatography–mass spectrometry , shellfish poisoning , electrospray ionization , selected reaction monitoring , toxin , fish <actinopterygii> , aquatic animal , fishery , biochemistry , biology
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 − H 2 O] + , [M + H − 2H 2 O] + , in addition to fragment ions that are characteristic of these cyclic polyethers. A highly specific and sensitive LC/MS 3 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 r 2 = 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.