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Direct identification of yessotoxin in shellfish by liquid chromatography coupled with mass spectrometry and tandem mass spectrometry
Author(s) -
Draisci Rosa,
Giannetti Luigi,
Lucentini Luca,
Ferretti Emanuele,
Palleschi Luca,
Marchiafava Camilla
Publication year - 1998
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/(sici)1097-0231(19981015)12:19<1291::aid-rcm314>3.0.co;2-y
Subject(s) - chemistry , mass spectrometry , chromatography , tandem mass spectrometry , liquid chromatography–mass spectrometry , analyte , selected reaction monitoring , analytical chemistry (journal)
A new method for the direct identification of yessotoxin (YTX), a polyether compound belonging to the diarrhoeic shellfish poisoning (DSP) toxins, using liquid chromatography coupled with mass spectrometry and tandem mass spectrometry (LC/MS and LC/MS/MS) is reported. Full‐scan ionspray mass spectra of YTX, as acquired in single MS negative ion mode by flow injection analysis (FIA), showed the most intense ion at m/z 1141, assigned to the [M−2Na+H] − , the ion at m/z 1163, assigned to the [M−Na] − and a signal at m/z 1185, due to the deprotonated molecule [M−H] − of the analyte taken here to be the disodium salt. Collision induced dissociation of the precursor ion at m/z 1141, as obtained by FIA negative tandem mass spectrometry experiments, showed the most intense fragment ions in the higher mass region, at m/z 1061, m/z 924, m/z 855, m/z 713, which are characteristic of the structure of the analyte. Ionspray reversed phase LC/MS and LC/MS/MS was performed by isocratic elution at 30 μL/min, with a mobile phase of acetonitrile–ammonium acetate 4 m M , 80:20 (v/v), using a 1.0 mm i.d. C 18 column. The detection of YTX in Italian shellfish samples collected in 1997 from the Adriatic sea was successfully carried out using this method, permitting demonstration of a false negative result obtained by the official mouse bioassay during routine control monitoring. © 1998 John Wiley & Sons, Ltd.