Direct identification of yessotoxin in shellfish by liquid chromatography coupled with mass spectrometry and tandem mass spectrometry

✍ Scribed by Rosa Draisci; Luigi Giannetti; Luca Lucentini; Emanuele Ferretti; Luca Palleschi; Camilla Marchiafava

• Publisher: John Wiley and Sons
• Year: 1998
• Tongue: English
• Weight: 145 KB
• Volume: 12
• Category: Article
• ISSN: 0951-4198
• DOI: 10.1002/(sici)1097-0231(19981015)12:19<1291::aid-rcm314>3.0.co;2-y

✦ Synopsis

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 [MÀ2NaH] À , the ion at m/z 1163, assigned to the [MÀNa] À and a signal at m/z 1185, due to the deprotonated molecule [MÀH] À 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 mL/min, with a mobile phase of acetonitrile-ammonium acetate 4 mM, 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.