Development of a method for the identification of azaspiracid in shellfish by liquid chromatography-tandem mass spectrometry

被引:48
作者
Draisci, R
Palleschi, L
Ferretti, E
Furey, A
James, KJ
Satake, M
Yasumoto, T
机构
[1] Ist Super Sanita, Med Vet Lab, I-00161 Rome, Italy
[2] Cork Inst Technol, Dept Chem, Ecotoxicol Res Unit, Bishoptown, Cork, Ireland
[3] Tohoku Univ, Fac Agr, Aoba Ku, Sendai, Miyagi 9818555, Japan
[4] Japan Food Labs, Tama Lab, Tokyo 2060025, Japan
关键词
shellfish poisoning; food analysis; azaspiracid; toxins;
D O I
10.1016/S0021-9673(99)01023-7
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Azaspiracid is the main toxin responsible for a number of recent human intoxications in Europe resulting from shellfish consumption. The first micro liquid chromatography-tandem mass spectrometry (micro-LC-MS-MS) method was developed for the determination of this novel shellfish poisoning toxin in mussels. The analyte was extracted from whole mussel meat with acetone and chromatographed on a C-18 reversed-phase column (1.0 mm I.D.) by isocratic elution at 30 mu l/min with acetonitrile-water (85:15, v/v), containing 0.03% trifluoroacetic acid. The toxin was ionised in an ionspray interface operating in the positive ion mode, where only the intact protonated molecule, [M+H](+), was generated at m/z 842. This served as precursor ion for collision-induced dissociation and three product ions, [M+H-nH(2)O](+) with n=1-3, were identified for the unambiguous toxin confirmation by selected reaction monitoring LC-MS-MS analysis. A detection limit of 20 pg, based on a 3:1 signal-to-noise ratio, was achieved for the analyte. This LC-MS-MS method was successfully applied to determine azaspiracid in toxic cultivated shellfish from two regions of Ireland. (C) 2000 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:13 / 21
页数:9
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