Liquid Chromatography/Mass Spectrometry of Domoic Acid and Lipophilic Shellfish Toxins with Selected Reaction Monitoring and Optional Confirmation by Library Searching of Product Ion Spectra
Liquid Chromatography/Mass Spectrometry of Domoic Acid and Lipophilic Shellfish Toxins with Selected Reaction Monitoring and Optional Confirmation by Library Searching of Product Ion Spectra
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DOI：
10.5740/jaoacint.sgemccarron
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发表时间：
2014-03-01
影响因子：
1.6
通讯作者：
Quilliam, Michael A.
中科院分区：
文献类型：
--
作者：
McCarron, Pearse;Wright, Elliott;Quilliam, Michael A.
建立了一种三重四极线性离子阱质谱联用分析贝类中软骨藻酸和亲脂毒素的LC/MS方法。建立并验证了软骨藻酸、冈田酸、甲藻毒素、氮唑酸、果仁毒素、叶豆毒素、裸子二胺、螺内酯和品纳毒素的常规定量分析方法。该方法具有良好的检出限、线性度、精密度和准确度。利用仪器的高灵敏度，通过减少引入质谱仪的样品量来减轻基质效应。可选地，样品可以使用信息依赖采集（IDA）方法进行分析，无论是在正模式还是负模式下，都可以通过将样品获得的全部产物离子光谱与专门构建的光谱库中的光谱相匹配来提供额外的确认级别。采用方法对2011年腹泻性贝类中毒（DSP）事件中涉及的一种新的认证标准物质和加拿大贻贝（Mytilus edulis）进行了分析。预定的SRM方法可以筛选和定量多种藻毒素。由于此前在加拿大该地区未观察到DSP，因此使用IDA和光谱搜索方法完成了对假定毒素的阳性鉴定。对2011年有毒贻贝样本的分析显示，存在高水平的甲藻毒素-1，这解释了DSP症状，以及pectenotoxins， yessotoxins和各种环亚胺。
LC/MS methodology for the analysis of domoic acid and lipophilic toxins in shellfish was developed using a hybrid triple quadrupole linear ion trap mass spectrometer. For routine quantitation a scheduled selected reaction monitoring (SRM) method for the analysis of domoic acid, okadaic acid, dinophysistoxins, azaspiracids, pectenotoxins, yessotoxins, gymnodimines, spirolides, and pinnatoxins was developed and validated. The method performed well in terms of LOD, linearity, precision, and trueness. Taking advantage of the high instrument sensitivity, matrix effects were mitigated by reducing the amount of sample introduced to the mass spectrometer. Optionally, samples can be analyzed using information dependent acquisition (IDA) methods, either in positive or negative mode, which can provide an extra level of confirmation by matching the full product ion spectra acquired for a sample with those from a specially constructed spectral library. Methods were applied to the analysis of a new certified reference material and Canadian mussels (Mytilus edulis) implicated in a 2011 diarrhetic shellfish poisoning (DSP) incident. The scheduled SRM method enabled the screening and quantitation of multiple phycotoxins. As DSP had not previously been observed in this area of Canada, positive identification of putative toxins was accomplished using the IDA and spectral search method. Analysis of the 2011 toxic mussel samples revealed the presence of high levels of dinophysistoxin-1, which explained the DSP symptoms, as well as pectenotoxins, yessotoxins, and variety of cyclic imines.