National Research Council Canada, Institute for Marine Biosciences, Halifax, NS, Canada.
Anal Bioanal Chem. 2011 May;400(3):835-46. doi: 10.1007/s00216-011-4803-z. Epub 2011 Mar 24.
A freeze-dried mussel tissue certified reference material (CRM-FDMT1) containing multiple groups of shellfish toxins has been prepared. Toxin groups present in the material include okadaic acid and the dinophysistoxins, azaspiracids, yessotoxins, pectenotoxins, spirolides and domoic acid. In this work, analytical methods have been examined for the characterisation of the candidate CRM. A comprehensive extraction procedure was developed, which gave good recovery (>98%) for all lipophilic toxins studied. A fast liquid chromatography-mass spectrometry (LC-MS) method was developed that separates the major toxins according to the MS ionisation mode of optimum sensitivity. Matrix effects associated with analysis of these extracts using the developed LC-MS method were assessed. Standard addition and matrix-matched calibration procedures were evaluated to compensate for matrix effects. The methods and approaches will be used for the precise characterisation of the homogeneity and stability of the various toxins in CRM-FDMT1 and for the accurate assignment of certified values. The developed methods also have excellent potential for application in routine regulatory monitoring of shellfish toxins.
已制备一种含有多组贝类毒素的冷冻干燥贻贝组织标准物质（CRM-FDMT1）。该物质中存在的毒素组包括 okadaic 酸和 dinophysistoxins、azaspiracids、yessotoxins、pectenotoxins、spirolides 和 domoic 酸。在这项工作中，对候选 CRM 的特征分析方法进行了检查。开发了一种综合提取程序，该程序对所有研究的亲脂性毒素都具有良好的回收率（>98%）。开发了一种快速液相色谱-质谱（LC-MS）方法，根据最佳灵敏度的 MS 电离模式对主要毒素进行分离。评估了使用开发的 LC-MS 方法分析这些提取物时与基质相关的影响。评估了标准添加和基质匹配校准程序，以补偿基质效应。这些方法和方法将用于精确表征 CRM-FDMT1 中各种毒素的均一性和稳定性，并准确赋值认证值。开发的方法还具有在贝类毒素常规监管监测中应用的巨大潜力。
