National Research Council Canada, Institute for Marine Biosciences, Halifax, NS, Canada.
Anal Bioanal Chem. 2011 May;400(3):847-58. doi: 10.1007/s00216-011-4787-8. Epub 2011 Mar 6.
A candidate certified reference material (CRM) for multiple shellfish toxins (domoic acid, okadaic acid and dinophysistoxins, pectenotoxins, yessotoxin, azaspiracids and spirolides) has been prepared as a freeze-dried powder from mussel tissues (Mytilus edulis). Along with the certified values, the most important characteristics for a reference material to be fit-for-purpose are homogeneity and stability. Acceptable between-bottle homogeneity was found for this CRM. Within-bottle homogeneity was assessed using domoic acid, and it was shown that repeated subsampling of the CRM can be performed precisely down to 0.35 g. Both short- and long-term stability studies carried out under isochronous conditions demonstrated excellent stability of the various toxins present in the material. While degradation of some analytes was observed at +60°C in short-term studies, it was determined that shipping at ambient temperature is adequate. No instability was detected in long-term stability studies, and it was shown that the material can be held at +18°C safely for up to 1 year. To guarantee stability of the CRM over its lifetime the stock will be maintained at -20°C. The results of the homogeneity and stability testing show that CRM-FDMT1 is appropriate for its intended use in quality assurance and quality control of shellfish toxin analysis methods.
一种贝类毒素（包括软骨藻酸、大田软海绵酸和膝沟藻毒素、扇贝毒素、石房蛤毒素、短裸甲藻毒素和芋螺毒素）候选有证参考物质（CRM）已制备成贻贝组织（贻贝）的冻干粉末。除了有证值外，适合特定用途的参考物质的最重要特性是均一性和稳定性。该 CRM 具有可接受的瓶间均一性。采用软骨藻酸评估了瓶内均一性，结果表明可以精确地重复分取 CRM 至 0.35g。在等时条件下进行的短期和长期稳定性研究均表明，该材料中存在的各种毒素具有极好的稳定性。虽然在短期研究中观察到一些分析物在+60°C 时发生降解，但结果表明在环境温度下运输是足够的。在长期稳定性研究中未检测到不稳定现象，表明在+18°C 下该材料可安全保存长达 1 年。为了保证 CRM 在其整个寿命期间的稳定性，库存将保持在-20°C。均一性和稳定性测试的结果表明，CRM-FDMT1 适合用于贝类毒素分析方法的质量保证和质量控制。
