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建立了原多甲藻酸毒素( azaspiracids,AZAs)及其代谢产物的液相色谱-串联质谱检测方法,考察了目标代谢产物检测方法和非目标多离子检测方法,将二级质谱图与标准品谱库进行比对,从而获得高精准定性。通过对产毒藻、蓄积代谢实验样品和实际阳性样品综合分析,共检出11种AZAs,其中包括AZA-2,3,6,11,12,16,17,28和36,以及 AZAs的谷胱甘肽结合型代谢产物。结果发现,目标代谢产物检测法可无偏差地筛出常规代谢物,而且对低浓度代谢产物表现出更佳的响应。本方法重现性好,数据分析简单,对操作人员的专业要求不高,更适合 AZAs的监控要求。

A liquid chromatography-tandem mass spectrometry method was developed for the analysis of azaspiracids and their metabolites. Both target metabolites and non-objective com-pounds detection methods were investigated,and the secondary mass spectra were compared with the standard spectra libraries to achieve high precision qualitative analysis. As a result,11 metabolites including AZA-2,3,6,11,12,16,17,28 and 36,as well as the glutathione conju-gated metabolites of AZAs were analyzed in toxin-producing algae,accumulated samples of metabolic experiments and positive samples. Conventional metabolites were unbiased detected by target metabolites detection method,and showed a better response to low concentration metabolites. The method has excellent reproducibility,and is easy for operators. It can be used for the routine monitoring of AZAs.

参考文献

[1] Jauffrais T;Marcaillou C;Herrenknecht C;Truquet P;Sechet V;Nicolau E;Tillmann U;Hess P.Azaspiracid accumulation, detoxification and biotransformation in blue mussels (Mytilus edulis) experimentally fed Azadinium spinosum.[J].Toxicon: An International Journal Devoted to the Exchange of Knowledge on the Poisons Derived from Animals, Plants and Microorganisms,20124(4):582-595.
[2] Jauffrais, T.;Kilcoyne, J.;Herrenknecht, C.;Truquet, P.;Sechet, V.;Miles, C. O.;Hess, P..Dissolved azaspiracids are absorbed and metabolized by blue mussels (Mytilus edulis).[J].Toxicon: An International Journal Devoted to the Exchange of Knowledge on the Poisons Derived from Animals, Plants and Microorganisms,2013:81-89.
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