液相色谱-串联质谱法筛查原多甲藻酸毒素及其代谢产物

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。

Liquid chromatography-tandem mass spectrometry analysis for azaspiracids and their metabolites

A liquid chromatography-tandem mass spectrometry method was developed for the analysis of azaspiracids and their metabolites. Both target metabolites and non-objective compounds 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 conjugated 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.