液相色谱-串联质谱法筛查原多甲藻酸毒素及其代谢产物  

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

作　　者：吴海燕[1,2] 郭萌萌[1,2] 赵春霞[1,2] 谭志军[1,2] 顾海峰[3] 翟毓秀[1,2] 卢立娜[1,2] 

机构地区：[1]农业部水产品质量安全检测与评价重点实验室,中国水产科学研究院黄海水产研究所,山东青岛266071 [2]农业部水产品质量安全风险评估实验室(青岛),山东青岛266071 [3]国家海洋局第三研究所,福建厦门361000

出　　处：《色谱》2016年第4期401-406,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(41106109);中央级基本科研业务费项目(20603022011004;20603022015017-2)~~

摘　　要：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 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.

关 键 词：液相色谱-串联质谱法 原多甲藻酸毒素 代谢产物 定性分析 

分 类 号：O658[理学—分析化学]