色谱

色谱 ›› 2016, Vol. 34 ›› Issue (4): 401-406.DOI: 10.3724/SP.J.1123.2015.11043

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法筛查原多甲藻酸毒素及其代谢产物

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   

  1. 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
  • 收稿日期:2015-11-26 出版日期:2016-04-08 发布日期:2012-11-16
  • 通讯作者: 谭志军
  • 基金资助:

    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).

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

WU Haiyan1,2, GUO Mengmeng1,2, ZHAO Chunxia1,2, TAN Zhijun1,2, GU Haifeng3, ZHAI Yuxiu1,2, LU Lina1,2   

  1. 1. Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture, China;Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China;
    2. Laboratory of Quality & Safety Risk Assessment for Aquatic Products(Qingdao), Ministry of Agriculture, Qingdao 266071, China;
    3. Third Institute of Oceanography, State Oceanic Administration, Xiamen 361000, China
  • Received:2015-11-26 Online:2016-04-08 Published:2012-11-16
  • Supported by:

    National Natural Science Foundation of China (No. 41106109);Special Funds for the Basic R & D Program in the Central Non-Profit Research Institutes (Nos. 20603022011004, 20603022015017-2).

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被引次数

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。

关键词: 代谢产物, 定性分析, 液相色谱-串联质谱法, 原多甲藻酸毒素

Abstract:

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.

Key words: azaspiracids (AZAs), liquid chromatography-tandem mass spectrometry (LC-MS/MS), metabolites, qualitative analysis

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