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引用本文:吴海燕,陈佳琦,董晨帆,王松,崔海栋,谭志军.UHPLC-LTQ-Orbitrap-MS非定向筛查贝类中氮杂螺环酸毒素及其代谢产物.海洋与湖沼,2020,51(6):1432-1439.
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UHPLC-LTQ-Orbitrap-MS非定向筛查贝类中氮杂螺环酸毒素及其代谢产物
吴海燕,陈佳琦,董晨帆,王松,崔海栋,谭志军
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 青岛 266071;2.上海海洋大学食品学院 上海 201306;3.青岛卫辽医用生物材料有限公司 青岛 266071
摘要:
为了分析复杂贝类和微藻中的氮杂螺环酸毒素(AZAs)及其代谢产物,建立一种基于超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱(UHPLC-LTQ-Orbitrap-MS)联用技术的非定向筛查分析方法。采用Full MS/dd MS2、PRM和Target-SIM/dd MS2三种质谱鉴定模式,整合多种数据采集挖掘策略,通过研究多种AZAs在不同基质样品中的质谱裂解规律及特征碎片离子丰度,实现AZAs及其衍生物的快速筛查检测和精准鉴别。结果表明:PRM模式能有效排除AZAs同分异构体的干扰,获得更高的专属性,适用于目标代谢物筛查;应用Full MS/dd MS2和PRM结合的方式,根据AZAs裂解途径及多种AZAs代谢产物裂解规律,在贝类中共鉴别出20种AZAs系列化合物,其中包括初步推测了3种新型AZAs代谢产物的结构。应用本方法还发现AZA9、AZA10、AZA19等代谢物均随代谢过程持续升高,是AZA2在贝类代谢过程中的末端产物。该方法能够为复杂基质中的AZAs系列毒素及其衍生常规检测与精准鉴别提供参考,可应用于解析AZAs毒素在贝类体内的代谢转化机制研究。
关键词:  氮杂螺环酸毒素  贝类  高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱  代谢
DOI:10.11693/hyhz20200300057
分类号:O656.22
基金项目:国家重点研发计划资助,2017YFF0211103号;国家自然科学基金,41806138号。
UNTRAGETED SCREENING OF AZASPIRACIDS AND ITS METABOLITES IN SHELLFISH AND TOXIN PRODUCING ALGAE BY UHPLC-LTQ-ORBITRAP
WU Hai-Yan1,2, CHEN Jia-Qi1,2, DONG Chen-Fan1,2,3, WANG Song4,5, CUI Hai-Dong4,5, TAN Zhi-Jun1,2
1.Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture;2.Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China;3.College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China;4.Qingdao Value&5.Value Medical Biomaterial Co., Ltd, Qingdao 266071, China
Abstract:
Azaspiracids (AZAs), one kind of lipid-soluble shellfish toxins, with the lowest provisional acute reference dose (ARfD) and relative high toxicity among all kinds of shellfish toxins, are easily accumulated to high levels in shellfish and can persist for long periods. Consumption of AZAs contaminated shellfish could cause severe acute gastrointestinal poisoning, posing threats to public health, and concerns on quality of shellfish products. In recent years, AZAs contamination has become a worldwide problem. AZAs producing microalgae are extensively distributed around the coasts of China, resulting in increased AZAs accumulation in shellfish. It is therefore necessary to assess the potential risk of AZAs in shellfish. However, the mechanism for AZAs detoxification in human remains poorly documented, and often generates inaccurate safety assessments. In this study, ultra-high-performance liquid chromatography linear ion trap/orbitrap high-resolution mass spectrometry (UHPLC-LTQ-Orbitrap) was used to integrate the untargeted screening analysis method of AZAs and its metabolites in shellfish. The mass spectrum characterization of AZA standard solution and positive matrix samples was analyzed for routine detection and accurate identification in three identification modes: Full MS/dd MS2, PRM, and target-SIM /dd MS2. The results show that PRM could effectively eliminate the interference of isomers and obtain higher specificity. Non-target high-throughput screening analysis by Full MS/dd MS2 and the PRM were conducted for metabolic samples. Twenty AZA species and three new AZA metabolites were identified from various samples. Therefore, this method can provide a reference for accurate routine detection of AZAs in complex matrixes and for studying the metabolic transformation mechanism.
Key words:  azaspiracid  shellfish toxin  ultra-high-performance liquid chromatography linear ion trap/orbitrap high-resolution mass spectrometry (UHPLC-LTQ-Orbitrap)  metabolite
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