分散固相萃取净化-液相色谱-串联质谱法检测贝类中软骨藻酸  

Determination of domoic acid in shellfish by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction

作　　者：方力[1] 吴凡 邱凤梅[3] 余新威[1] 朱严华 Fang Li;Wu Fan;Qiu Fengmei;Yu Xinwei;Zhu Yanhua(Key Laboratory of Health Risk Factors for Seafood of Zhejiang Province,Zhoushan Municipal Center for Disease Control and Prevention,Zhoushan 316021,China;Wannan Medical College,School of Laboratory Medicine,Wuhu 241002,China;Daishan Center for Disease Control and Prevention,Zhoushan 316200,China;School of Food and Pharmacy,Zhejiang Ocean University,Zhoushan 316022,China)

机构地区：[1]浙江省海产品健康危害因素关键技术研究重点实验室,舟山市疾病预防控制中心,舟山316021 [2]皖南医学院检验学院,芜湖241002 [3]岱山县疾病预防控制中心,舟山316200 [4]浙江海洋大学食品与医药学院,舟山316022

出　　处：《卫生研究》2021年第1期116-120,142,共6页Journal of Hygiene Research

基　　金：舟山市医药卫生科技计划项目(No.2020YA01);舟山市公益类科技计划项目(No.2021C31071)。

摘　　要：目的建立分散固相萃取净化-液相色谱串联质谱定量检测4种贝类基质中软骨藻酸的方法。方法0.1 g样品用25%甲醇水溶液提取后,用50 mg HLB和5 mg GCB吸附剂吸附净化,过0.22μm PTFE滤膜,C18柱分离(100 mm×2.1 mm,1.9μm),电喷雾离子化,选择反应监测模式检测,基质匹配外标法定量。结果在1.0~50.0 ng/mL浓度范围内,软骨藻酸呈现良好的线性关系,相关系数≥0.9994;以3倍基线噪声所对应的浓度为检出限,方法检出限为5μg/kg;在20、50和100μg/kg的加标水平时,方法的日内和日间回收率分别为91.6%~109.2%和90.9%~109.3%,日内与日间相对标准偏差均<8.2%。结论该检测方法准确、快速、成本低、易操作,能满足贝类食品中软骨藻酸的公共卫生应急检测或日常监测要求。OBJECTIVE A method utilizing liquid chromatography-tandem mass spectrometry(LC-MS/MS)coupled with dispersive solid phase extraction for quantitative analysis of domoic acid in four kinds of shellfish was established.METHODS The sample of 0.1 g was extracted with 25% methanol aqueous solution,the extract was purified by dispersive solid phase extraction with 50 mg HLB and 5 mg GCB,and then filtered through a PTFE membrane.The analytes were separated on a C18 column(100 mm×2.1 mm,1.9μm),and detected in selected reaction monitoring(SRM)mode via positive electrospray ionization.The matrix matching and external standard method was used for quantitation.RESULTS Domoic acid showed good linearity in the concentration range between 1.0 ng/mL and 50.0 ng/mL with correlation coefficients higher than 0.9994.The detection limits of domoic acid in shellfish was 5μg/kg.The inter-and intra-day recoveries were 91.6%-109.2% and 90.9%-109.3%,respectively.The inter-and intra-day ralitive standard deviations(RSDs)were lower than 8.2% at spiked concentrations of 20,50 and 100μg/kg.CONCLUSION The method is accurate,fast,easy to operate,which can satisfy the requirements of public health emergency testing or routine testing.

关 键 词：分散固相萃取 贝类 软骨藻酸 失忆性贝类毒素 液相色谱-串联质谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学] R155.51[轻工技术与工程—食品科学与工程]