| 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 |
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| 引用本文： | 方力,吴凡,邱凤梅,余新威,朱严华. 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[J]. 卫生研究, 2021, 0(1): 116-120,142 |
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| 作者姓名： | 方力 吴凡 邱凤梅 余新威 朱严华 |
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| 作者单位： | 浙江省海产品健康危害因素关键技术研究重点实验室;皖南医学院检验学院;岱山县疾病预防控制中心;浙江海洋大学食品与医药学院 |
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| 基金项目： | 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)。 |
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| 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0.22 μm 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...
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| 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 |
Determination of domoic acid in shellfish by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction |
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| Fang Li,Wu Fan,Qiu Fengmei,Yu Xinwei,Zhu Yanhua. Determination of domoic acid in shellfish by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction[J]. Journal of hygiene research, 2021, 0(1): 116-120,142 |
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| Authors: | Fang Li Wu Fan Qiu Fengmei Yu Xinwei Zhu Yanhua |
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| Affiliation: | (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) |
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| Abstract: | 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. |
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| Keywords: | dispersive solid phase extraction shellfish domoic acid amnesic shellfish poisoning liquid chromatography-tandem mass spectrometry |
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