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当前位置: 首页 > 文章 > 液相色谱-高分辨质谱测定贝类中虾夷扇贝毒素 安徽农业科学 2020 (9) 208-209+216
Position: Home > Articles > Determination of Yessotoxins in Shellfish by Liquid Chromatography-High Resolution Mass Spectrometry Journal of Anhui Agricultural Sciences 2020 (9) 208-209+216

液相色谱-高分辨质谱测定贝类中虾夷扇贝毒素

作  者：
吴祥庆;杨姝丽;余焘;吴明媛;黄鸾玉;黄国秋
单  位：
广西壮族自治区水产科学研究院
关键词：
贝类毒素;虾夷扇贝毒素;液相色谱-高分辨质谱
摘  要：
[目的]建立贝类产品中虾夷扇贝毒素(YTX)的液相色谱-四极杆-静电轨道场离子阱高分辨质谱检测方法。[方法]以牡蛎和文蛤为研究对象,样品经甲醇提取,采用QuEChERS净化,经Hypersil GOLD C_(18)色谱柱分离,乙腈和0.002 mol/L甲酸铵溶液(含0.2%甲酸)为流动相梯度洗脱,负离子全扫描+数据依赖二级扫描,提取一级谱图中准分子离子精确质量数定量,二级质谱图中特征离子精确质量数定性。[结果]虾夷扇贝毒素(YTX)在12 min内出峰,定量限为0.3μg/kg,在9.05～181.00μg/L范围内线性良好,相关系数r=0.996 4,回收率96.3%～102.8%,相对标准偏差(RSD)小于14.2%(n=6)。[结论]该研究为贝类毒素监控提供了技术支持。
译  名：
Determination of Yessotoxins in Shellfish by Liquid Chromatography-High Resolution Mass Spectrometry
作  者：
WU Xiang-qing;YANG Shu-li;YU Tao;Guangxi Academy of Fishery Sciences;Soil and Fertilizer Working Station of Guangxi Zhuang Autonomous Region;
关键词：
Shelfish toxin;;Yessotoxins(YTX);;Liquid chromatography-high resolution mass spectrometry
摘  要：
[Objective]The research aimed to establish a method for the simultaneous determination of Yessotoxins(YTX) in shellfish by liquid chromatography-quadrupole-orbitrap mass spectrometry.[Method]Oyster and clam samples were extracted with methanol and purified with QuEChERS technology.The analytes were isolated by Hypersil GOLD C_(18) column and gradient eluted with acetonitrile-0.002 mol/L ammonium formate solution(0.1% formic acid).YTX were determined by orbitrap mass spectrometry through negative ion scanning, full scan mode and data dependent scan mode.[Result]The retention time of YTX was all within 12 min.The limits of quantification(LOQ) was 0.3 μg/kg.The calibration curves showed good linearity within the concentration range of 9.05-181.00 μg/L,r=0.996 4;the average recovery rate was 96.3%-102.8% and the relative standard deviations(RSD) were less than 14.2%(n=6).[Conclusion] The study provides technical support for the monitoring of shellfish toxins.

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