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液相色谱-串联质谱法测定虾夷扇贝和长牡蛎中软骨藻酸的残留
引用本文:陈燕清,陈舜胜,于慧娟,蔡友琼,惠芸华.液相色谱-串联质谱法测定虾夷扇贝和长牡蛎中软骨藻酸的残留[J].分析试验室,2010,29(12).
作者姓名:陈燕清  陈舜胜  于慧娟  蔡友琼  惠芸华
作者单位:1. 上海海洋大学食品学院,上海,201306
2. 农业部水产品质量监督检验测试中心,上海,200090
基金项目:农业部标准制修订项目(11273)资助
摘    要:建立了液相色谱-串联质谱测定虾夷扇贝和长牡蛎中贝类毒素软骨藻酸残留的检测方法。样品经50%甲醇提取,LC-SAX柱净化,3mL0.1mol/L甲酸溶液洗脱,电喷雾离子源(ESI),在正离子、多反应监测方式(MRM)模式下进行定性与定量,定性离子对为m/z 311.98/265.91,m/z 311.98/247.9,m/z 311.98/192.91,以m/z 311.98/265.91为定量离子对,外标法定量。结果表明,方法的检测限为0.01μg/g,定量限为0.02μg/g。在0.02~10μg/mL范围内线性相关系数为0.9999。当添加软骨藻酸质量分数为20~1000 ng/g时,虾夷扇贝样品中软骨藻酸的平均回收率为81.3%~105.4%,RSD为3.9%~8.9%(n=6);长牡蛎样品中软骨藻酸的平均回收率为83.5%~106.6%,RSD为4.6%~6.4%(n=6)。方法满足对贝类产品中软骨藻酸残留的测定。

关 键 词:虾夷扇贝  长牡蛎  软骨藻酸  液相色谱串联质谱  多反应监测  

The determination of residue of domoic acid by high performance liquid chromatography-tandem mass spectrometry in patinopecten yessoensis and crassostrea gigas
CHEN Yan-qing,CHEN Shun-sheng,YU Hui-juan,CAI You-qiong,HUI Yun-hua.The determination of residue of domoic acid by high performance liquid chromatography-tandem mass spectrometry in patinopecten yessoensis and crassostrea gigas[J].Chinese Journal of Analysis Laboratory,2010,29(12).
Authors:CHEN Yan-qing  CHEN Shun-sheng  YU Hui-juan  CAI You-qiong  HUI Yun-hua
Institution:CHEN Yan-qing1,CHEN Shun-sheng1,YU Hui-juan2,CAI You-qiong2 and HUI Yun-hua2(1.College of Food Science,Shanghai Ocean University,Shanghai 201306,2.Ministry of Agriculture Supervision and Testing Center for Aquatic Products,Shanghai 200090)
Abstract:In this study,a high-performance liquid chromatography-tandem mass spectrometric method was established for the determination of residue of domoic acid in shellfish.The sample was extracted by 50% methanol,purified on a LC-SAX column,eluted with 3mL of 0.1 mol/L formic acid,and qualitatively and quantitatively determined by electrospray ionization(ESI) ion source,in the positive ion,multiple reaction monitoring mode(MRM),qualitative ion pairs of m/z 311.98/265.91,m/z 311.98/247.9,m/z 311.98/192.91,and m/z 3...
Keywords:Patinopecten yessoensis  Crassostrea gigas  domoic acid  high-performance liquid chromatography-tandem mass spectrometry  multiple reaction monitoring  
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