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  

The determination of residue of domoic acid by high performance liquid chromatography-tandem mass spectrometry in patinopecten yessoensis and crassostrea gigas

作　　者：陈燕清[1] 陈舜胜[1] 于慧娟[2] 蔡友琼[2] 惠芸华[2] 

机构地区：[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

出　　处：《分析试验室》2010年第12期21-24,共4页Chinese Journal of Analysis Laboratory

基　　金：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。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 311.98/265.91 also for quantitative ion,with external standard method.The result showed that the limit of detection（LOD） and quantitation（LOQ） were 0.01μg/g and 0.02μg/g.The calibration curves showed good linearity for DA in the ranges of 20～10 μg/mL,and the correlative coefficient was 0.9999.At spiked level of 20～1000 ng/g for DA,average recoveries of DA in the Patinopecten yessonensis samples were 81.3%～105.4%,and RSDs were 3.9%～8.9%（n=6）;average recoveries of DA in the Crassostrea gigas samples were 83.5%～106.6%,and RSDs were 4.6%～6.4%（n=6）.The method was reliable and sensitive for the determination of domoic acid residue in shellfish.

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 

分 类 号：O657.63[理学—分析化学]