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液相色谱-串联质谱检测贝类组织中5种脂溶性贝毒素
引用本文:姚建华,谭志军,周德庆.液相色谱-串联质谱检测贝类组织中5种脂溶性贝毒素[J].分析化学,2010,38(12).
作者姓名:姚建华  谭志军  周德庆
作者单位:中国水产科学研究院黄海水产研究所;上海海洋大学食品学院;
基金项目:国家863计划,国家科技支撑计划项目
摘    要:建立了液相色谱-串联质谱分析贝类组织中米氏裸甲藻(GYM)贝毒素、螺环内酯毒素(SPX1)、大田软骨酸(OA)贝毒素、蛤毒素(PTX2)、原多甲藻酸(AZA1)贝毒素的方法.用甲醇-水(4: 1, V/V)溶液对贝类组织中GYM, SPX1, OA, PTX2和AZA1进行提取,MAX阴离子交换柱净化后,采用液相色谱分离,除OA以负离子选择反应监测外,GYM, SPX1, PTX2和AZA1以电喷雾离子源正离子选择反应监测模式进行质谱分析.5种脂溶性贝毒素GYM, SPX1, OA, PTX2和AZA1在各自相应浓度范围内线性良好,相关系数>0.99.扇贝闭壳肌空白样品添加5种贝毒素的提取率均为78.6%~94.4%(n=6); 精密度(RSD)为6.8%~14.9%.贝类组织中5种贝毒素GYM, SPX1, OA, PTX2和AZA1的检出限分别为0.10, 0.21, 2.00, 0.32和0.04 μg/kg.

关 键 词:脂溶性贝毒素  贝类组织  液相色谱-串联质谱

Determination of Five Lipophilic Marine Toxins in Shellfish by Liquid Chromatography with Tandem Mass Spectrometry
YAO Jian-Hua,TAN Zhi-Jun,ZHOU De-Qing.Determination of Five Lipophilic Marine Toxins in Shellfish by Liquid Chromatography with Tandem Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2010,38(12).
Authors:YAO Jian-Hua  TAN Zhi-Jun  ZHOU De-Qing
Institution:YAO Jian-Hua1,2,TAN Zhi-Jun1,ZHOU De-Qing 1 1(Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Qingdao 266071) 2(College of Food Science and Technology,Shanghai Ocean University,Shanghai 201306)
Abstract:A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method for the determination of five lipophilic marine toxins including Gymnodimine(GYM),Spirolide-1(SPX1),Okadaic acid(OA) Pecenotoxin-2(PTX2) and Azaspiracid-1(AZA1) in shellfish was developed.After being extracted with methanol and water(80 /20,V/V),the extract was cleaned by solid phase extraction of MAX column,then determined by a reversed phase HPLC gradient program coupled with tandem mass spectrometry in selectedreaction-monitoring mode.GYM...
Keywords:Lipophilic marine toxins  Shellfish  Liquid chromatography-tandem mass spectrometry  
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