色谱

色谱

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法检测贝类产品中的原多甲藻酸贝类毒素

姚建华1,2, 谭志军1, 周德庆1*, 郭萌萌1, 邢丽红1, 杨守国1,2   

  1. 1. 中国水产科学研究院黄海水产研究所, 山东 青岛 266071; 2. 上海海洋大学食品学院, 上海 201306
  • 收稿日期:2009-11-05 修回日期:2010-01-05 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 周德庆

Determination of azaspiracid-1 in shellfishes by liquid chromatography with tandem mass spectrometry

YAO Jianhua1,2, TAN Zhijun1, ZHOU Deqing1*, GUO Mengmeng1, XING Lihong1, YANG Shouguo1,2   

  1. 1. Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China; 2. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China
  • Received:2009-11-05 Revised:2010-01-05 Online:2010-04-28 Published:1980-12-25
  • Contact: ZHOU Deqing

PDF

686

被引次数

27

摘要： 建立了一种贝类组织中原多甲藻酸(azaspiracid, AZA)贝类毒素主要成分AZA1的高效液相色谱-串联质谱检测方法。本方法采用甲醇-水(80:20, v/v)溶液对贝类组织中AZA1进行提取,并用MAX阴离子交换固相萃取(SPE)柱富集净化,使用Atlantis dC18(150 mm×4.6 mm, 5.0 μm)色谱柱分离,以含有50 mmol/L甲酸和2 mmol/L甲酸铵的乙腈-水溶液(80:20, v/v)为流动相进行等度洗脱,质谱采用选择反应监测(SRM)模式。AZA1在5 min内获得完全分离,且在48.85～2 442 ng/L范围内线性良好,相关系数为0.998 1。该方法检出限(S/N=3)为11.00 pg/g,添加水平为36.64、73.27、146.54 pg/g时的平均回收率为75.8%～82.5%(n=6),相对标准偏差小于10%。利用该方法对采自大连、青岛、广州水产品市场上的112个贝类样品进行了分析,发现采自大连和广州的部分贝类样品中含有AZA1。结果表明,该方法具有简单、快速、灵敏度高等特点,能充分满足贝类中AZA1检测的要求。

关键词: 贝类产品 , 液相色谱-串联质谱: 贝毒素, 原多甲藻酸

Abstract: A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of azaspiracid-1 (AZA1) in shellfishes was described. After being extracted using methanol and water (80:20, v/v), the extract was cleaned-up by solid phase extraction (SPE) of MAX column, then determined by using a reversed-phase high performance liquid chromatography (HPLC) isocratic program coupled with tandem mass spectrometry in selected reaction monitoring mode (SRM). And the extract was eluted with acetonitrile-water (80:20, v/v) on an Atlantis dC18 column (150 mm × 4.6mm, 5.0 μm) with mobile phase containing 50 mmol/L formic acid and 2 mmol/L ammonium formate. The detection limit was 11.00 pg/g. The calibration curve was linear (R2=0.998 1) in the range of 48.85~2 442 ng/L. The average recoveries of the shellfish tissue extract at three spiked levels (36.64, 73.27, 146.54 pg/g) were from 75.8% to 82.5% (n=6). The relative standard derivations (RSDs) were less than 10%. The 112 shellfish samples from the local markets of Dalian, Qingdao, Guangzhou were detected by the method, and AZA1 was detected in some samples from Dalian and Guangzhou. The results showed that the method is simple, rapid, sensitive and suitable for the detection of AZA1 in shellfishes.

Key words: azaspiracid, shellfish , shellfish poisoning, liquid chromatography with tandem mass spectrometry (LC-MS/MS)