主管：中华人民共和国司法部
主办：司法鉴定科学研究院
ISSN 1671-2072  CN 31-1863/N
中国司法鉴定

中国司法鉴定 ›› 2012 ›› Issue (2): 22-25.

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HPLC-MS法测定鲜鱼中河豚毒素

金玉娥，马佳鸣，熊丽蓓等   

  1. 上海市疾病预防控制中心，上海 200336
  • 收稿日期:2012-01-02 出版日期:2012-03-15 发布日期:2022-07-12
  • 通讯作者: 汪国权（19 —），男，主任技师。
  • 作者简介:金玉娥（1977—），女，主管技师，主要从事食品环境中污染物分析。Email∶yejin@scde.sh.cn。

Determination of Tetrodotoxin in Fish by HPLC-MS

JIN Yu-e， MA Jia-ming， XIONG Li-bei, etc.   

  1. Shanghai Municipal Center for Disease Control and Prevention， Shanghai 200336， China
  • Received:2012-01-02 Published:2012-03-15 Online:2022-07-12

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摘要：

目的 建立用液相色谱-质谱（ HPLC- MS） 法测定鲜鱼中河豚毒素含量的方法。方法 样品经粉碎、酸性水溶液提取、蛋白酶解、石油醚脱脂、有机溶剂甲醇沉淀、固相萃取柱净化后，以液相色谱-质谱法测定，外标法定量。结果 鱼肉和鱼肝中河豚毒素在0.10～10 mg/kg范围内呈良好线性关系，相关系数分别为0.9998和0.9991，平均回收率为94.6%~102%，相对标准偏差RSD小于6.6%，方法的最低检出限为0.03 mg/kg。结论 该方法操作简便、快速，为饮用水及水产品中河豚毒素的检测、相关的司法鉴定等提供了准确有效的科学依据。

关键词: 河豚毒素, 鱼, 三氟乙酸, 液相色谱-质谱

Abstract:

Objective To develop a method for the determination of tetrodotoxin in fish by high performance liquid chromatography-mass spectrometry （HPLC-MS）. Method After being extracted with acetate acid， hydrolyzed by papain， with fat removed by petroleum ether， precipitated with methanol， and further purified by SPE， samples were analyzed by HPLC-MS and quantified with the external standard method. Results The linear range of tetrodotoxin was 0.10-10 mg/kg in fish meat and liver （R=0.9998 and 0.9991， respectively）. The mean recovery was 94.6%~102% and RSD was below 6.6%. The limit of detection was 0.03 mg/kg. Conclusion The established method is simple and efficient. It can provided an accurate and effective approach for the detection of tetrodotoxin in drinking water and fishes in forensic toxicology identification.

Key words: tetrodotoxin, fish, trifluoroacetic acid, HPLC-MS

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