法医学杂志 ›› 2010, Vol. 26 ›› Issue (6): 432-435.DOI: 10.3969/j.issn.1004-5619.2010.06.008

• 论著 • 上一篇    下一篇

液相色谱-串联质谱法分析生物检材中的河豚毒素

达  情1,2,刘  伟2,沈保华2,沈  敏2   

  1. (1. 苏州大学 医学部法医学系,江苏 苏州 215123; 2. 司法部司法鉴定科学技术研究所 上海市法医学重点实验室,上海 200063)
  • 发布日期:2010-12-25 出版日期:2010-12-28
  • 通讯作者: 通信作者:刘伟,女,主任法医师,硕士研究生导师,主要从事法医毒物学研究;E-mail:liuw@ssfjd.cn 通信作者:沈敏,女,研究员,博士研究生导师,主要从事法医毒物学研究;E-mail:minshensfjd@hotmail.com
  • 作者简介:达情(1985—),女,江苏南通人,硕士研究生,主要从事法医毒物学研究;E-mail:darcy5358@sina.com
  • 基金资助:

    科技部公益基金资助项目(GY0702);上海市科委资助项目(072512019)

Determination of TTX in Biological Samples by LC-MS/MS

DA QING1,2, LIU WEI2, SHEN BAO-HUA2, SHEN MIN2   

  1. (1. Department of Forensic Medicine, Medical College of Soochow University, Suzhou 215123, China; 2. Shanghai Key Laboratory of Forensic Medicine, Institute of Forensic Science, Ministry of Justice, P.R.China, Shanghai 200063, China)
  • Online:2010-12-25 Published:2010-12-28

摘要: 目的 建立血液、尿液以及肝中河豚毒素(tetrodotoxin,TTX)的液相色谱-串联质谱分析方法,并进行方法学验证。 方法 血液、尿液和肝用1%乙酸甲醇溶液去蛋白后,上清液用固相萃取法净化,LC-MS/MS检测。 结果 血液、尿液和肝中TTX检出限分别为2 ng/mL、2 ng/mL和4 ng/g。血液和尿液在4~100 ng/mL、肝在5~100 ng/g的范围内线性关系良好,相关系数r≥0.997 3;日内精密度和日间精密度均在12.80%以内;回收率大于47.2%。 结论 所建方法高效、灵敏、准确,可以为河豚毒素中毒的法医学鉴定、临床诊治以及食品安全的监控提供技术保障。

关键词: 法医毒理学, 河豚毒素, 固相萃取, 液相色谱-串联质谱法

Abstract: Objective To propose a method for determination of tetrodotoxin(TTX) in human blood, urine and liver by liquid chromatography with tandem mass spectrometry(LC-MS/MS). Methods Solid phase extraction is used after the samples are precipitated, then the samples will be analyzed by LC-MS/MS. Results The limits of detection were 2 ng/mL in blood and urine and 4 ng/g in liver for TTX respectively, the linear correlation coefficients were not less than 0.997 3, both of the intra-day and inter-day precisions were less than 12.80%, the recoveries for all kinds of specimens were more than 47.2%. Conclusion This method is efficient, sensitive and accurate and was successfully validated for implementation in forensic toxicological analysis.

Key words: forensic toxicology, tetrodotoxin, solid phase extraction, liquid chromatography-tandem mass spectrometry

中图分类号: