液相色谱-串联质谱法分析生物检材中的河豚毒素  

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

作　　者：达情[1,2] 刘伟[2] 沈保华[2] 沈敏[2] 

机构地区：[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

出　　处：《法医学杂志》2010年第6期432-435,共4页Journal of Forensic Medicine

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

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2ng/mL、2ng/mL和4ng/g。血液和尿液在4～100ng/mL、肝在5～100ng/g的范围内线性关系良好,相关系数r≥0.9973;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。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.

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 

分 类 号：DF795.1[医药卫生—法医学]