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液相色谱-串联质谱法分析生物检材中的河豚毒素
作者姓名:Da Q  Liu W  Shen BH  Shen M
作者单位:1. 苏州大学,医学部法医学系,江苏,苏州,215123;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
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
基金项目: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。

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  

Determination of TTX in biological samples by LC-MS/MS
Da Q,Liu W,Shen BH,Shen M.Determination of TTX in biological samples by LC-MS/MS[J].Journal of Forensic Medicine,2010,26(6):432-435.
Authors:Da Qing  Liu Wei  Shen Bao-hua  Shen Min
Institution:DA Qing1,2,LIU Wei2,SHEN Bao-hua2,SHEN Min2(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)
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 th...
Keywords:forensic toxicology  tetrodotoxin  solid phase extraction  liquid chromatography-tandem mass spectrometry  
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