亲水液相色谱三重四极杆质谱联用法快速检测尿液和血浆中河豚毒素  

Rapid Determination of Tetrodotoxin in Human Urine and Plasma Using Hydrophilic Interaction Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

作　　者：张秀尧[1] 蔡欣欣[1] 

机构地区：[1]温州市疾病预防控制中心,温州325001

出　　处：《分析化学》2009年第12期1829-1833,共5页Chinese Journal of Analytical Chemistry

基　　金：温州市医学重点学科;温州市第三轮"311"工程建设项目基金(No.2008012)资助

摘　　要：建立了快速检测尿液和血浆中河豚毒素的亲水液相色谱三重四极杆质谱联用分析方法。样品经乙腈沉淀、TSK-gel Amide-80亲水色谱柱分离后,采用电喷雾串联质谱多反应监测(MRM)模式检测,基体匹配标准外标法定量。尿液和血浆样品的线性范围分别为3～500μg/L和1～200μg/L,加标回收率分别为96%～108%和100%～105%,相对标准偏差小于9%和16%(n=6),样品的检出限分别为1.0和0.3μg/L(S/N=3)。本方法简单、快速、灵敏、特异性强。A rapid method for the detection of tetrodotoxin（TTX） in human plasma and urine was developed by hydrophilic interaction liquid chromatography-tandem mass spectrometry. After a simple protein precipitation step was undertaken, the subsequent analysis of TTX was achieved on a TSK-gel amide-80 column using an ammonium formate-methanol-acetonitrile gradient with a cycle time of 13 min, and detected by positive electrospray ionization tandem mass spectrometry in the MRM mode, and quantified by matrix-match standard solution. It was found that linearity in urine was observed within concentration ranged from 3μg/L to 500μg/L, that in plasma 1μg/L to 200μg/L and that limits of detection （ S/N = 3 ） for urine and plasma were 1 and 0.3μg/L, respectively. The average recoveries were 96% - 108% and 100% - 105% for TTX spiked in urine and plasma, respectively, with relative standard deviations of 1.7% - 8.6% and 8.9% - 16% （n =6）. This method was simple, selective and sensitive to detect TTX in urine and plasma for both clinical and forensic purposes.

关 键 词：亲水液相色谱三重四极杆质谱法 河豚毒素 尿液 血浆 

分 类 号：R115[医药卫生—公共卫生与预防医学]