液相色谱-电喷雾离子阱质谱联用分析河豚毒素  

Determination of Tetrodotoxin by Liquid Chromatography Coupled with Electrospray Ion-trap Mass Spectrometry

作　　者：李爱峰[1,2] 于仁成[3] 周名江[3] 

机构地区：[1]中国海洋大学海洋环境与生态教育部重点实验室 [2]中国科学院海洋研究所海洋生态与环境科学重点实验室,青岛266071 [3]中国科学院海洋研究所海洋生态与环境科学重点实验室

出　　处：《分析化学》2007年第3期397-400,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.30571426);973重点基础研究项目课题(No.2001CB409704);国家十五科技攻关计划(No.2001BA804A20)资助项目

摘　　要：应用C18反相色谱柱和HILIC亲水作用色谱柱,建立了河豚毒素（TTX）的液相色谱-电喷雾离子阱质谱联用分析方法。应用反相色谱法,在选择离子监测（SIM）模式下,对TTX的分析具有良好的线性响应（r=0.9992）,方法检出限（S/N=3）为120pg,相对标准偏差（RSD）低于10%;应用亲水色谱法,在SIM和选择反应监测（SRM）模式下同样具有良好的线性响应（r=0.9996和r=0.9998）,检出限（S/N=3）分别为15pg和3.75pg,在SIM模式下RSD低于10%,在SRM模式下RSD处于10%~20%之间。亲水作用色谱柱大大提高了方法的灵敏度,由于SIM模式具有较高的精密度,建议应用HILIC色谱柱的SIM模式定量分析TTX。Two methods for tetrodotoxin analysis using liquid chromatography coupled with electrospray iontrap mass spectrometry （LC-ESI-MS） have been established with C18 reversed phase column and hydrophilie interaction liquid chromatography （HILIC） column, respectively. Sensitivity and reproducibility of the methods were compared. The method using C18 column in selected ion monitoring （SIM） mode had a detection limit （ S/N = 3 ） of 120 pg, and a good linearity of the calibration curve was obtained for tetrodotoxin （ r = 0. 9992）. High reproducibility of the method was observed, with a relative standard deviation （RSD） below 10%. The method using HILIC column in SIM mode and selected reaction monitoring （SRM） mode had detection limits （ SIN = 3 ） of 15 and 3.75 pg, respectively. Good linearity of the calibration curves was obtained for tetrodotoxin （r =0. 9996 and 0.9998 in SIM and SRM mode, respectively）. The reproducibility was high in SIM mode but relatively poor in SRM mode. Based on the results, the method using HILIC column in SIM mode was suggested for the analysis of tetrodotoxin with LC-MS system.

关 键 词：液相色谱-电喷雾离子阱质谱联用 河豚毒素 选择离子监测 选择反应监测 

分 类 号：O657.63[理学—分析化学]