离子色谱-质谱联用测定牛奶中的高氯酸盐、溴酸盐和碘离子  

Analysis of Perchlorate,Bromate and Iodide in Milk Using Ion Chromatography-Electrospray Tandem Mass Spectrometry

作　　者：张萍[1] 史亚利[1] 蔡亚岐[1] 牟世芬[1] 

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085

出　　处：《分析测试学报》2007年第5期690-693,共4页Journal of Instrumental Analysis

基　　金：国家重点基础研究计划(973项目)(2003CB415001);国家自然科学基金资助项目(20577058;20475060);中国科学院重要方向性项目(KZCX3-SW-432)

摘　　要：以离子色谱-质谱联用同时测定了不同品牌牛奶中的高氯酸盐、溴酸盐和碘离子。以高容量、强亲水性IonPac AS20（2 mm）为分析柱,EGC在线产生KOH为淋洗液,串联质谱检测。ESIMS/MS以多元反应监测（MRM）模式分别监控高氯酸盐的m/z100.8/84.9、98.8/82.9离子对,溴酸盐的m/z126.8/110.9、126.8/95.0离子对和碘离子的m/z126.8/127.0离子对,并分别对高氯酸盐、溴酸盐和碘离子以m/z98.8/82.9、126.8/110.9和126.8/127.0离子对的峰面积进行定量。该方法对高氯酸盐、溴酸盐和碘离子的检出限（S/N=3）分别为0.02、0.1和0.5μg/L,线性相关系数分别是0.999（0.05～50μg/L）、0.999（0.5～100μg/L）、0.998（1～1 000μg/L）。高氯酸盐和碘离子的样品加标回收率分别在102%～108%之间和86%～114%之间。A sensitive and selective method was proposed for simultaneously confirmation and quantification of perchlorate,bromate and iodide in milk samples at low parts-per-billion levels.Using high capacity and hydroxide selective column IonPac AS20 and electrospray tandem mass spectrometry（IC-ESI MS/MS） in the negative ESI and multiple reaction monitoring mode,analytes were separated and detected.The eluent KOH was generated on-line by EGC.The transitions of m/z 100.8/84.9 and 126.8/95.0 were monitored for confirmation and m/z 98.8/82.9,126.8/110.9,126.8/127.0 for quantifying the analytes.This approach yielded low limits of detection（S/N=3） which were 0.01 μg/L for perchlorate,0.2 μg/L for bromate and 0.5 μg/L for iodide.A linear calibration was obtained with a correlation coefficient of 0.999 8 for perchlorate（0.05-50 μg/L） and bromate（0.5-100 μg/L） and 0.998 6 for iodide（1-1 000 μg/L）.The method was applied to the simultaneous detection of perchlorate,bromate and iodide in milk samples.The recoveries from spiked samples were 102%-108% for perchlorate and 86%-114% for iodide.

关 键 词：高氯酸盐 溴酸盐 碘离子 离子色谱-串联质谱 牛奶 

分 类 号：O657.75[理学—分析化学] O657.63[理学—化学]