摘要
建立了一种测定痕量高氯酸盐的离子色谱-质谱联用方法。选用高容量、强亲水性的阴离子交换柱IonPac AS20(2mm)进行分离,以淋洗液自动发生器在线产生的KOH为淋洗液,采用等浓度淋洗。在不添加有机溶剂的情况下,淋洗液经过抑制器抑制后直接进入电喷雾-串联质谱(ESI-MS-MS),以负离子模式进行检测。同时采用多元反应监测(MRM)模式对高氯酸盐进行监控,以100.8/84.9、98.8/66.9和100.8/68.9为监控离子对,以98.8/82.9离子对的峰面积进行定量。高氯酸盐质量浓度在0.05~50μg/L范围内具有良好的线性(r=0.9985),检出限(S/N=3)为0.01μg/L。将该方法用于饮用水以及地下水、雪水等环境水样中高氯酸盐的分析,并进行了加标回收实验,回收率在86%~110%之间,将实际自来水样品连续11次进样,所得高氯酸盐的峰面积的相对标准偏差(RSD)为1.6%。
In this paper the ion chromatography-electrospray tandem mass spectrometry (IC-ESI-MS-MS) was developed for the determination of perchlorate in drinking water and environmental water.Perchlorate was separated with high capacity and hydroxide selective column using KOH eluent generating on-line from EGC.ESI-MS-MS detection was performed by the negative electronspray ionization and multiple reaction monitoring (MRM) mode.The transition of 98.8/82.9 was monitored for quantifying the main analyte.The transition 100.8/84.9,98.8/66.9 and 100.8/68.9 were monitored for confirmation.The detection limit of perchlorate was as low as 0.01 μg/L.The method was applied to the detection of perchlorate in tap water,ground water and snow water.The recoveries of spiked standard were in the range of 86%~110%.RSD of the peak area for the eleven successive injections of tap water was 1.6%.
出处
《分析试验室》
CAS
CSCD
北大核心
2007年第4期34-37,共4页
Chinese Journal of Analysis Laboratory
基金
国家重点基础研究计划973(2003CB415001)
国家自然科学基金(20475060
20577058)
中国科学院重要方向性(KZCX3-SW-432)项目资助
关键词
高氯酸盐
离子色谱-串联质谱
饮用水
环境水
Perchlorate
Ion chromatography-electrospray tandem mass spectrometry
Drinking water
Environmental water