摘要
建立了离子色谱-质谱联用技术测定活性污泥样品中高氯酸盐的分析方法。以高容量、强亲水性的IonPae AS20（2mm）阴离子交换柱为分析柱，EGC在线产生等浓度KOH为淋洗液，淋洗液经抑制成水后将样品带入质谱检测。ESI-MS-MS以多元反应监测模式监控100．8／84．9、98．8／66．9、100．8／68．9和98．8／82．9离子对。以98．8／82．9离子对的峰面积进行定量。该方法对高氯酸盐的检出限（S／N=3）为0．01μg／L，高氯酸盐在0．05—100μg／L浓度范围内具有良好的线性，线性相关系数r=0．9988。0．2μg／L的标准溶液重复进样9次，高氯酸盐峰面积的相对标准偏差（RSD）为2．3％。运用该方法测定采自不同地区的活性污泥样品中的高氯酸盐，并对样品加标回收，得回收率在88．5％-102．2％之间。
A rapid method for the highly sensitive determination of perchlorate was set up by ion chromatography/electrospray ionization tandem mass spectrometry （IC/ESI-MS/MS） in the negative ESI and multiple reaction monitoring （MRM） mode. Using high capacity and hydroxide selective column IonPac AS20, perchlorate was separated by KOH eluent generated form EGC. The transition 100.8/84.9, 98.8/66.9 and 100.8/68.9 ion pairs were monitored for confirming the target analyte and 98.8/82.9 ion pair for quantifying. The detection limit of quantitation of the method （ S/N= 3 ） was as good as 0.01 g/L for perchlorate. A linear calibration was obtained over the range of 0.05 to 100 g/L with a correlation coefficient of 0. 9988. The relative standard deviation for nine successive injection of 0.2 μg/L perchlorate was 2.3%. The method was applied to the detection of perchlorate in sludge samples, which were obtained from different areas in China. The recoveries of spiked standard were 88.5% -102.2%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第1期131-134,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No20475060
20577058)
国家重点基础研究计划(973项目)(No2003CB415001)
中国科学院重要方向性项目(NoKZCX3-SW-432)
关键词
高氯酸盐
离子色谱
串联质谱
污泥
Perchlorate, ion chromatography/electrospray ionization tandem mass spectrometry, sludge
