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%.