A developed method was proposed for determination of perchlorate in surface water by ion chromatography tandem mass spectrometry. The method was optimized based on the US EPA method, the anion exchange column was used as the analytical column with the mobile phase of potassium hydroxide. Large numbers of the weakly retained anion in detected solution were switched out to waste and the strongly retained of perchlorate was switched to mass, and analyzed by tandem mass spectrometry with negative ion electrospray under selected ion monitoring( SIM) . The detection limit of the method was 0. 031 μg/L and the relative standard deviations for sample were 2. 26%-4. 45%, the recoveries obtained were 93. 0%-98. 0%. Perchlorate concentrations in the main rivers in Sichuan Province ranged from no detected to 68. 0 μg/L, which showed that the pollution of perchlorate in surface water was not to be neglected.%采用离子色谱-串联质谱测定地表水中高氯酸盐,在US EPA相应分析方法的基础上进行了优化,以阴离子交换柱为分析柱,氢氧化钾为淋洗液,经抑制电导检测后通过阀切换将检测液中大量弱保留的阴离子切到废液后再将强保留的高氯酸盐切入质谱,电喷雾负离子模式电离,选择离子反应监测( SIM)高氯酸盐。方法检出限达0.031μg/L,实际样品相对标准偏差为2.26%~4.45%,加标回收率为93.0%~98.0%。四川省内主要河流的高氯酸盐浓度在未检出~68.0μg/L之间,高氯酸盐污染不容忽视。
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