超高效液相色谱-串联质谱法测定生活饮用水中氯酸盐和高氯酸盐

Determination of chlorate and perchlorate in drinking water by ultra performance liquid chromatography- tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  氯酸盐  高氯酸盐  生活饮用水

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  chlorate  perchlorate  drinking water

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定生活饮用水中的氯酸盐和高氯酸盐的含量。方法 采用Anionic Polar Pesticide色谱柱(2.1 mm×150 mm, 5 μm)为分析柱对高氯酸盐、氯酸盐进行分离, 选用 50 mmol/L甲酸铵甲酸水溶液(含0.9%甲酸)和乙腈作为流动相进行梯度洗脱。在电喷雾离子源, 负离子多反应监测模式下测定, 通过内标法进行定量。结果 氯酸盐和高氯酸盐在0.5~80 μg/L范围内线性关系良好, 相关系数r2不低于0.999, 氯酸盐和高氯酸盐的检出限、定量限均分别为0.5 μg/L和1.0 μg/L。氯酸盐和高氯酸盐在1.0、2.0、20.0、80 μg/L 4个水平下回收率为83.98%~106.80%, 相对标准偏差为0.57%~3.50%(n=6)。结论 该方法简便、快捷、准确, 适用于快速检测生活饮用水中的氯酸盐和高氯酸盐。

英文摘要:

      Objective To establish a method for the simultaneous determination of chlorate and perchlorate in drinking water by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Perchlorate and chlorate were separated by Anionic Polar Pesticide column (2.1 mm×150 mm, 5 μm) using 50 mmol/L ammonium formate aqueous solution (containing 0.9% formic acid) and acetonitrile as the mobile phase for gradient elution. The assay was conducted in electrospray ion source, negative ion multiple reaction monitoring mode, and quantified by internal standard method. Results The linearity was good over the range of 0.5-80 μg/L for chlorate and perchlorate, with the correlation coefficient r2 of not less than 0.999. The detection limits and limits of quantitation of chlorate and perchlorate were 0.5 μg/L and 1.0 μg/L, respectively. The recoveries of chlorate and perchlorate at the 1.0, 2.0, 20.0, and 80 μg/L levels were 83.98%-106.80%, and the relative standard deviation was 0.57%-3.50% (n=6). Conclusion The method is simple, rapid and accurate, and suitable for the rapid detection of chlorate and perchlorate in drinking water.