超高效液相色谱串联质谱法测定环境样品中高氯酸盐和氯酸盐的含量

Determintation Ofperchlorate and Chlorate in Environmental Samples by ULTRS Performance Liquid Chromatography Tandem Mass Spectrometry

为测定环境样品(水体、土壤)中高氯酸盐和氯酸盐的含量,本文采用超高效液相色谱串联质谱法,选用Thermo Acclaim Trinity P1复合离子交换柱(50mm×2.1mm,3μm)作为分析柱,以高氯酸盐内标(HClO_(4)-O_(4))、氯酸盐内标(ClO_(3)-^(18)O_(13))定量,采用ESI-方式、MRM模式,进行检测。结果显示,高氯酸盐、氯酸盐分别在0.05~100μg/L、0.1~200μg/L范围内线性关系良好,R^(2)≥0.9992。高氯酸、氯酸盐的检出限分别为0.025μg/L、0.2μg/L,定量限为0.05μg/L、1.0μg/L。在高、中、低浓度3个添加水平下,水体样品中高氯酸盐、氯酸盐回收率在95%~105%,土壤样品在80%~108%之间,RSD<5%。该方法前处理过程简单,灵敏度高、准确性好,适用于水体和土壤等环境样品中高氯酸盐和氯酸盐的检测。

In order to determine the content of perchlorate and chlorate in environmental samples(water and soil),this paper selected UPLC-MS,Thermo Acclaim Trinity P1 composite ion exchange column(50 mm×2.1 mm,3μm)was used as the chromatogram column.Using perchlorate(HClO_(4)-O_(4))、Chlorate(ClO_(3)-^(18)O_(13))as the internal standard,negative ion scanning and multi-reaction monitoring(MRM)mode were used for UPLC-MS detection.The results showed that The linear range of perchlorate and chlorate were 0.05-100μg/L and 0.1-200μgg/L,R^(2)≥0.9992.The limits of detection of perchloric acid and chlorate were 0.025μg/L and 0.2μg/L,and the limits of quantification were 0.05μg/L and 1.0μg/L,respectively.The recoveries of perchlorate and chlorate in water samples and soil samples were 95%-105%and 80%-108%,and the relative standard deviations were RSD<5%,respectively.This method has the advantages of simple pretreatment,high sensitivity and good accuracy,It is suitable for the determination of perchlorate and chlorate in environmental samples such as water and soil.