固相萃取-超高效液相色谱-串联质谱法测定土壤中的高氯酸盐

Determination of perchlorate in soil by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  高氯酸盐  土壤

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  perchlorate  soil

中文摘要:

      目的 建立了一种同位素稀释超高液相色谱-串联质谱法测定土壤中高氯酸盐含量的分析方法。方法试样经0.2%乙酸水溶液和二氯甲烷提取, 上清液经HLB小柱净化, 液相色谱-串联质谱法测定, 内标法定量。结果 高氯酸盐在0.1~100 μg/L浓度范围内线性关系良好, 相关系数为0.9995, 检出限为0.3 μg/kg, 定量限为1.0 μg/kg, 加标回收率在85.2%~102%, 相对标准偏差(relative standard deviation, RSD)小于8.0%。结论 该方法简便、可靠、稳定,可用于土壤中高氯酸盐含量的测定。

英文摘要:

      Objective To establish a method for the determination of perchlorate content in soil by isotope dilution ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by 0.2% acetic acid solution and dichloromethane, purified by HLB column, determined by liquid chromatography-tandem mass spectrometry and quantified by internal standard method. Results Perchlorate had a good linear relationship in the concentration range of 0.1–100 μg/L, the correlation coefficient was 0.9995, the limit of detection was 0.3 μg/kg, the limit of quantification was 1.0 μg/kg, the recovery rates were 85.2%–102%, and the relative standard deviation (RSD) was less than 8.0%. Conclusion This method is simple, reliable, and stable, and can be used for the determination of perchlorate in soil.