直接进样法-超高效液相色谱串联质谱法测定黑龙江流域水中10种农药残留

Determination of 10 kinds of pesticide residues by direct injection-ultra high performance liquid chromatography tandem mass spectrometry in Heilongjiang river

中文关键词:  直接进样  水  农药  超高效液相色谱串联质谱法

英文关键词:direct injection  water  pesticide  ultra high performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立直接进样-超高效液相色谱串联质谱法(ultra high performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)测定黑龙江流域水中10种农药残留的分析方法。方法 水样无需富集, 经0.22 μm微孔滤膜过滤后, 超高效液相色谱分离, 动态多反应监测模式(dynamic multi reaction monitoring, DMRM)质谱分析, 基质匹配标准曲线外标法定量。结果 10种农药的检出限(S/N=3)在0.1~3.0 μg/L之间, 定量限(S/N=10)在0.2~5.0 μg/L之间, 在各自线性范围内, 具有良好的线性关系(r≥0.997), 在5.0、10.0和50.0 μg/L 3个添加水平下平均回收率在78.0%~109.9%之间, 相对标准偏差(relative standard deviation, RSD)小于20%(n=6)。结论 该方法简单、快速、灵敏度高, 在10 min内完成10种农药的检测分析, 可用于流域水中多种农药残留的快速检测。

英文摘要:

      Objective To establish a method for the determination of 10 kinds of pesticides in Hei longjiang river water by direct injection-ultra high performance liquid chromatography tandem mass spectrometry in river water. Methods The 10 target compounds were separated by ultra performance liquid chromatography, analyzed by dynamic multiple reaction monitoring mode (DMRM) mass spectrometry, matrix matched standard and quantified by external standard solution. Results The limits of detection of 10 pesticides (S/N=3) were in the range of 0.1–3 μg/L, the limits of quantitative (S/N=10) were 0.2–5.0 μg/L. In the scope of their respective linear, 10 kinds of pesticides had a good linear relationship (r=0.997), the average recoveries were in the range of 78.0%-109.9% at 5.0, 10.0, 50.0 μg/L 3 concentration, the relative standard deviations (RSDs) less than 20% (n=6). Conclusion This method is simple, fast and sensitive. It can be used for the analysis and detection of 10 kinds of pesticides in 10 min, which can be used for rapid detection of pesticide residues in river water.