超高效液相色谱-串联质谱法同时测定槟榔中 10种农药残留

Simultaneous determination of 10 kinds of pesticides residues in areca catechu by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  鸡蛋  氟虫腈及其代谢物  气相色谱法  高效液相色谱-串联质谱法

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  areca catechu  pesticide residues  simultaneous determination

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法同时测定槟榔中10种农药残留的快速检测方法。方法 样品采用80%乙腈-水溶液进行提取, 使用N-丙基乙二胺(primary secondary amine, PSA)-无水硫酸镁进行净化, 0.1%的甲酸-乙腈作为梯度洗脱的流动相, 多反应监测(multiple reaction monitoring, MRM)模式进行定量分析。结果 10种农药在0.5~200 ng/mL范围内呈良好线性, 相关系数均大于0.995, 检出限(limit of detection, LOD)为0.6~3.9 μg/kg, 对样品进行3个水平浓度的加标回收实验, 回收率在85.6%~107.2%之间, 相对标准偏差(relative standard deviation, RSD)在3.7%~9.6%之间。结论 该方法具有操作简便, 回收率高, 精密度好等优点, 为规范槟榔的外源性污染提供有效的测定方法。

英文摘要:

      Objective To establish a rapid method for simultaneous determination of 10 kinds of pesticide residues in areca catechu by ultra performance liquid chromatography-tandem mass spectrometry (UPLC- MS/MS). Methods The samples were extracted by 80% acetonitrile-water solution, and purified with the PSA- anhydrous magnesium sulfate. A mixture of 0.1% formic acid-acetonitrile was used for gradient elution as mobile phase and quantitative analysis was conducted by the multiple reaction monitoring mode (MRM). Results Good linearities were obtained for 10 kinds of pesticides in the concentration range of 0.5-200 ng/mL with correlation coefficients (r) more than 0.995. The limits of detection (LOD) were 0.6-3.9 μg/kg, and the recoveries were in the range of 85.6%-107.2% at the spiked levels, with relative standard deviations (RSDs) of 3.7%-9.6%. Conclusion This method has high recovery rate, good precision and is easy to operate, which is suitable for simultaneous determination of exogenous pollution of areca catechu.