气相色谱-串联质谱法测定蔬菜中氟乐灵等8种农药的残留量

Determination of 8 kinds of pesticide residues in vegetables by gas chromatography- tandem mass spectrometry

中文关键词:  农药残留  气相色谱-串联质谱法  蔬菜

英文关键词:pesticides residues  gas chromatography-tandem mass spectrometry  vegetables

中文摘要:

      目的 建立气相色谱-串联质谱法同时测定蔬菜中氟乐灵、嘧霉胺、甲霜灵、二甲戊灵、氟虫腈、溴螨酯、哒螨灵、苯醚甲环唑8种农药的残留量。方法 样品经乙腈提取, 以乙酸乙酯+乙醇(9:1, V:V)作为洗脱液经Carbon/NH2固相萃取柱净化, 采用DB-5MS毛细管色谱柱分离; 质谱采用电子轰击离子源模式电离, 多反应监测模式测定。结果 8种农药在0.02~2.0 mg/L范围内呈现良好的线性关系, 相关系数r为0.995~0.999; 样品中添加0.02、0.20、2.0 mg/L 3个浓度水平的8种农药混标工作液进行加标回收试验, 平均回收率为83.2%~119.4%, RSD为1.8%~8.9 %(n=5), 检出限为0.005~0.010 mg/kg。结论 该方法快速、准确, 可适合蔬菜中多种农药残留的定量检测。

英文摘要:

      Objective To establish a method for determination of 8 kinds of pesticides residues including trifluralin, pyrimethanil, metalaxyl, pendimethalin, fipronil, bromopropylate, pyridaben and difenoconazole in vegetables by gas chromatography-tandem mass spectrometry. Method Samples were extracted with acetonitrile, cleaned up with solid phase extration column of Carbon/NH2, and separated by DB-5MS column. Electron ionization (EI) mode and multiple reaction monitoring mode (MRM) were used in mass spectrometry. Results Eight kinds of pesticides had a good linear relationship in the range of 0.02~2.0 mg/L with correlation coefficient of 0.995~0.999. The mean recoveries spiked at 3 levels of 0.02, 0.20, and 2.0 mg/L in samples were in the range of 83.2%~119.4% with the relative standard deviations of 1.8%~8.9%(n=5), and the limits of detection were in the range of 0.005~0.010 mg/kg. Conclusion The method is rapid and accurate, which can be applied for the quantitative detection of multi-pesticide residues in vegetables.