气相色谱-串联质谱法检测花生油中的250种 农药残留

Determination of 250 kinds of pesticide residues in peanut oil by gas chromatography-tandem mass spectrometry

中文关键词:  农药残留  气相色谱-串联质谱法  花生油

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

中文摘要:

      目的 建立气相色谱-串联质谱法同时测定花生油中250种农药残留的分析方法。方法 样品经酸化乙腈提取, 以乙腈+甲苯(3:1, V:V)作为洗脱液经C18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, 多反应监测模式对样品进行测定。 结果 本方法分为7组, 完成250种目标化合物的分离分析。250种农药残留在0.02~0.2 mg/L 范围内呈现良好的线性关系, 相关系数r为0.990~0.999; 样品中添加5、10和20 μg/kg 3个浓度水平的250种农药混标工作液进行加标回收试验, 平均回收率为70%~130%, RSD 为1.8%~8.9% (n=5), 检出限为5~10 μg/kg。结论 该方法准确、灵敏、重现性好、高通量, 适合测定花生油中的多种农药残留。

英文摘要:

      Objective To establish a method for simultaneous determination of 250 kinds of pesticides residues in peanut oil by gas chromatography-tandem mass spectrometry (GC–MS/MS). Methods Samples were extracted with 1% acetic acetonitrile, cleaned up by C18 solid phase extraction column (SPE), and separated by DB-5MS column. Electron ionization (EI) mode and multiple reaction monitoring mode (MRM) were used in mass spectrometry. Results The 250 kinds of pesticides had good linear relationships in the ranges of 0.02~0.2 mg/L with correlation coefficients of 0.990~0.999. The average recoveries spiked at 3 levels of 5, 10 and 20 μg/kg in samples were in the ranges of 70%~130% with the relative standard deviations (RSDs) of 1.8%~8.9% (n=5), and the limits of detection were in the range of 5~10 μg/kg. Conclusion The method is rapid, reproducible and accurate, which can be applied for the quantitative determination of multi-pesticide residues in peanut oil.