气相色谱-三重四级杆质谱法同时测定农药中32种隐性添加成分

Simultaneous determination of 32 kinds of implicitly added ingredients in pesticides by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  隐性添加  农药  气相色谱-三重四级杆质谱法

英文关键词:implicitly added  pesticide  gas chromatography-triple quadrupole mass spectrometry

中文摘要:

      目的 建立气相色谱-三重四级杆质谱法(gas chromatography-triple quadrupole mass spectrometry, GC-MS/MS)对农药制剂中32种隐性添加农药成分的分析方法。方法 样品采用丙酮直接提取, 正己烷定容, 内标法定量, 气相色谱-串联质谱仪检测。结果 32种农药的平均添加回收率为71.51%~100.88%, 相对标准偏差(relative standard deviation, RSD)为1.36%~7.43%, 检出限为0.03%~0.17%, 定量限为0.1%~0.5%。采用建立的方法对抽检的农药产品进行检测, 结果表明部分农药中检出隐性成分, 在0.5%的苦参碱水剂中检出1.6%的氰戊菊酯, 在5%的高效氯氟氰菊酯中检出3.5%的氟虫腈。结论 该方法高效、准确, 可用于同时测定农药中的32种隐性添加农药成分。

英文摘要:

      Objective To establish a method for determination of 32 kinds of implicitly added ingredients in pesticide formulations by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). Methods The samples were directly extracted with acetone, and volumed with n-hexane. Then they were detected by GC-MS/MS and quantified by internal standard method. Results The average recoveries of 32 kinds of pesticides were 71.51%-100.88% and the relative standard deviations (RSDs) were 1.36%-7.43%. The limits of detection were 0.03%-0.17%, and the limits of quantification were 0.1%-0.5%. The established method was used to detect pesticide products, and the results showed that some of the pesticides were detected in recessive ingredients. Totally 1.6% of fenvalerate was detected in 0.5% of matrine aqueous solution, and 3.5% of fipronil was detected in 5% of lambda-cyhalothrin. Conclusion The method is efficient and accurate, which can be used for simultaneous determination of 32 kinds of implicitly added ingredients in pesticides.