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
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。
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.
标题: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
英文标题:Simultaneous determination of 32 kinds of implicitly added ingredients in pesticides by gas chromatography-triple quadrupole mass spectrometry
作者:
李俊 贵州省农产品质量安全监督检验测试中心
蔡滔 贵州省农产品质量安全监督检验测试中心
周雪丽 贵州省农产品质量安全监督检验测试中心
卢平 贵州大学精细化工研究开发中心教育部绿色农药与生物工程重点实验室;贵州省农产品质量安全监督检验测试中心
刘佳 贵州省农产品质量安全监督检验测试中心
陈会 贵州省农产品质量安全监督检验测试中心
王震 贵州省农产品质量安全监督检验测试中心
庞宏宇 贵州省农产品质量安全监督检验测试中心
王艺蓉 贵州省农产品质量安全监督检验测试中心
吴玉娥 贵州省农产品质量安全监督检验测试中心;农业部农产品质量安全风险评估实验室(贵阳)
罗华兰 贵州省农产品质量安全监督检验测试中心;农业部农产品质量安全风险评估实验室(贵阳)
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,
发表日期:2018-05-10
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- 5.09 MB
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