| 气相色谱-串联质谱检测烟草中15种苯氧羧酸类除草剂残留 |
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| 基金项目:国家质检总局科研项目(2015IK085) |
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| 中文摘要:建立了气相色谱-串联质谱技术对烟草中15种苯氧羧酸类除草剂农药残留量的分析方法。样品采用乙腈提取、Carbon TPT固相萃取柱净化、三甲基硅烷化重氮甲烷衍生化，采用气相色谱-串联质谱对15种苯氧羧酸类除草剂进行测定,通过保留时间、选择离子及相对丰度定性，外标法定量。结果表明,15种苯氧羧酸类除草剂在20~1 000 μg/L浓度范围内均呈良好线性关系，相关系数大于0.992,检出限为0.9~3.3 μg/kg，定量下限为3.2~10.8 μg/kg。在20,100,200 μg/kg 3个加标水平下的平均回收率为71.5%~105.6%，相对标准偏差(RSD)为4.5%~14.9%。该方法简便、快速、灵敏，适用于烟草中15种苯氧羧酸类除草剂的同时检测。 |
| 中文关键词:烟草 苯氧羧酸类除草剂 气相色谱-串联质谱（GC-MS/MS) 固相萃取(SPE) 甲酯化 |
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| Determination of 15 Kinds of Phenoxyacid Herbicides in Tobacco by Gas Chromatography-Tandem Mass Spectrometry |
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| Abstract:A method was developed for the simultaneous determination of 15 phenoxyacid herbicides in tobacco.Samples were extracted with acetonitrile(MeCN),then cleaned up with TPT SPE column.The methylation of analyte was performed with trimethylsily-diazmethan,and the detection was carried out by gas chromatography-tandem mass spectrometry(GC-MS/MS).The method showed a good linearity over the concentration range of 20-1 000 μg/L with correlation coefficients all above 0.992.The limits of detection and quantitation were 0.9-3.3 μg/kg and 3.2-10.8 μg/kg,respectively.The average recoveries of analytes at three fortified levels(20,100,200 μg/kg) were in the range of 71.5%-105.6%,with RSDs of 4.5%-14.9%.The proposed method is simple,rapid and sensitive,and is suitable for the simultaneous determination of 15 phenoxyacid herbicides in tobacco. |
| Key Words:tobacco phenoxyacid herbicides gas chromatography-tandem mass spectrometry(GC-MS/MS) solid phase extraction(SPE) methylation |
| 引用本文：曹桂红,王兴宁.气相色谱-串联质谱检测烟草中15种苯氧羧酸类除草剂残留[J].分析测试学报,2017,36(7):911-915. |
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