分散固相萃取-超高压液相色谱-串联质谱法测定黄瓜中的嗪胺灵
目的 建立黄瓜中嗪胺灵残留的液质串联快速分析检测方法。方法 样品中的嗪胺灵经乙腈提取用N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化, 利用超高压液相色谱-串联质谱(UPLC-MS/MS)在多反应监测模式下进行检测。结果 以碎片离子对 432.8>212.9、432.8>82.9定性、离子对432.8>97.8进行外标法定量。仪器在0.01~1.00 mg/kg范围内, 具有良好线性关系。在0.02~1.00 mg/kg添加水平范围内, 嗪胺灵在黄瓜中的平均回收率为85.3%~92.2%, 其相对标准偏差为2.8%~7.5%。该方法的检出限(LOD)为2.0 μg/kg, 定量限为(LOQ)为20 μg/kg。结论 本方法简便、快速、准确, 能满足国内外法规的要求, 可用于黄瓜样品中嗪胺灵的农药残留确证检测。
Objective A rapid method has been developed for the determination of germicide triforine residues in cucumber. Methods The triforine from cucumber sample, which was extracted by acetonitrile and cleaned up by primary secondary amine (PSA) and graphitized carbon black (GCB), was determined by ultra perssure liquid chromatography-mass spectrometry under multiple reaction monitoring mode, then quantified by matrix-match standard solution. Results The qualitative results were obtained based on retention time, the precursor ion and three daughter ions, and the quantitation results were on the characteristic 432.8>212.9 ion, 432.8>82.9 ion and 432.8>97.8 ion. Average recoveries of triforine in cucumber samples were found in the range of 85.3%~92.2％ at four spiking levels from 0.02 mg/kg to 1.0 mg/kg with relative standard deviations of 2.8%~7.5%. Limit of detections of triforine were 2.0 μg/kg, while limit of quantifications were 20 μg/kg, respectively. Conclusion The method is simple, rapid, and accurate, and it can meet the requirements of the domestic and international legislation. The method adapts to confirm residues of triforine pesticides in cucum-ber samples.
标题：分散固相萃取-超高压液相色谱-串联质谱法测定黄瓜中的嗪胺灵
英文标题：Determination of triforine in cucumber by dispersive solid phase extraction-ultra perssure liquid chromatography-electrospray ionization tandem mass spectrometry
作者：
陈武瑛 湖南省农业科学院植物保护研究所
张德咏 湖南省农业科学院植物保护研究所
李宗云 湖南省农业科学院植物保护研究所
何明远 湖南省农业科学院植物保护研究所
罗香文 湖南省农业科学院植物保护研究所
刘建宇 湖南省农业科学院植物保护研究所
刘绍文 湖南省农业科学院植物保护研究所
刘勇 湖南省农业科学院植物保护研究所
中文关键词:嗪胺灵,超高压液相色谱-串联质谱法,分散固相萃取,黄瓜,
英文关键词:triforine,UPLC-MS/MS,dispersive solid phase extraction,cucumber,
发表日期：2013-09-05
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