高效液相色谱串联质谱法同时测定蜂王浆中氟胺氰菊酯、三唑醇和蝇毒磷残留

Simultaneous Determination of Tau-Fluvalinate, Triadimenol and Coumaphos Residues in Royal Jelly Using High Performance Liquid Chromatography Tandem Mass Spectrometry

建立一种使用高效液相色谱串联质谱（HPLC．MS—MS）仪同时测定蜂王浆中的氟胺氰菊酯、三唑醇和蝇毒磷等药物残留量的方法。采用碱性条件下的乙腈萃取，并用HLBdx柱净化，经HPLC．MS—MS电喷雾电离源，正离子多反应检测模式检测，外标法定量。结果表明：蝇毒磷的检出限为2μg／kg，三唑醇和氟胺氰菊酯的检出限为1gg／kg，在5～100gg／kg之间线性关系良好，相关系数均大于0．9940，对于5、10、50gg／kg水平添加回收率范围在78．9％～102．1％之间，变异系数范围在2．1％～13．6％之间。该分析方法适合蜂王浆中氟胺氰菊酯、三唑醇和蝇毒磷的同时测定，相对标准偏差和回收率测定结果符合对食品和农产品中痕量药物的测定要求。

A method for the determination and quantification of tau-fluvalinate, triadimenol and coumaphos in royal jelly was established by HPLC-MS-MS. Tau-fluvalinate, triadimenol and coumaphos residues were extracted by acetonitrile under alkaline condition, and clean-up of the extracts was carried out using HLB solid phase extraction （SPE） column. Quantification was conducted by HPLC-MS-MS coupled with multiple reaction-monitoring （MRM） system using electron spray ionization source in an extemal standard mode. The detection limits for coumaphos, triadimenol and tau-fluvalinate residues were 2μg/kg and 1 μg/kg, respectively. The recovery rates of tau-fluvalinate, triadimenol and coumaphos residues at three spiked levels （5, 10 p.g/kg and 50 μg/kg） in different samples were in the range of 78.9%- 102.1% with relative standard deviation of 2.1%- 13.6%. The linear range of detection was 5-100 μg/kg （r 〉 0.9940）. This method can be successfuUv aoolied to the qualitative and quantitative analysis of royal jelly samoles.