采用超高效液相色谱-串联质谱结合改良QuEChERS方法快速分析农产品中天然除虫菊酯6种成分残留

Modified QuEChERS combined with UPLC-MS/MS in rapid analysis of six compounds of pyrethrins residues in agricultural products

建立了以改良QuEChERS作为前处理方法，结合超高效液相色谱-串联质谱（UPLC—MS／MS）检测农产品中除虫菊酯6种化合物残留量的检测方法。对QuEChERS的净化试剂和萃取盐进行优化，最终选用0．1％醋酸乙腈和dSPE萃取盐包萃取净化。采用多重反应监测（MRM）采集模式测定，除虫菊酯的检出限可达0．2μg/kg，最低定量限可达5．0μg／kg。在0．2～5．0μg／mL内具有良好的线性相关性，R。在0．999以上。除虫菊酯在菠菜、大蒜、大姜、胡萝h和大头菜基质中的加标回收率为85．6％～117．5％，相对标准偏差（RSD）值为0．4％～8．9％。改良的QuEChERS方法前处理简单，通用性强、回收率高，可以作为检测农产品中该类农药残留的有效前处理方法。

A analytical method for determining six compounds of pyrethrins in agricultural products was developed by modified-QuEChERS coupled with UPLC-MS/MS）. Purification and extraction reagents were optimized and 0.1% acetic acid in acetonitrile and dSPE extraction formula was selected. Multiple reaction monitoring （MRM） was applied for qualitative and quantitative analysis of pyrethrins. The detection limits and quantitative limits for pyrethrins were 0.2 μg/kg and 5.0 μg/kg, respectively. The calibration curve of pyrethrins showed a good linearity within the range 0.2-5.0 μg/mL （R2 〉0. 999）. Spiked recoveries ranged from 85.6% to 117.5% in five matrix of spinach, garlic, ginger, carrot and turnip, with the relative standard deviation （RSD） of 0.4% to 8.9%. The modified QuEChERS methods provided higher recoveries and extraction efficiency due to its simple operations and wide universality. It is an effective pretreatment method in analyzing the residues of pyrethrins in agricultural products.