【摘要】 建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定水果蔬菜中烯肟菌胺残留量的方法。样品经乙腈提取、净化后采用Thermo Scientific Hypersll GOLD色谱柱分离,电喷雾正离子源(ESI+)选择反应监测(SRM)模式检测,外标法定量。结果表明:采用QuEChERS方法和SPE方法净化后,烯肟菌胺的基质效应分别为-9.5%~-42.4%和-14.9%~-54.1%,均表现为基质抑制效应。烯肟菌胺在1~400μg/L浓度范围内具有良好的线性关系,决定系数均大于0.998,2种净化方法的检出限分别为0.06μg/kg和0.02μg/kg。在2、20和200μg/kg 3个添加水平下,2种方法的回收率分别在83.8%~100.3%和82.4%~102.4%之间,相对标准偏差分别在2.5%~7.1%和4.1%~10.2%之间。2种方法均灵敏、可靠,可根据需要选择不同的净化方法 。更多还原

【Abstract】 Two HPLC-MS/MS method s for the analysis of fenaminstrobin residue in fruits and vegetables were developed and validated. The samples were extracted with acetonitrile and cleared up by the methods of QuEChERS extraction and solid phase extraction( SPE) on amino column. The chromatographic separation was carried out by Thermo Scientific Hypersll GOLD column. Fenaminstrobin was detected by electro-spray ionization( ESI+), and selected the reaction monitoring( SRM) mode. Quantification was performed by peak area external standard methods using matrix-matched calibration curves. The results showed that the matrix effects were-9.5%~-42.4% and-14.9%~-54.1%, respectively, using the two different purification methods. Good linear relationship(R~2>0.998) was achieved in the range of 1 ~400 μg/L, and the limit of detection( LOD) of the two methods was 0.06 μg/kg and 0.02 μg/kg, respectively. At 2, 20 and 200 μg/kg spiked levels, the recoveries was 83.8% ~100.3%,82.4%~102.4%, and the relative standard deviations(RSD) was 2.6%~7.1%, 4.1%~10.2%, respectively. Both of the methods were sensitive and reliable, and were suitable for the determination of residues in fruits and vegetables.更多还原