超高效液相色谱-串联质谱法测定香草兰中多菌灵和甲霜灵残留

Determination of carbendazim and metalaxyl in vanilla by ultra performance liquid chromatography-tandem mass spectrometry

建立了香草兰样品中多菌灵和甲霜灵残留的超高效液相色谱-串联质谱（UPLC—MS／MS）检测方法。样品用乙腈溶液提取，经氨基活性碳复合固相萃取柱净化，以多离子反应监测（MRM）模式进行测定。多菌灵和甲霜灵的最低检出限均为2．0Ixg／kg，在10．0～500．0ng／mL的线性范围内，相关系数均大于0．99。多菌灵在香草兰中的添加回收率为84．2％-100.3％，相对标准偏差（RSD）为1.3％～5.4％；甲霜灵在香草兰中的添加回收率为80．4％～100．0％，相对标准偏差（RSD）为1．7％～6．2％。该方法灵敏度高、准确性好、分析时间短，适用于香草兰样品中多菌灵和甲霜灵残留量的检测。

An analytical method was developed for the determination of carbendazim and metalaxyl in vanilla by using ultra performance liquid chromatography coupled with tandem mass spectrometry（UPLC-MS/MS）. The pesticides were extracted by acetonitrile, and cleaned up by earbon/NH2 solid phase extraction （SPE） column, then quantified with multiple reactions monitoring （MRM）. The limits of detection （LOD） for both pesticides were 2.0 la, g/kg. Calibration curves exhibited good linearity over the concentration range from I0.0 to 500.0 ng/mL, with their correlation coefficients above 0.99. Average recoveries for carbendazim spiked at 3 levels ranged from 84.2% to 100.3%, with a relative standard deviations（RSD） range from 1.3% to 5.4%. Average recoveries for metalaxyl spiked at 3 levels ranged from 80.4% to 100.0%, with a RSD range from 1.7% to 6.2%. The developed method was sensitive, rapid and reliable. As a result, it can be applied for determination of earbendazim and metalaxyl in vanilla.