啶酰菌胺在番茄和土壤中残留分析方法研究

Study on Residue Analytic Method Study of Boscalid in Tomato and Soil

建立了番茄和土壤中啶酰菌胺残留量的高效液相色谱一串联质谱检测方法。样品中加入乙腈,分别采用匀浆和机械振荡2种提取方式。无需净化直接过膜上机。以甲醇和水(含0.1%甲酸)为流动相梯度洗脱,电喷雾正离子(ESI^+)模式电离,多反应监测(MRM)模式检测,外标法定量。啶酰茵胺在0.005~1.5mg/L范围内线性关系良好,相关系数(r)≥0.999 0;番茄中啶酰茵胺回收率为95.16%~117.68%,变异系数为2.74%~4.11%:土壤中啶酰茵胺回收率为97.65%~108.67%,变异系数为2.70%~4.52%。最小检出量为2×10^(-11)g,最小检出浓度为0.01mg/L。该方法操作简单,快速准确,满足农药残留分析要求。

A method was established for the determination of boscalid residue in tomato and soil by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Boscalid was extracted from samples by acetonitrile and by homogenized mixing and mechanical oscillation separately.The extract was directly filtered through 0.22μm of organic membrane without purification and injected into LC-MS/MS.The analyte was separated with the mobile phases of water and methanol(containing 0.1%formic acid),detected by MS/MS with positive electrospray ionization(ESI^+)in multiple reaction monitoring(MRM) mode,and quantified by external standard method.The correlation coefficient(r) of boscalid was not lower than 0.999 0 at the concentration range from0.005~1.5mg/L.The average recoveries and coefficient of variations of the method were 95.16%~117.68%,2.74%~4.11%for tomato and 97.65%~108.67%,2.70%~4.52%for soil.The minimum detectable amount and concentration was 2×10^(-11)g and 0.01mg/L.The method is simple,fast and accurate enough to meet the requirements of pesticide residue analysis.