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建立了番茄果实和土壤中氟吡菌胺残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。用乙腈水溶液提取样品中的氟毗菌胺,以C_(18)柱为分析柱、乙腈-甲酸水溶液为流动相,采用超高效液相色谱-串联质谱多反应监测、电喷雾正离子源、外标法定量。氟吡菌胺在0.05~1.00 mg/L范围内与峰面积呈良好的线性关系,线性方程为y=6964.10x-143.28,决定系数为0.996 8。向对照番茄果实、对照土壤中分别添加氟吡菌胺标样,使其添加量分别为0.10 mg/kg、0.40 mg/kg和2.00 mg/kg,平均回收率分别为92.43%~103.32%和92.75%~104.46%,相对标准偏差分别为3.8%~4.9%和3.4%~4.4%。番茄果实和土壤中氟吡菌胺的定量限分别为1.0μg/kg和1.7μg/kg,检出限分别为0.3μg/kg和0.5μg/kg。
A UPLC-MS / MS method was developed for the determination of fluopicolide in tomato fruits and soils. The samples were extracted with acetonitrile aqueous solution of difenoconid, C_ (18) column as the analytical column, acetonitrile - formic acid aqueous solution as mobile phase, using ultra performance liquid chromatography - tandem mass spectrometry multiple reaction monitoring, electrospray positive ion source, the outer Standard method of quantitative. Fluopicolide had a good linear relationship with the peak area in the range of 0.05-1.00 mg / L, the linear equation was y = 6964.10x-143.28, and the determination coefficient was 0.996 8. The standard samples of fluopicolide were added to control tomato and control soils with the average recoveries of 0.10 mg / kg, 0.40 mg / kg and 2.00 mg / kg, respectively. The average recoveries were 92.43% ~ 103.32% and 92.75% % ~ 104.46%, the relative standard deviations were 3.8% ~ 4.9% and 3.4% ~ 4.4% respectively. The limit of quantification of fluopicolide in tomato fruits and soils was 1.0 μg / kg and 1.7 μg / kg, respectively. The limits of detection were 0.3 μg / kg and 0.5 μg / kg, respectively.