超高效液相色谱-串联质谱法同时测定水果蔬菜中11种杀菌剂

Simultaneous determination of 11 kinds of fungicides in fruit and vegetable by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  杀菌剂  水果  蔬菜

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  fungicide  fruit  vegetable

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定水果蔬菜中多菌灵、甲基硫菌灵、甲霜灵、嘧霉胺、烯酰吗啉、咪鲜胺、三唑酮、腐霉利、苯醚甲环唑、丙环唑和戊唑醇11种杀菌剂。方法 水果蔬菜采用QuEChERS前处理方法, 以C18色谱柱为分离柱, 以乙腈-0.05%甲酸水溶液为流动相进行梯度洗脱, 用超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS), 以电喷雾电离(electrospray ionization, ESI)、多反应监测(multiple reaction monitoring, MRM)模式检测11种杀菌剂, 外标法定量。结果 方法的线性范围为0.5~50.0 μg/L, 线性相关系数为0.9991~1.000, 检出限0.001 mg/kg; 3个水平的平均加标回收率88.0%~101.2%; 相对标准偏差(relative standard deviation, RSD)均小于9.1%。结论 该法具有操作简单、干扰少、快速、准确可靠等特点, 适用于水果蔬菜中多种杀菌剂的检测。

英文摘要:

      Objective To establish a method for determination of 11 fungicides (carbendazim, thiophanate-methyl, metalaxyl, pyrimethanil, dimethomorph, prochloraz, triadimefon, procymidone, difenoconazole, propiconazole and penconazole) in fruit and vegetable by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods QuEChERS pretreatment method was used and the separation was performed on a C18 column with the gradient elution of acetonitrile and 0.05% formic acid water. The 11 kinds of fungicides in fruits and vegetables were detected by UPLC-MS/MS with eletrospray ionization (ESI) in mode of multiple reaction monitoring (MRM). Quantification was performed by external standard calibration. Results The calibration curves of 11 kinds of fungicides showed good linearity in range of 0.5~50.0 μg/L, with correlation coefficient in range of 0.9991~1.000. The limit of detection of the method was 0.001 mg/kg. The recoveries of three spiked levels were 88.0%~101.2%, and relative standard deviations (RSDs) of 11 kinds of fungicides were all less than 9.1%. Conclusion This method has the advantages of simple operation, less disturbance, rapidity and accuracy, which is suitable for determination of 11 kinds of fungicides in fruit and vegetable.