超高效液相色谱-串联质谱法同时测定水果中3种苯并咪唑类杀菌剂

Determination of Three Benzimidazole Fungicides in Fruits by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

目的:构建一种超高效液相色谱-串联质谱法(Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS/MS)同时测定水果中3种苯并咪唑类杀菌剂的方法。方法:试样匀浆后用1%甲酸-乙腈超声提取,提取液经乙二胺-N-丙基硅烷和无水硫酸镁净化,采用UPLC-MS/MS测定。结果:3种杀菌剂线性关系良好,相关系数R2均大于0.999,定量限在0.05~1.16μg·kg^(-1),选定3个浓度进行添加回收验证实验,回收率为87.1%~103.2%,相对标准偏差为1.4%~6.5%。结论:该方法简捷、准确,可满足水果中3种苯并咪唑杀菌剂的快速检测与确证分析要求。

Objective:To develop a method for simultaneous determination of three benzimidazole fungicides in fruits by ultra-high performance liquid chromatography-tandem mass spectrometry.Method:The samples were homogenized,followed by ultrasonic extraction with 1%formic acid-acetonitrile,the extraction solution was purified by primary secondary amine and anhydrous magnesium sulfate,and detected by UPLC-MS/MS.Result:The linearity of each fungicide was good,with linear correlation coefficients were greater than 0.999,and the limits of detection were 0.05~1.16μg·kg^(-1),three concentrations were selected for the addition and recovery experiment,and the recovery rate of spiked samples were 87.1%~103.2%,and the relative standard deviations were 1.4%~6.5%.Conclusion:The method is simple,convenient and accurate,and is suitable for the rapid detection and confirmatory analysis of three benzimidazole fungicides in fruits.