蔬菜和水果中杀菌剂的高效液相色谱-串联质谱检测法

Determination of microbicides in vegetables and fruits by LC-MS/MS

目的建立高效液相色谱-串联质谱(LC-MS/MS)法定量测定蔬菜和水果中11种杀菌剂的方法。方法样品以快速样品前处理技术(Qu ECh ERS法)净化,经LC-MS/MS检测,以选择离子扫描(SIM)模式检测目标化合物的特征离子进行定性定量分析。结果11种杀菌剂在测定的范围内线性关系良好(r>0.9990),方法的检出限为0.4~2.5μg/kg(S/N=3)。在加标水平为40、60、80μg/L时,方法的回收率为75.6%~108.2%,相对标准偏差为1.2%~7.5%。结论该方法前处理简单,分析时间短、选择性好和灵敏度高,适用于蔬菜和水果中杀菌剂的检测。

[Objective]To establish the high performance liquid chromatography tandem mass spectrometry(LC-MS/MS)method for quantitative determination of 11 microbicides in vegetables and fruits.[Methods]The samples were purified by Qu ECh ERS,detected by LC-MS/MS.The characteristic ions of target compound were qualitatively and quantitatively analyzed by LC-MS/MS under SIM mode.[Results]Within the range,the linear relation of 11 microbicides was well(r>0.9990),and the detection limits were 0.4-2.5μg/kg(S/N=3).When the standard addition levels were 40,60 and 80μg/L,the recovery rates were 75.6%-108.2%,and the RSD were 1.2%-7.5%.[Conclusion]This method has the advantages of simple pretreatment,short analysis time,good selectivity and high sensitivity,which is suitable for the determination of microbicides in vegetables and fruits.