气相色谱-串联质谱法测定水果中的溴菌腈农药残留

Determination of bromothalonil residue in fruits by gas chromatography-tandem mass spectrometry

目的建立固相萃取结合气相色谱-串联质谱检测溴菌腈在水果中残留量的分析方法。方法样品中加入乙腈并匀浆提取,过滤后盐析,静置分层后取上层清液过复合氨基柱净化,最后用乙酸乙酯定容,GC-MS-MS上机检测。结果本方法检测水果中溴菌腈的残留量的方法在0.010 mg/L~0.25 mg/L内线性关系良好,相关系数为0.991~0.999,方法定量限为0.010 mg/kg。添加水平为0.010 mg/kg、0.10 mg/kg、0.20 mg/kg时回收率在88.2%~115.2%,相对标准偏差为2.2%~9.1%。结论本文建立的气相色谱-串联质谱法检测水果中溴菌腈的残留量的方法,简单、快速、准确,精密度和准确度都满足要求,可用于日常检测水果中溴菌腈的残留量。

Objective To establish a method for the determination of bromothalonil in fruits by gas chromatography-tandem mass spectrometry(GC-MS/MS)with solid phase extraction(SPE).Methods The samples were extracted with acetonitrile by homogenizer,filtered,salted out,purified by SPE column of CARB/NH2 and then dilute with ethyl ether to volume.The targeted compounds were detected by GC-MS/MS.Results The results showed that the linearity of bromothalonil residue in fruits ranged from 0.010 mg/L to 0.25 mg/L,with the linear correlation coefficients ranged from 0.991 to 0.999.The limits of quantification(LOQ)of bromothalonil was 0.010 mg/kg.The average spiked recoveries at levels of 0.010 mg/kg,0.10 mg/kg and 0.20 mg/kg were in the range of 88.2%-115.2%,with the relative standard deviations(RSD)between 2.2%and 9.1%.Conclusion The method was suitable for the screening and quantification of bromothalonil in fruits due to its simplicity,good sensitivity and accuracy.