QuEChERS-分散液液微萃取/气相色谱-串联质谱法高通量快速检测蔬果中152种农药残留

High-throughput Rapid Detection of Multi-pesticide Residues in Vegetables and Fruits by Gas Chromatography-Tandem Mass Spectrometry Combined with QuEChERS-Dispersed Liquid-Liquid Microextraction

建立了QuEChERS-分散液液微萃取(DLLME)/气相色谱-串联质谱法(GC-MS/MS)高通量同时测定蔬果中152种农药残留的分析方法。蔬果样品采用QuEChERS方法经乙腈提取,离心后取上清液加微量三氯甲烷(CHCl3)进行DLLME,提取液以电子轰击电离源(EI)/气相色谱-串联质谱法选择反应监测模式(SRM)测定。结果显示,152种农药(含异构体)在5.0~200μg/L质量浓度范围内线性良好,相关系数均在0.995以上;在低、中、高3个加标浓度水平下的回收率为60.6%~119%,相对标准偏差(RSD,n=6)为1.5%~20%;方法检出限为0.14~2.3μg/kg,定量下限为0.45~7.7μg/kg。该方法操作简单、样品和溶剂用量少,定性准确,灵敏度高,适用于蔬果等新鲜农产品中高通量多农残快速筛查检测。

A high sensitivity and throughput method was developed for the simultaneous determination of152 pesticide residues in vegetables and fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS ) with QuEChERS-dispersed liquid-liquid microextraction (DLLME ).Pesticide residues in vegetables and fruits samples were extracted by QuEChERS method with acetonitrile.Then after centrifugation,the acetonitrile supernatant was added with trace chloroform (CHCl3 ) for DLLME.The extract was analyzed by (GC-MS/MS ) with electron impact ion source (EI ) in selective reaction monitoring mode (SRM ).Results showed that there were good linear relationships for152 pesticides including isomers in the range of 5.0-200 μg/L with correlation coefficients above 0.995. The recoveries for the analytes at low,medium and high levels were in the range of 60.6 %-119 %,with relative standard deviations (RSD, n =6 ) of1.5 %-20 %. The limits of detection and the limits of quantitation were in the ranges of 0.14-2.3 μg/kg and 0.45-7.7 μg/kg,respectively.The method is simple,accurate and sensitive.It is suitable for the high-throughput and rapid detection of multi-residues in fresh agricultural products such as vegetables and fruits.