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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
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曹小云,陈树干,曾楚莹,黎秀娟,王露 广东省深圳市盐田区疾病预防控制中心 
基金项目:深圳市盐田区产业发展资金医疗卫生科技项目(20150109)
中文摘要: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5.0~200 μg/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0.14~2.3 μg/kg,定量下限为0.45~7.7 μg/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。
中文关键词:QuEChERS  分散液液微萃取(DLLME)  气相色谱-串联质谱联用(GC-MS/MS)  农药多残留  蔬菜水果
 
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
Abstract:A high sensitivity and throughput method was developed for the simultaneous determination of 152 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 for 152 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) of 1.5%-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.
Key Words:QuEChERS  dispersive liquid-liquid micro extraction(DLLME)  gas chromatography tandem mass spectrometry(GC-MS/MS)  multi pesticide residues  vegetables and fruits
引用本文:曹小云,陈树干,曾楚莹,黎秀娟,王露.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[J].分析测试学报,2019,(8):920-930.
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