分散固相萃取净化与气相色谱-串联质谱法同时测定蔬菜中157种农药残留

Determination of 157 pesticide residues in vegetables by using dispersive solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry

【目的】建立一种分散固相萃取净化结合气相色谱-串联质谱法测定蔬菜中157种农药化合物的分析方法。【方法】样品经过乙腈和QuEChERSEN-提取包提取,用无水硫酸镁150 mg、N-丙基乙二胺(primary secondary amine,PSA)75 mg、石墨化碳黑(graphitized carbon black,GCB)5 mg的填料管净化,在GC-MS/MS的动态多反应监测(dMRM)模式下检测,基质匹配标准曲线法定量分析。【结果】157种化合物在各自质量浓度范围内线性关系良好,相关系数均大于0.992 1,检出限范围为0.032~6.198μg/kg,定量限为0.107~19.496μg/kg。在0.01、0.02、0.10mg/kg加标水平下157种农药的平均回收率为74.5%~117.3%,RSD(n=6)为0.4%~10.5%。【结论】该方法前处理简单、快速、灵敏,能够满足多种农残的同时检测需求,可广泛应用于蔬菜等样品的筛查和定量检测。

【Objective】The study aimed to develop a method of the determination of 157 pesticide compounds in vegetables by using the dispersive solid phase extraction purification combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).【Method】The samples were extracted with acetonitrile and QuEChERS EN-extraction package,cleaned-up with purifying packing tubes including 150 mg MgSO4,75 mg PSA and 5 mg GCB,and then was detected by GC-MS/MS in dynamic multi-reaction monitoring(dMRM)mode,followed by quantitative analysis with the matrix-matched standard curve.【Result】The results showed that 157 pesticides had good linear relationships in the range their concentrations,the correlation coefficients were all greater than 0.9921,the limits of detection(LOD)were 0.032~6.198μg/kg,and the limits of quantification(LOQ)were 0.107~19.496μg/kg.The average rates of recovery for 157 pesticides were 74.5%~117.3%and RSDS(n=6)were 0.4%~10.5%at the markup levels of 0.01,0.02 and 0.10 mg/kg.【Conclusion】The method is simple,rapid and sensitive,and may meet the requirements for multiple pesticide residues detection,which can be widely used in the rapid screening and quantitative detection of vegetable samples.