目的 建立快速测定蔬菜中有机磷和硫丹类农药残留的固相萃取-气相色谱-质谱仪联用检测方法。方法 采用乙腈提取,Carb/NH₂固相萃取柱净化, DB-17MS石英毛细管色谱柱,以GC-MS选择离子监测模式检测蔬菜中12种有机磷和3种硫丹类。结果 15种农药组分线性范围在0.2~1.0 μg/ml之间,标准曲线线性系数r＞0.99,检出限在0.01~0.08 mg/kg,定量下限0.05~0.26 mg/kg之间,样品高、低两个浓度加标回收率在76%~117%之间,相对标准偏差(RSD)在1.27%~6.53%之间。结论 方法准确度高、灵敏度好、重现性好、快速,适用于蔬菜中有机磷和硫丹类农药残留测定。

Objective To establish the method of solid phase extraction(SPE) pretreatment technology -gas chromatography-mass spectrometry ( GC-MS), for the determination of fifteen pesticide residues,such as organophosphorus and endosulfan in vegetables. Methods The target pesticides in samples were extracted with acetonitrile,and cleaned-up by the solid phase extraction column ( SPE) called Carb/NH₂,the samples were separated with DB-17 MS column (30×0.25 m),Selected ion monitoring (SIM) was used to detect the pesticide of twelve organophosphorus residues and three endosulfan residues in vegetables. Results The standard curve range of the method was among 0.2~1.0 μg/ml,and the correlation coefficient of standard curve was more than 0.99 .The limits of detection(LOD) of the method were among 0.01~0.08 mg/kg,and the limits of quantification ( LOQ) were among 0.05~0.26 mg/kg .The recoveries of the method were between 76% and 117%. The relative standard deviations of high and low concentrations(RSD) were between 1.27% and 6.53%. Conclusion The method has the advantages of high accuracy, good sensitivity, good reproducibility, simple and rapid, and so on. It was suitable for the determination of organophosphorus and endosulfan pesticide residues in vegetables.