固相萃取-气相色谱-质谱仪联用同时测定蔬菜中多种有机磷和硫丹类农药残留

Simultaneous determination of organophosphorus and endosulfan pesticide residues in vegetables by solid phase extraction coupled with gas chromatography-mass spectrometry

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0.2~1.0μg/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% and6.53%.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.