全自动固相萃取气相色谱-质谱法测定蔬菜中五氯硝基苯和百菌清残留量

Determination of Quintozene and Chlorothalonil Residues in Vegetables by Gas Chromatography/Mass Spectrometry with Automated Solid Phase Extraction

目的:建立全自动固相萃取气相色谱-质谱联用(Auto-SPE GC-MS)同时测定蔬菜中五氯硝基苯和百菌清残留量的分析方法。方法:蔬菜样品经乙腈溶剂提取,经过全自动固相萃取仪净化后,采用内标法进行检测。结果:在0.10~2.00μg/mL添加水平,五氯硝基苯的平均回收率在82.6%~91.6%,相对标准偏差为7.0%~9.6%(n=10)。百菌清的平均回收率在83.0%~95.1%,相对标准偏差为6.5%~11.0%(n=10)。以信噪比RSN=3计算两种农药残留的最低检出限,五氯硝基苯的最低检出限为0.003 mg/kg,百菌清的最低检出限为0.001 mg/kg。结论:该方法自动化程度高,结果准确度和重现性好,检出限较低,可满足蔬菜中五氯硝基苯和百菌清残留量的同时检测要求。

Objective:A multiresidue analytical method was developed for determination of quintozene and chlorothalonil residues in Vegetables by gas chromatography-mass spectrometry with automated solid phase extraction(Auto SPE GC-MS).Method:Samples were extracted by acetonitrile and cleaned by automated solid phase extraction,then tested with internal standard method.Result:The recovery of quintozene ranged from 82.6%to 91.6%at spiked level of 0.10~2.00μg/mL,the relative standard deviation was varied from 7.0%to 9.6%(n=10).The LOD of quintozene was 0.003 mg/kg.The recovery of chlorothalonil ranged from 83.0%to 95.1%at spiked level of 0.10~2.00μg/mL,the relative standard deviation was varied from 6.5%to 11.0%(n=10).The LOD of chlorothalonil was 0.001 mg/kg.Conclusion:The method is accurate,reproducible,with a relatively low detection limit.It is effective to determinate quintozene and chlorothalonil residues in Vegetables.