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

作　　者：王钟[1,2] 赵志强 徐文杰 何漪 王敏[1,2] WANG Zhong;ZHAO Zhiqiang;XU Wenjie;HE Yi;WANG Min(ZIBO Center for Disease Control and Prevention,Zibo 255026,China;Zibo Key Laboratory of Environmental Organic Pollution and Population Health Monitoring and Analysis,Zibo 255026,China)

机构地区：[1]淄博市疾病预防控制中心,山东淄博255026 [2]淄博市环境有机污染与人群健康监测分析重点实验室,山东淄博255026

出　　处：《食品安全导刊》2021年第34期111-114,118,共5页China Food Safety Magazine

基　　金：淄博市科技发展计划项目(2017kj010071);山东省医药卫生科技发展计划项目(2017WS378)。

摘　　要：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.

关 键 词：蔬菜 五氯硝基苯 百菌清 气相色谱-质谱法 全自动固相萃取 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]