全自动固相萃取仪GC-MS/MS法测定蔬菜中五氯硝基苯和百菌清残留量  

Determination of pentachloronitrobenzene and chlorothalonil residues in vegetables by automated solid phase extractor with GC-MS/MS method

作　　者：侯建荣[1] 甘平胜[1] 李晓晶[1] 刘苗[1] 邓芬芳[1] 曾涛 潘心红[1] 李静[1] HOU Jianrong;GANPingsheng;LI Xiaojing;LIU Miao;DENG Fenfang;ZENG Tao;PAN Xinhong;LI Jing(Guangzhou Center for Disease Control and Prevention,Guangdong 510440,China)

机构地区：[1]广州市疾病预防控制中心,广东510440

出　　处：《医学动物防制》2020年第9期917-918,F0003,F0004,共4页Journal of Medical Pest Control

基　　金：广东省医学科学技术研究基金(A2019060);广州市卫生健康科技项目-西医类一般引导项目(20201A011065)。

摘　　要：目的建立全自动固相萃取GC-MS/MS联用测定蔬菜中五氯硝基苯和百菌清农药残留的方法。方法样品经丙酮+二氯甲烷(1+1)提取,全自动固相萃取仪净化定容,采用内标法进行检测。结果所得五氯硝基苯线性方程为y=0.0514x-1.67,相关系数为0.9999;百菌清线性方程为y=0.0315x-0.9696,相关系数为0.9997,五氯硝基苯和百菌清的检出限分别为0.001 mg/kg、0.0005 mg/kg,精密度为3.25%~6.19%,加标回收率为77.8%~94.6%。结论该方法具有良好的线性、较低的检出限以及较好的密度和准确度,可满足蔬菜中五氯硝基苯和百菌清的同时检测要求。Objective To establish a combination of automated solid phase extraction and GC-MS/MS method to determine the pentachloronitrobenzene and chlorothalonil residues in vegetables.Methods The sample was extracted with acetone and dichloromethane(1+1),then the purification and constant volume were completed by the fully automated solid phase extractor.Finally the sample was detected by internal standard method.Results The linear equation of pentachloronitrobenzene was y=0.0514 x-1.67,with the correlation coefficient of 0.9999.And that of chlorothalonil was y=0.0315 x-0.9696,with the correlation coefficient of 0.9997.The detection limits of pentachloronitrobenzene and chlorothalonil were 0.001 mg/kg and 0.0005 mg/kg,respectively.The precision ranged from 3.25%to 6.19%,and the recovery was in the range of 77.8%~94.6%.Conclusion This method has excellent linearity,lower detection limit and superior precision and accuracy,which can meet the requirements of simultaneous detection of pentachloronitrobenzene and chlorothalonil in vegetables.

关 键 词：蔬菜 全自动固相萃取仪 GC-MS/M法 五氯硝基苯 百菌清 残留量 

分 类 号：R155.54[医药卫生—营养与食品卫生学]