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固相萃取富集-气相色谱质谱法测定人参中的19种有机氯农药
Determination of 19 Organochlorinated Pesticides in Panax Ginseng Using Solid-phase Extraction and Gas Chromatography-mass Spectrometry
【作者】 侯志广; 乌美男; 张铎; 赵晓峰; 王鑫宏; 逯忠斌;
【Author】 HOU Zhi-guang,WU Mei-nan , ZHANG Duo, ZHAO Xiao-feng,WANG Xin-hong, LU Zhong-bin * (College of Resource and Environmental Science, Jilin Agricultural University, Jilin 130118, China)
【机构】 吉林农业大学资源与环境学院;
【摘要】 建立了以固相萃取技术富集,气相色谱-质谱法进行分离和检测人参中19种有机氯农药的方法。对样品中六六六的4种异构体、滴滴涕的4种异构体、硫丹的2种异构体、五氯苯、六氯苯、五氯硝基苯、七氯、艾氏剂、百菌清、腐霉利、狄氏剂及异狄氏剂共19种有机氯农药的残留量进行了测定。人参中有机氯农药用乙腈萃取,SPE弗罗里硅土小柱净化。采用DB-17ms弹性石英毛细管柱分离样品,GC-MASS检测19种有机氯农药的残留量,加样添加水平为0.05~2.00mg·kg-1,方法的最低检出限为0.010~0.020mg·kg-1;平均回收率为71%~112%;RSD为2.1%~19.5%。本法操作简便,灵敏,准确。结果表明,该方法可以成功地应用于人参中19种有机氯农药残留的分析。
【Abstract】 A gas chromatographic-mass spectrometry(GC/MS)method for the trace analysis of 19 Organochlorinated Pesticide residues in Panax ginseng was described.The target compounds includingα-benzene hexaclhloride (BHC),β-BHC,γ-BHC, δ-BHC, p, p′-dichloro-diphenyl-dichloroethylene ( p, p′-DDE), p, p′- dichloro-diphenyl-dichloroethane ( p, p′- DDD) , o, p ′ -dichloro-diphenyl-trichloroeth-ane ( op ′ - DDT) , p, p ′ - DDT, pentachlorobenzene (PCB) , hexachlorobenzene (HCB), pentachloronitrobenzene( PCNB) , hep tachlor (HEPT), aldrin, chlorothalonil (CTO), endosulfan Ⅱ,endosulfanⅠ, procymidone ,diedrin, and endrin. The 19 Organochlorinated pesticides were extracted from the sample Panax ginseng with acetonitrile,the extract was cleaned up with a column of 6 mL Fiorisil by means of SPE.The 19 Organochlorinated pesticides were separated from each other through DB -17MS capillary column(30 m ×025 mm×0.25 mm)and determinated by GC-MS. The recoveries ranged from 71% to 112%.When the added level was 0.05~2.00 mg·kg -1 ,RSD were 2.1%~19.5% (n=5) and the limit of detection was 0.010~0.020 mg·kg -1 .The method is rapid, sensitive and suitable for the analysis of pesticides. The results demonstrated that the method could be successfully applied to a broad range of target pesticides in a diverse range of sample.
【Key words】 gas chromatographic-mass spectrometry; solid-phase extraction; organochlorinated pesticide residues; panax;
- 【会议录名称】 农业环境与生态安全——第五届全国农业环境科学学术研讨会论文集
- 【会议名称】农业环境与生态安全——第五届全国农业环境科学学术研讨会
- 【会议时间】2013-04-19
- 【会议地点】中国江苏南京
- 【分类号】S481.8
- 【主办单位】农业部环境保护科研监测所、中国农业生态环境保护协会