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气相色谱法测定烟草中有机磷农药残留量
          
GC Determination of Residual Amounts of Organophosphorus Pesticides in Tobacco

摘    要
提出了用气相色谱-脉冲火焰光度检测器(GC-PFPD)测定烟草中5种有机磷农药残留量的方法,采用乙腈超声提取烟草中残留的有机磷农药,提取液经蒸干等操作后,用凝胶渗透色谱法净化.用乙酸乙酯及环己烷(1+1)混合溶液作流动相淋洗凝胶柱,分取部分淋出液用HP-5弹性石英毛细管柱进行分离,GC-PFPD检测,外标法定量.所测5种农药的标准加入回收率在81.4%~99.8%之间,测得结果的相对标准偏差(n=6)在3.27%~8.42%之间.方法的检出限(3S/N)在0.02~0.04 mg·L-1之间.
标    签 气相色谱法   脉冲火焰光度检测器   凝胶渗透色谱   残留有机磷农药   烟草   GC   PFPD   Gel permeation chromatography   Residual organophosphorus pesticides   Tobacco  
 
Abstract
Five organophosphorus pesticides as residues remained in tobacco were determined by gas chromatography with pulse flame photometric detector (PFPD).The powdered tobacco sample,after dehydration,was extracted with acetonitrile ultrasonically for 1 h,and the extract was evaporated to near dryness with a rotary evaporator.The residue was taken up with ethyl acetate,cyclohexane and a mixture of NaCl and anhydrous Na2SO4 (mixed in the ratio of 1 to 1 by mass).The supernatant was taken and purified by gel permeation chromatography with a mixture of cyclohexane and ethyl acetate (mixed in the ratio of 1 to 1 by vol.) as mobile phase for elution.The eluate was collected,concentrated to 1 mL and diluted to 5.0 mL with ethyl acetate.One μL of the solution was taken for GC analysis.HP-5 elastic quartz capillary column was used for separation,and method of external standard was adopted in the determination.Detection limits (3S/N) for the 5 pesticides were in the range from 0.02 to 0.04 mg·L-1.Recovery and precision were tested and results of recovery obtained were in the range of 81.4% to 99.8%,with values of RSD′s (n=6) ranged from 3.27% to 8.42%.

中图分类号 O657.7

 
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所属栏目 工作简报

基金项目 中烟公司资助项目(2007JC01)

收稿日期 2009/4/25

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备注何超(1981-),男,湖北人,硕士,主要研究方向为有机分析.

引用该论文: HE Chao,LIU Yue-hua,HUANG Hai-tao,CHU Yu-jie,ZHAO Ji-shou. GC Determination of Residual Amounts of Organophosphorus Pesticides in Tobacco[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(6): 663~665
何超,刘跃华,黄海涛,褚玉洁,赵吉寿. 气相色谱法测定烟草中有机磷农药残留量[J]. 理化检验-化学分册, 2010, 46(6): 663~665


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参考文献
【1】付广云,韩长秀.有机磷农药及其危害[J].化学教育,2005(1):9-10.
 
【2】彭喜春,赖毅东.咸鱼制品中有机磷农药残留的毛细管CC-NPD法测定[J].食品科学,2006,27(9):226-228.
 
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