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.
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
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
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