基质固相分散-气相色谱法测定烟草中多种有机膦农药残留
GC Determination of Residual Organophosphorus Pesticides in Tobacoo by Treatment of Samples with Matrix Solid Phase Dispersion
摘 要
采用基质固相分散法并用丙酮作溶剂提取烟草中残留的有机膦农药.提取液浓缩近干用丙酮定容至1 mL,供气相色谱测定用.在HP-5毛细管色谱柱上,5种农药达到很好分离并用脉冲火焰光度检测器进行测定.测得5种农药的检出限(3S/N)在0.02~0.04 μg·g-1之间.对方法的精密度和回收率作了试验,测得其相对标准偏差(n=5)在1.1%~3.6%之间,回收率在89.85%~102.66%之间.
气相色谱
有机膦农药
烟草
Matrix solid phrase dispersion
Gas chromatography
Organophosphorus pesticide
Tobacoo
Abstract
Residual amounts of organophosphorus pesticides in samples of tobacoo were dispersed by matrix sold phase dispersion technique,and eluted with acetone. The extract obtained was concentrated and made up to 1 mL,the solution in acetone was used for GC determination. By using the HP-5 capillary chromatofraphic column,5 organophosphorus pesticides were separated and determinaed by PFPD. The values of detection limit (3S/N) found were in the range of 0.02-0.04 μg·g-1. Precision and recovery of the method were tested,and values of RSD′s (n=5) and of recovery found were in the ranges of 1.1%-3.6% and 89.85%-102.66% respectively.
中图分类号 O657
所属栏目 工作简报
基金项目
收稿日期 2008/10/16
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备注范逸平(1983-),男,安徽黄山人,硕士研究生,主要从事有机化学分析.
引用该论文: FAN Yi-ping,DUAN Li-ping,ZHANG Hui-zi,HUANG Hai-tao,WANG Rui,YANG Guang-yu. GC Determination of Residual Organophosphorus Pesticides in Tobacoo by Treatment of Samples with Matrix Solid Phase Dispersion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(12): 1377～1379
范逸平,段利平,张慧梓,黄海涛,王锐,杨光宇. 基质固相分散-气相色谱法测定烟草中多种有机膦农药残留[J]. 理化检验－化学分册, 2009, 45(12): 1377～1379
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参考文献
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【2】张洪非,胡清源,王芳,等.烟草农药分析方法研究进展[J].中国烟草学报,2007,4(13):65-69．
【3】宫兆晶,李培武,张文,等.基质固相分散-气相色谱法测定油菜籽中多种有机磷农药残留[J].中国油料作物学报,2007,29(3):333-338．
【4】HOPPER M L. Extract ion and clean up of organochlorine and organophosphorus pesticide residue in fats by supercritical fluid techniques[J]. AOAC Int,1997,80(3):639-646．
【5】MURUGAVERL B,KENT J. Online supercritical fluid extraction/chromatography system for t race analysis of pesticides in soybean oil and rendered fats[J]. Journal of Microcolumn Separation,1991,3:11-16．
【6】TUIJA P,GIORGIS I,MONICA W,et al. P ressurised fluid extraction (PFE) as an alternative general method for the determination of pesticide residues in rape seed[J]. The Analyst,2002,127:554-559．
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