大口径毛细管柱气相色谱测定烟草中6种拟除虫菊脂农药残留量

Determination of Pyrethrums Residue in Tobacco by Wide-Bore Capillary Gas Chromatography

报道了用大口径毛细管柱气相色谱同时测定烟草中甲氰菊脂、三氟氯菊脂、氯菊脂、氯氰菊脂、氰戊菊脂、溴氰菊酯 6种拟除虫菊脂农药残留量的方法。样品农药残留经丙酮提取 ,凝结液除杂 ,石油醚萃取 ,弗罗里硅土柱净化 ,OV 1 0 1大口径毛细管柱分离 ,电子捕获检测器 (ECD)检测。本法的检出限为 0 0 0 1～ 0 .0 0 5mg/kg。 6种农药标准加入回收率为 85 5%～ 1 0 2 .0 % ,相对标准偏差 4 6%～ 1 7.5%。

This paper describes an efficient method for the determination of six kinds of pyrethrums residue (fenprathrin, cyholothrin, permethrin, cypermethrin, fenvalerate, deltemethrin) in tobacco. The pyrethrums was extracted from the tobacco sample with acetone, and the undesirable components were separated. Then it was extracted with the petroleum ether and through the column of Florisil acidic siliceous earth in series, and determinated by wide-bore capillary (OV-101 30m 0.53 mm) gas chromatography with electron capture detector. The detection limits were 0.001 similar to 0.005 mg/kg. The recoveries were 85.5% similar to 102.0% and the relative standard deviation is 4.6% similar to 17.5%. This method is simple, sensitive, and suitable for pesticide residue analysis.