气相色谱法测定中毒样品鱼体中三种拟除虫菊酯农药的方法研究

Study of Three Kinds of Pyrethroids in Poisonous Fish Sample with Gas Chromatography

目的 建立食物中毒样品鱼体中农药氯氰菊酯、氰戊聚酯、溴氰菊酯的气相色谱的测定方法。方法 采用气相色谱法。以电子捕获检测器 ,3%ov - 1 0 1色谱柱 ,气化温度 2 6 0℃ ,检测器温度 2 6 0℃ ,柱温2 4 0℃为测定条件。结果 氯氰菊酯、氰戊菊酯、溴氰菊酯在 0～ 0 .4ug/ml范围内呈良好的线性关系 (r =0 .9999、0 .999、0 .987)。方法的最小检出量氯氰菊酯 4× 1 0 -1 2 g、氰戊菊酯 5× 1 0 -1 2 g、溴氰菊酯 3× 1 0 -1 2 g ;最小检出浓度氯氰菊酯 4 .0ug/kg、氰戊菊酯 5 .0ug/kg、溴氰菊酯 3.0ug/kg。方法的回收率为氯氰菊酯 93.3%～ 1 0 1 .2 %、氰戊聚酯 98.0 %～ 1 0 1 .8%、溴氰菊酯 87.5 %～ 1 0 3.6 %。结论 本方法可适用于粮食、蔬菜等食品中拟除虫菊酯的测定 ,而且快速、准确。

Objective To set up a new method to detect Cypermethrin, Fenvalerate and Deltamethrin in poisonous fish samples. Methods With 3% ov-101 column and electronic capture detector, gas chromatography was adopted to examine insecticides in samples. The operating conditions were gasified temperature 260℃, detector temperature and column temperature 240℃. Results Within range from 0 to 0.4ug/ml, linear relation between the Pyrethroids content and peak value was observed Of Cypermethrin, Fenvalerate and Deltamethrin, the minimum content and the minimum concentration which were detectable were 4.0×10 -12 g and 4.0ug/kg, 5.0×10 -12 g and 5.0ug/kg, 3.0×10 -12 g and 3.0ug/kg respectively. The recycle rate of Cypermethrin was 93.3%～101.2%. That of Fenvalerate was 98.0%～101.8% and that of Deltamethrim was 87.5%～103.0%. Conclusions With its rapidity, accuracy and simplicity, this method could be applied to detect Pyrethroids in foodstuff, such as the grains and vegetable samples.