气相色谱法测定水果、蔬菜中多种拟除虫菊酯类农药残留

DETERMINATION OF MULTI-RESIDUES OF PYRETHROID IN FRUITS AND VEGETABLES BY GAS CHROMATOGRAPHY

[目的]建立快速、准确测定水果、蔬菜中4种拟除虫菊酯类农药残留量的方法。[方法]微波加速反应系统提取农药残留,固相萃取(SPE)柱净化,毛细管柱气相色谱法-μECD检测器测定。[结果]可同时分离检测4种拟除虫菊酯类农药残留,检出限均可达到0.001μg/mL,甲氰菊酯在0.001～5μg/mL范围内、其他3种菊酯在0.001～10μg/mL范围内线性关系良好,相关系数r>0.9990;回收率为76.2%～105.9%,相对标准偏差为3.4%～12.0%。[结论]本方法灵敏度高、净化效果好、节省时间。

To establish a method of determining 4 pyrethroid pesticide residues in fruits and vegetables rapidly and accurately. The pesticide residues were extracted by microwave preparation systems, purified by a florisil SPE column, and then determined by capillary gas chromatography-μECD. The method can simultaneously determine 4 pyrethroid pesticides re sidue s, with the detection limits of 0.001 μg/mL, the liner range of 0.001-5 μg/mL by fenpropathrin and 0.001-10 μg/mL by the other three. The coefficients of correlation were more than 0.9990.The recoveries of four pesticides were between 76.2 % -105.9 %, and the relative standard deviations were 3.4%-12.0%. This method was preponderant in sensitivity, time-saving and purification.