SPE-HPLC法同时测定大白菜中吡虫啉等5种农药残留方法研究

构建了利用固相萃取-高效液相色谱(SPE-HPLC)同时测定大白菜中吡虫啉、多菌灵、除虫脲、灭幼脲、辛硫磷5种农药残留量的方法。固相萃取采用乙腈萃取,氨基柱净化;高效液相色谱采用C18色谱柱进行分离,最佳色谱条件为:柱温40℃,进样量20μL,检测波长270 nm,选择水与甲醇+乙腈混合液(3+1)作梯度洗脱,流速为1.0 mL/min。结果表明:该方法在0.02~1.0μg/mL浓度范围内有良好的线性关系,5种农药的回收率在88.5%～98.8%之间,相对标准偏差在1.84%～4.62%之间,适用于大部分蔬菜中吡虫啉等5种农药残留量的检测。

Simultaneous Determination of Five Pesticide Residues in Chinese Cabbages by SPE-HPLC

A method for simultaneous determination of five pesticide residues including imidacloprid,carbendazim,diflubenzuron,chlorbenzuron and phoxim in Chinese cabbages was established by using solid-phase extraction high performance liquid chromatography(SPE-HPLC).The samples were extracted by acetonitrile and cleaned up with amido cartridge.Chromatographic separation was performed on a RP-C18 column,and the best chromatographic conditions were determined: the column temperature was 40℃,the injection volume was 20 μL and the detection wave length was 270 nm,using water and methanol-acetonitrile(3∶1) as mobile phase with flow rate of 1.0 mL/min.The results showed that a good linear correlation was obtained in the range of 0.02～1.0 g/mL,the recovery ratio of five pesticide residues ranged from 88.5% to 98.8%,the relative standard deviation(RSD) ranged from 1.84% to 4.62%.it’s applicable to the detection of five pesticide residues such as imidacloprid in most of the vegetables.