甘蓝中毒死蜱和噻虫嗪残留的高效液相色谱分析

HPLC Analysis of Chlorpyrifos and Thiamethoxam Residues in Cabbage

为建立同时检测甘蓝中毒死蜱和噻虫嗪残留的快速分析方法,采用甲醇振荡提取样品,经弗罗里硅土-活性炭柱净化,以丙酮/正己烷洗脱,HPLC-UV检测,外标法定量,对毒死蜱和噻虫嗪在甘蓝中的残留进行了检测.结果表明：毒死蜱和噻虫嗪的混合标样添加水平为0.1～5.0 mg/kg时,毒死蜱和噻虫嗪的回收率分别为85.3％～91.2％和83.2％～86.1％,相对标准偏差均小于5％,检出限分别为0.031 mg/kg和0.039 mg/kg,准确度和精密度均达到农药残留分析的要求.该法简便快速,灵敏度高,适用于甘蓝中毒死蜱和噻虫嗪的残留量检测.

To explore the simultaneous detection method of chlorpyrifos and thiamethoxam residues in cabbage,a method was developed for the analysis of chlorpyrifos and thiamethoxam in cabbage by high performance liquid chromatography （HPLC）.The residues of chlorpyrifos and thiamethoxam in cabbage were extracted by methanol in the vibrator,purified on the glass column of forisil＋activated carbon,eluted with acetone/n-hexane,and determined by HPLC equipped with UV detector.The results showed that recoveries of chlorpyrifos and thiamethoxam were 85.3%～91.2% and 83.2%～86.1% measured at 0.1～ 5.0 mg/kg fortification level,respectively.This method was highly precise with a relative standard deviation of 〈 5%.The detection limit of chlorpyrifos and thiamethoxam was calculated to 0.031 mg/kg and 0.039 mg/kg,respectively.The method was proved to be simple,rapid,sensitive,reproducible and applicable for the residue determination of chlorpyrifos and thiamethoxam in cabbage.