气相色谱法检测卷心菜中啶虫脒和吡虫啉残留

采用模拟添加法,确立以XAD-2为柱填料,环己烷/乙酸乙酯V(环乙烷)∶V(乙酸乙酯)=1∶1]为淋洗剂的柱层析法提取、净化残留于卷心菜中啶虫脒和吡虫啉的前处理方法;建立以中等极性SUBTM-5柱、色谱柱程序升温、FID/MSD检测的气相色谱残留样品确证性检测方法。结果显示,优化色谱条件下啶虫脒和吡虫啉出峰时间均不超过8 min,且在0.5~100μg.L-1内有良好的线性响应,啶虫脒为Y=11.599X+221.578(r2=0.995 5),吡虫啉线性回归方程为Y=179.751X+2 592.787(r2=0.997 4),啶虫脒和吡虫啉最小检出量分别为3.5×10-7mg和5.1×10-7mg,残留样本的平均前处理时间均不超过20 min,它们在0.25、0.5和1.0 mg.kg-1添加水平下的平均添加回收率均大于75%,各添加量6次测定值的相对标准偏差均小于5%,啶虫脒和吡虫啉的定量检测限分别为0.005 3和0.007 1 mg.kg-1。表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠。

Determination of Acetamiprid and Imidacloprid Residue in Cabbage by Gas Chromatography

The sample pretreatment method of XAD-2 column chromatography was build by the modeling addition experiment and the confirmatory detection method was established by GC-FID/MSD to acetamiprid and imidacloprid residue in cabbage.The result indicated that:(i) The retention time of acetamiprid and imidacloprid were all less than 8 minutes under the optimization chromatography conditions and the calibration curve of peak area(Y) and mass density of pesticide(X) was linear,which were Y=11.599X+221.578(r2=0.995 5)...