采用乙酸-微波处理优化韭菜中有机磷农药残留检测方法的研究

Optimization of detection method of organophosphorus pesticide residues in leeks by acetic acid-microwave treatment

中文关键词:  韭菜基质  干扰  有机磷农药残留  乙酸-微波处理

英文关键词:leek matrix  interference  organophosphorus pesticide residues  acetic acid-microwave treatment

中文摘要:

      目的 构建乙酸-微波处理消除韭菜基质对有机磷农药残留检测干扰的方法。方法 通过对韭菜基质与有机磷农药的检测, 分析韭菜基质对有机磷农药残留检测干扰, 采用10%乙酸和中高火微波分别处理10、20、30、40、50、60 s, 分析各处理的韭菜本底变化。韭菜样品中添加0.08 mg/kg水平的有机磷农药标准物质, 采用10%乙酸和中高火微波, 分别处理50、60 s, 分析乙酸-微波处理对检测结果准确性的影响。结果 确定了韭菜保留时间为12.145、16.119、17.169 min对应的本底峰分别对甲拌磷、毒死蜱、甲拌磷砜色谱峰造成干扰; 韭菜的本底干扰峰面积及峰高随处理时间的延长呈下降趋势, 当处理时间达到50 s以上时, 韭菜本底峰从11个降为4个, 且3种干扰峰都未检测到; 处理时间50 s时, 各有机磷农药的加标回收率为79.2%~105.9%, 相对标准偏差为7.2%~13.5%。结论 乙酸-微波处理50 s可有效消除韭菜基质对有机磷农药残留检测的干扰, 从而有效提高了有机磷农药残留检测结果的准确性。

英文摘要:

      Objective To establish a method to eliminate the interference of leek matrix on the detection of organophosphorus pesticide residues by acetic acid and microwave treatment. Methods The leek matrix and organophosphorus pesticide were detected to analyze the interference of leek matrix on the determination of organophosphorus pesticide residues, the backgroud changes of leeks treated with 10% acetic acid and medium-high microwave for 10, 20, 30, 40, 50, 60 s were analyzed, and the recoveries of organophosphorus pesticides spiked in leek samples with 0.08 mg/kg and treated with 10% acetic acid and medium-high power microwave for 50 s and 60 respectively were determined. Results The retention time of 12.145, 16.119, 17.169 min of the background peaks of leek matrix could interfere the peaks of phorate, chlorpyrifos and phorate sulfone, respectively, and the area and peak height of the background interfering peaks of leek decreased with the increase of the treatment time. When the treatment time reached 50 s or more, the background peaks of leeks decreased from 11 to 4, and none of the 3 interference peaks were detected. The recoveries of organophosphorus pesticides spiked at 50 s were 79.2%?105.9% with the relative standard deviations of 7.2%?13.5%. Conclusion The acetic acid-medium-high microwave treatment for 50 s can effectively eliminate the interference of leek matrix on the detection of organophosphorus pesticide residues, thus effectively improve the accuracy of the detection results.