摘要
基于UPLC-MS/MS建立可同时测定多菌灵、腐霉利、吡虫啉、啶虫脒、乙酰甲胺磷、毒死蜱、甲胺磷、二甲戊灵、氧乐果这 9 种韭菜中易残留农药的分析方法.样品经乙腈提取,QuEChERS净化,优化的质谱及色谱参数,MRM监测模式下检测,基质配标,外标法定量.结果表明,多菌灵在 1～200 μg/kg、腐霉利在5～500 μg/kg、其余7 种农药在 1～500 μg/kg线性关系良好,R在 0.99 以上,定量限均可达到 10 μg/kg;在 10、50、100、200 μg/kg 4 个添加水平,9 种农药平均回收率在70%～115%之间,RSD在 0.6%～6.7%.该方法简便、高效、准确,可在 4 min内完成韭菜中9 种易残留农药的检测.
Abstract
Based on QuEChERS and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),a method for simultaneous detection of 9 pesticide residues in Chinese chives was established,including Carbendazim,Procymidone,Imidacloprid,Acetamiprid,Orthene,Chlorpyrifos,Methamidophos,Pendimethalin,Omethoate.The Chinese chive samples were extracted by acetonitrile,cleaned-up by QuEChERS method and then determined by optimized UPLC-MS/MS method in multi-reaction monitoring(MRM)mode,quantified by matrix matching external standard method.The results showed that carbendazim had a good linear relationship in 1～200 μg/kg,procymidone in 5-500 μg/kg and the other 7 pesticides in 1～500 μg/kg,with R above 0.99 and limit of quantification up to 10 μg/kg.The recoveries for all compounds spiked at levels of 10,50,100,200 μg/kg,which are ranged from 70%to 115%,with relative standard deviations(RSDs)are 0.6%～6.7%.The method was simple,efficient,reliable,and was suitable for simultaneous determination of 9 pesticide multi-residues in Chinese chives within 4 min.
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