中文摘要：本文基于QuEChERS方法和LC/MS/MS分析方法研究了一个可检测干草本植物中具有较广泛理化性质的323种农药残留的多残留分析方法，为了获得更高的精度和更低的基质效应，本文对萃取程序、清洗和基质效应三个参数进行了优化，最高效的萃取程序是在10ML水样中水化2g干草本植物并浸泡十分钟；本文采取C-18、伯胺和石墨化碳黑三种不同分散固相萃取法来避免对目标提取物的干扰；清洗过程消除了基质效应，但是也完全清洗掉了几种杀虫剂；与 SPE不同的是：在没有预期基质效应较少的情况下，所有物质的回收效果都很好；此外，本文还研究了样本稀释和液相色谱-质谱联用法，在不进行样本稀释的情况下，3ml注射量为最佳敏感条件；本文通过在0.01、0.05和0.1mg/kg三种浓度下的回收试验对该方法进行了验证，平均回收率在70%-120%范围内，相对标准差为20%。
 
 
外文摘要：A multiresidue method was studied for determination of 323 pesticides representing a wide range of physicochemical properties in dry herbs (chamomile and parsley) based on QuEChERS method and LC-ESI-MS/MS analysis. In the current study, three different parameters were optimised for a higher accuracy and a lower matrix effects: extraction procedures, cleanup and matrix effect. Optimum extraction efficiency was obtained at sample hydration of 10mL water on 2g dry herbs and soaking time for 10min. Use of different extraction techniques supported the use of mechanical shaker in comparison with ultrasound and handed shaking. As a way to remove interfering components from final extract, different cleanup techniques were studied: three dispersive solid phase extraction (D-SPE) (C-18, primary secondary amine and graphitised carbon black) have been investigated; matrix effect was reduced, but several pesticides were lost during the cleanup process. Unlike the SPE (hydrophilic lipophilic balanced polymer) produced a good recovery with all substances without expected reduction in matrix effect. Moreover, sample dilution and LC-MS/MS injection volume were studied, 3 mu L injection volume was found to be the best sensitive condition without sample dilution. The developed method was validated by performing recovery tests at 0.01, 0.05 and 0.1mg/kg, the average recoveries ranged from 70% to 120%. The reproducibility expressed as relative standard deviation (RSD %) was 20%.
外文关键词：Pesticide residues, herbs, LC-MS, MS, matrix effect, cleanup, QuEChERS
作者：Abbas, Mohamed S.; Soliman, Amira Sh.; El-Gammal, Hassan A.; Amer, Mohamed E.; Attallah, Emad R.
作者单位：Minist Agr & Land Reclamat, Agr Res Ctr, Cent Lab Residue Anal Pesticides & Heavy Met Foo, Giza, Egypt.
期刊名称：INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY
期刊影响因子：1.208
出版年份：2017
出版刊次：11
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