Southeast Regional Laboratory, U.S. Food and Drug Administration , 60 Eighth Street N.E., Atlanta, Georgia 30309, United States.
J Agric Food Chem. 2013 Mar 13;61(10):2315-29. doi: 10.1021/jf304191c. Epub 2013 Feb 27.
A simple and high-throughput screening method for the analysis of 136 pesticides in avocado ( Persea americana ) by LC-(+)-ESI-MS/MS and GC-MS/MS is presented. A modified QuEChERS sample preparation method was developed to improve the extraction recovery of highly lipophilic pesticides. Extracts from minced avocados after acetonitrile (MeCN) extraction were directly injected to LC-MS/MS, whereas other GC-amenable compounds were treated with the modified QuEChERS procedure for GC-MS/MS analysis. The average recoveries for 79 pesticides quantified by LC-MS/MS at 10, 50, and 200 ng/g fortifying levels were 86.1% or better (with maximum RSD at 9.2%), whereas GC-MS/MS analysis demonstrated 70.2% or better (RSD < 18%) for average recovery from 57 compounds at the same spike levels. The application of LC- and GC-MS/MS combined with the improved extraction procedures led to the current method, which can quantitate these pesticides even if they are present in avocados below the targeted action level by FDA. This method demonstrated the improved recovery of several challenging lipophilic pesticides in highly fat-rich avocados.
本文介绍了一种用于鳄梨(Persea americana)中 136 种农药的 LC-(+)-ESI-MS/MS 和 GC-MS/MS 分析的简单高通量筛选方法。开发了一种改良的 QuEChERS 样品前处理方法,以提高高度亲脂性农药的提取回收率。经乙腈(MeCN)提取后,鳄梨碎块的提取物直接注入 LC-MS/MS,而其他可进行 GC 分析的化合物则采用改良的 QuEChERS 程序进行 GC-MS/MS 分析。在 10、50 和 200ng/g 加标水平下,79 种农药通过 LC-MS/MS 定量分析的平均回收率为 86.1%或更高(最大 RSD 为 9.2%),而 GC-MS/MS 分析在相同加标水平下,57 种化合物的平均回收率为 70.2%或更高(RSD<18%)。LC-和 GC-MS/MS 的应用与改进的提取程序相结合,导致了目前的方法,即使在鳄梨中的目标行动水平以下,该方法也可以定量这些农药。该方法证明了在富含脂肪的鳄梨中,几种具有挑战性的亲脂性农药的回收率得到了提高。