Agricultural Research Center, Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, P.O. Box: 12311, Dokki, Giza, Egypt.
Agricultural Research Center, Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, P.O. Box: 12311, Dokki, Giza, Egypt.
J Chromatogr B Analyt Technol Biomed Life Sci. 2020 May 15;1145:122106. doi: 10.1016/j.jchromb.2020.122106. Epub 2020 Apr 4.
In the current study, Pesticide residue extraction in beeswax was carried out using a mixture of acetonitrile-ethyl acetate (1:3, v/v). This mixture of solvents not only enables the melting of beeswax sample at a lower temperature than when using acetonitrile only but also introduces one phase solution. The sample extract was directly injected into both GC-MS/MS, of the commonly used split-less inlets, and into LC-MS/MS. Sample preparation and clean-up were also optimized. The developed method was validated according to SANTE/11813/2017 European Union guidelines. Three spiking levels of low concentrations 20, 50, 100 µg/kg were studied for the analysis of a total of 373 pesticides. Most of the studied pesticides have acceptable recovery between 80 and 110% with good reproducibility <10. There are 265 and 139 pesticides having a lower limit of quantifications equal 20 µg/kg using LC-MS/MS and GC-MS/MS, respectively. Finally, the developed method was successfully applied for the analysis of real beeswax samples.
在本研究中，采用乙腈-乙酸乙酯（1:3，v/v）混合液对蜂蜡中的农药残留进行提取。这种溶剂混合物不仅能够在比仅使用乙腈时更低的温度下熔化蜂蜡样品，而且还能引入单相溶液。样品提取物直接注入到 GC-MS/MS 和 LC-MS/MS 中，通常使用不分流进样口。还对样品制备和净化进行了优化。该方法是根据欧盟 SANTE/11813/2017 指南进行验证的。研究了低浓度 20、50、100μg/kg 的三个加标水平，总共分析了 373 种农药。大多数研究的农药在 80%到 110%之间具有可接受的回收率，并且重现性<10。使用 LC-MS/MS 和 GC-MS/MS 分别有 265 种和 139 种农药的定量限等于 20μg/kg。最后，该方法成功地应用于实际蜂蜡样品的分析。
