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Acetonitrile-Ethyl acetate based method for the residue analysis of 373 pesticides in beeswax using LC-MS/MS and
Muhammad M Issa1, Sherif M Taha1, Ashraf M El-Marsafy1
1Agricultural Research Center, Central Laboratory of Residue Analysis of Pesticides and Heavy Metals in Foods, P.O. Box: 12311, Dokki, Giza, Egypt.
Abstract:
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.
