Multiresidue method for simultaneous analysis of aflatoxin M1, avermectins,organophosphate pesticides and milbemycin in milk by ultra-performance liquid chromatography coupled to tandem mass spectrometry |
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Authors: | Marianna Ramos dos Anjos Izabela Miranda de Castro Maria de Lourdes Mendes de Souza Virgínia Verônica de Lima Francisco Radler de Aquino-Neto |
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Affiliation: | 1. Laboratório de Resíduos e Contaminantes, Embrapa Agroindústria de Alimentos, Rio de Janeiro, Brazil;2. Instituto de Química, LAB-RES/LADETEC, Universidade Federal do Rio de Janeiro, Rio de Janeiro, Brazil |
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Abstract: | A method developed for the simultaneous analysis of aflatoxin M1, abamectin, doramectin, eprinomectin, ivermectin, moxidectin, acephate, azinphos-ethyl, azinphos-methyl, diazinon, methamidophos, methidathion, mevinphos, pirimiphos-ethyl and pirimiphos-methyl in whole raw milk, based on the QuEChERS method for extraction and clean-up, with detection and quantification by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) is described. The method was validated according to parameters of the Analytical Quality Assurance Manual from the Brazilian Ministry of Agriculture and Commission Decision 2002/657/EC, and proved suitable for analysis of these analytes within the proposed working range, with recovery values between 77% and 110%, a standard deviation lower than 20%, limits of detection between 0.05 and 0.99 µg l?1, and limits of quantification between 0.15 and 1.98 µg l?1. Samples from animals treated with abamectin, doramectin, ivermectin and diazinon were analysed by the validated method. Residues of aflatoxin M1 were also found in field samples at levels below the established maximum residue limit. |
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Keywords: | aflatoxin M1 macrocyclic lactones milk organophosphate pesticides QuEChERS UPLC-MS/MS |
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