A multi-residue method for the determination of pesticides in high water content matrices by gas chromatography–single quadrupole mass spectrometry with electron ionisation (EI-GC/MS)
2012
de Oliveira, Mauro Lúcio Gonçalves | Madureira, Fernando Diniz | Aurélio, Fabiano | Pontelo, Ana Paula | Silva, Gilsara | Oliveira, Reginaldo | Paes, Cláudia
An EI-GC/MS method for the determination of pesticide residues in vegetable matrices with high water content was validated using papaya samples. The validation of a multi-residue pesticide method was in agreement with national and international regulations enabling the Ministry of the Agriculture, Livestock and Food Supply of Brazil to cover a large number of matrices and pesticide residues in its monitoring and control programmes. The extraction used 60 mL of ethyl acetate and 30 g of sample previously processed. After extraction, clean-up of all the extracts was carried out by percolation through GBC cartridges. The samples were then injected in an EI-GC/MS system. Calibration curves were prepared in quadruplet by fortifying blank extracts with a standard solution containing all the pesticides studied at 0.000, 0.005, 0.010, 0.020, 0.030, 0.050, 0.080 and 0.100 mg kg⁻¹. For the recovery study, blank samples were fortified at 0.010, 0.020, 0.030, 0.050 and 0.080 mg kg⁻¹ and then submitted to the extraction procedure. The complete procedure was repeated over four different days by two analysts. The regression parameters of calibration curves were calculated for each validation day. Linearity, selectivity, specificity, robustness, limits of detection and quantification were also assessed. The uncertainty was estimated for each analyte at each spike level studied. The method had recoveries between 91% and 105% and precision results ≤20%. Limits of quantification were below or equal to the maximum residue limits (MRLs) regulated by Brazilian legislation. The MRLs of the selected pesticides are not regulated by CODEX Alimentarius. The results are also in agreement with SANCO/10684/2009.
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