Determination of pesticide residues in high oil vegetal commodities by using various multi-residue methods and clean-ups followed by liquid chromatography tandem mass spectrometry
Łukasz Rajski, Ana Lozano, Ana Uclés, Carmen Ferrer, Amadeo R. Fernández-Alba
Journal of Chromatography A, 1304 (2013) 109– 120
DOI: http://dx.doi.org/doi:10.1016/j.chroma.2013.06.070
Abstract
Several extraction methods were evaluated in terms of recoveries and extraction precision for 113 pesticides in avocado: QuEChERS with various d-SPE clean-ups (Z-Sep, Z-Sep+, PSA+C18 and silica), miniLuke and ethyl acetate. Extracts were analysed using liquid chromatography coupled with triple quadrupole mass spectrometer working in multi-reaction monitoring mode. Z-Sep and Z-Sep+ are new types of material for high lipid matrices - these two sorbents contain ZrO2, which improves fat removal from the extracts. The QuEChERS protocol with Z-Sep provided the highest number of pesticides with recoveries in the 70-120% range along with the lowest amount of coextracted matrix compounds. Subsequently, this method was validated in two matrices - avocado and almonds. In the validation recoveries at two levels - 10 and 50 μg/kg - limit of quantitation, linearity, matrix effects, as well as the inter- and intraday precision were studied. In the avocado samples, 107 analytes had LOQs equal to 10 μg/kg (signal to noise of quantitative transition was equal 20 or more). In the almond samples, 92 pesticides had LOQs equal to 10 μg/kg (S/N ≥ 20) and 2 pesticides at 50 μg/kg. The validated method was employed in the analysis of real avocado and almond samples.
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Published 10-07-2013, 15:14:04
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