Abstract
With the aim of monitoring multiclass semi-polar pesticide residues in freshwater fatty fish, two QuEChERS approaches (so-called acetate buffered and unbuffered versions) were evaluated for the determination of 77 pesticide residues. Compounds were selected according to the dominant rainfed agriculture activities in South America. Unbuffered QuEChERS was finally chosen for validation purposes owing that it provided the best results in terms of recovery yields. Method performance was evaluated in two instrumental systems, liquid chromatography – tandem mass spectrometry (LC–MS/MS) in Scheduled MRM™ algorithm available on hybrid quadrupole – linear ion trap (QLIT) instrument, and gas chromatography – mass spectrometry (GC–MS) under selected ion monitoring (SIM) mode.Spiking experiments were carried out to determine the trueness, precision, linearity, limit of quantification of the method as well as matrix effect.The Unbuffered QuECHERS method described here:•Was validated for the analysis of 67 pesticide residues in fish muscle tissue.•Presented quantification limits in the range 1–15 μg kg−1 for the vast majority of the studied compounds.•Enable environmental monitoring of pesticide residues in fish due to their low LOQs.
Highlights
Analyst software v 1.5.1 (SCIEX) was used for data acquisition and processing. Both QuEChERS approaches were compared at mg kgÀ1 level, in terms of % Rec and repeatability, for the seventy-seven compounds listed in Recovery results at 50 mg kgÀ1 showed that the performance of these methods was very similar
The performance of the evaluated method was studied in terms of recoveries, limits of quantifications, precision, linearity and matrix effect according to SANTE guidelines [7]
Despite of the complexity of the sample, our results demonstrate that the methodology is suitable for analysis of trace concentrations of pesticide residues, enabling multi-class pesticide determination at low part per billion levels
Summary
Determination of multiclass, semi-polar pesticide residues in fatty fish muscle tissue by gas and liquid chromatography mass spectrometry. A Departamento de Química del Litoral-DQL, CENUR Litoral Norte, Universidad de la República (UdelaR), Ruta 3 Km 363, 60000, Paysandú, Uruguay b Grupo de Análisis de Compuestos Traza – GACT, Facultad de Química, Universidad de la República (UdelaR), General Flores 2124, 11800, Montevideo, Uruguay c Departamento de Desarrollo Tecnológico – DDT, Centro Universitario Regional del Este (CURE), Universidad de la República (UdelaR), Ruta 9 y Ruta 15, 27000, Rocha, Uruguay
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