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Multiresidual pesticide analysis using GC-MS/MS

Multiresidual analysis of pesticides is very challenging area because of the complex matrix in which it is necessary to analyze as much pesticide as possible in very low concentrations. Gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) is a powerful technique for determinantion of pesticide residues. Analysis on GC-MS/MS Agilent 7010 GC / MS Triple Quad requires a special approach to each matrix and analyte. The setup requires special instrument configuration and chromatography conditions. The instrument is equipped with a multi-mode inlet (MMI). Two columns HP-5ms 15 m 0.25x0.25 are interconnected by an electronic pneumatic control (EPC) configuration that allows the backflushing system to purge and eliminate unwanted heavy components from the column, shorten the time of analysis and reduce the need for system maintenance. Retention time lock (RTL) alows need to adjust the time segments after each column cut. GC-MS/MS multiple reaction monitoring has been developed for analysis of more than 200 pesticides. Two transitions are determined for each compound and collision energy were optimized for each. Qualitative and quantitative data analysis using MassHunter software were performed. Sample preparation for fruits, vegetables and cerals using QUECHERS method according to EN 15662: 2008 on QUECHERS method-dispersive SPE column was used. Validation parameters such as limit of quantification (LOQ), trueness, precision, specificity, robustness and linearity were evaluated, and validation procedures were carried out according to the requirements of SANTE 11813/2017 Document. During the validation of the method the minimum LOQ 0.01 mg kg-1 was achieved meeting criteria of Regulation 396/2005 covering analytes from Directive 2017/660. For baby food meeting criteria of Directive 2006/141 were achieved for Ethoprophos 0.008 mg kg-1, Propineb, Cadusaphos, Demeton S Methyl 0, 006 mg kg-1 and Fipronil 0, 004 mg kg-1, respectivelly.

multiresidual pesticde analysis, GC-MS/MS

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