Validation and application of micro flow liquid chromatography–tandem mass spectrometry for the determination of pesticide residues in fruit jams

• The 1st pesticide multi-residue monitoring study in five types of fruit jam samples.
• A sensitive µLC–MS/MS method was developed and validated.
• Dilution of the final QuEChERS extracts was applied to avoid matrix effect.
• The method was used to determine pesticides residues in 51 fruit jam samples.
• 80% of the analyzed samples were positive for at least one pesticide.

In this study, a very sensitive method was validated to determine pesticides residues in fruit jams using micro flow liquid chromatography–tandem mass spectrometry (µLC–MS/MS). A slurry of the fruit jams and water was prepared to yield homogeneous samples. Because of the high sensitivity achieved with the µLC-MS/MS equipment and to minimize matrix effects, the QuEChERS extracts were diluted 30-fold before the analysis. The validation was performed analyzing spiked samples at 9 and 45 µg kg−1 (n=5). The method met validation criteria of 70–120% recovery and RSD≤20% for 92% of the 107 pesticides evaluated. The reporting limit (RL) was 9 and 45 µg kg−1 for respectively 66% and 26% of the analytes, 5% of the compounds did not fulfill the requirements for validation and 3% were not detected at the studied concentrations. The validated method was applied to the analysis of 51 different fruit jam samples from Brazil and Spain and pesticide residues were detected in 41 samples, 26 of which contained at least one pesticide at concentration >10 µg kg−1.

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