CONDITION OPTIMISATIONFOR PESTICIDE RESIDUES DETERMINATION

Jelena Banić-Simičić, Maja Pandurević-Todorović, Nina Tomčić, Biljana Marošanović,SP LABORATORIJA A.D.

Industrijska 3, Bečej, Serbia

We were using raspberry matrix for this study. The raspberry matrix was spiked with 7 characteristic pesticides for raspberry (Cyprodinil, Pyrimethanil, Azoxystrobin, Boscalid, Chlorpyrifos, Trifloxystrobin, Fludioxonil). It was prepared in three trials and compared with pesticide standard solution in a suitable solvent (ACN or 1:1 Hexane:Acetone). Samples were analyzed for a week and statistical analysis was performed. The results were expressed by recovery.

There are many advantages in analysis of pesticides in food using ultra-efficient ionization source of the Triple Quadrupole GC/MS. In our standard work we are using QuEChERS method for sample preparation.

Figure 3. 3 different steps of sample preparation and recoveries

This study was performed using an Agilent 7890 GC coupled to an Agilent 7010 Triple Quadrupole GCMS with an ultra-efficient ionization source. The GC system was equipped with electronic pneumatic control (EPC), a Multi-Mode Inlet (MMI) with air cooling, an Agilent 7693 Automatic Liquid Sampler, and a backflushing system. Agilent MassHunter Software was used for instrument control, and for qualitative and quantitative data analysis. Figure 3.

Figure 1. Review of pesticides that we have analyzed in fruit samples

CONCLUSION:

Figure 2. Agilent 7010 Triple Quadrupole GC/MS

Based on these results it can be concluded that all three steps were successful but because of the best obtained recovery we decided for the second step for further analyzes.

FoodANALYSIS Congress; Safety, Quality, Novel Technologies; 15-16 September 2015, Cambridge, UK

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References:[1] EN 15662:2008 Foods of plant origin - Determination of pesticides residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE-QuEChERS-method

In this study our main occupation was to optimize sample preparation (QuEChERS method) and pesticide determination byGC/MS/MS. Sample preparation was done in three steps. First one was using extract solvent exchange from ACN to 1:1Hexane:Acetone, second was with ACN extract using constant temperature inlet, third one was ACN extract with Multi-ModeInlet and than instrumental determination for all three steps. (1)

Figure 4. Average recovery for Cyprodinil (%) Figure 5. Average recovery for Pyrimethanil (%) Figure 6. Average recovery for Trifloxystrobin (%) Figure 7. Average recovery for Azoxystrobin (%)

Figure 8. Average recovery for Chlorpyrifos (%) Figure 9. Average recovery for Boscalid (%) Figure 10. Average recovery for Fludioxonil (%)