Determination of pesticides in edible oils by liquid chromatography-tandem mass spectrometry employing new generation materials for dispersive solid phase extraction clean-up

• A novel method for pesticides residue determination was developed.
• Clean-up procedure was evaluated using several sorbents such as PSA, Z-Sep and EMR-Lipid.
• The method was validated following the criteria established by Document No. SANTE/11945/2015.
• The method was successfully applied to determine pesticide residue in real edible oil samples.

The goal of this work was to evaluate the efficiency of several sorbents on removal fats from edible oils (olive, soya and sunflower) during the clean-up step for posterior determination of 165 pesticides by UHPLC-QqQ-MS/MS system. The extraction procedure employed in this work was the citrate version of QuEChERS method followed by a step of freezing out with dry ice and clean-up evaluation using i) PSA with magnesium sulfate (d-SPE); ii) magnesium sulfate and Z-sep sorbent (d-SPE); iii) Z-sep (column SPE) and iv) Agilent Bond Elut QuEChERS Enhanced Matrix Removal-Lipid (EMR-Lipid). After evaluation of the recovery results at 10, 20 and 50 μg kg−1, the EMR-Lipid showed important advantages comparing to the other sorbents evaluated, such as better recovery rates and RSD%. The method was validated at the three concentrations described above. Analytical curves linearity was evaluated by spiking blank oil samples at 10, 20, 50, 100 and 500 μg kg−1. The method demonstrated good recoveries values between the acceptable range of 70–120% and RSD% < 20 for most of evaluated pesticides. In order to evaluate the performance of the method, this same procedure was employed to other oils such as soya and sunflower with very good results.