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

Journal of chromatography. A (2016-08-11)
Jonatan V Dias, Victor Cutillas, Ana Lozano, Ionara R Pizzutti, Amadeo R Fernández-Alba
ABSTRACT

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 50μgkg(-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 500μgkg(-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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Bulk
Supelco
Aldicarb-sulfone, mixture of E/Z - isomers, certified reference material, TraceCERT®
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Supel QuE, Z-Sep+ Bulk, pkg of 20 g