Large multiresidue analysis of pesticides in edible vegetable oils by using efficient solid phase extraction sorbents based on quick, easy, cheap, effective, rugged and safe methodology followed by gas chromatography tandem mass spectrometry.
The aim of this research was to adapt the QuEChERS method for routine pesticide multiresidue analysis in edible vegetable oil samples using gas chromatography coupled to tandem mass spectrometry (GC MS/MS) Several clean up approaches were tested: (a) D SPE with Enhanced Matrix Removal Lipid (EMR Lipid(tm) (b) D SPE with PSA; (c) D SPE with Z Sep; (d) SPE with Z Sep. Clean up methods were evaluated in terms of fat removal from the extracts, recoveries and extraction precision for 213 pesticides in different matrices (soybean, sunflower and extra virgin olive oil) The QuEChERS protocol with EMR Lipid d SPE provided the best reduction of co extracted matrix compounds with the highest number of pesticides exhibiting mean recoveries in the 70 120% range, and the lowest relative standard deviations values (4% on average) A simple and rapid (only 5min) freeze out step with dry ice (CO2 at 76degC) prior to d SPE clean up ensured much better removal of co extracted matrix compounds in compliance of the necessity in routine analysis. Procedural Standard Calibration was established in order to compensate for recovery losses of certain pesticides and possible matrix effects. Limits of quantification were 10mgkg( 1) for the majority of the pesticides. The modified methodology was applied for the analysis of different 17 oil samples. Fourteen pesticides were detected with values lower than MRLs and their concentration ranged between 10.2 and 156.0mgkg( 1)
Journal of chromatography. A