Determination of pesticides and their metabolites in processed cereal samples

Abstract

Fifteen pesticides including some of their metabolites (disulfoton sulfoxide, ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, malaoxon, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, terbufos sulfone, disulfoton sulfone and fensulfothion) were analysed in milled toasted wheat and maize as well as in wheat flour and baby cereals. The QuEChERS (quick, easy, cheap, effective, rugged and safe) methodology was used and its dispersive solid-phase extraction procedure was optimised by means of an experimental design with the aim of reducing the amount of co-extracted lipids and obtaining a clean extract. Gas chromatography with nitrogen phosphorus detection were used as the separation and detection techniques, respectively. The method was validated in terms of selectivity, recoveries, calibration, precision and accuracy as well as matrix effects. Limits of detection were between 0.07 and 34.8 µg kg⁻¹ with recoveries in the range of 71–110% (relative standard deviations were below 9%). A total of 40 samples of different origin were analysed. Residues of pirimiphos-methyl were found in six of the samples at concentrations in the range 0.08–0.47 mg kg⁻¹, which were below the MRLs established for this pesticide in cereal grains. Tandem mass spectrometry confirmation was also carried out in order to identify unequivocally the presence of this pesticide.

Keywords:

• cereals and grain
• processed foods
• pesticide residues
• GC/MS
• extraction
• in-house validation

Acknowledgments

M. A. G. C. thanks the Spanish Ministry of Education for the FPU grant at the University of La Laguna. J. H. B. thanks the Spanish Ministry of Science and Innovation for the Ramón y Cajal contract at the University of La Laguna. This work was supported by the Spanish Ministry of Science and Innovation (Projects AGL2008-00990/ALI, AGL2009-07884/ALI and UNLL08-3E-004).