Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection

The Quick Easy Cheap Effective Rugged and Safe multiresidue method (QuEChERS) has been validated for the extraction of 80 pesticides belonging to various chemical classes from various types of representative commodities with low lipid contents. A mixture of 38 pesticides amenable to gas chromatography (GC) were quantitatively recovered from spiked lemon, raisins, wheat flour and cucumber, and determined using gas chromatography–tandem mass spectrometry (GC–MS/MS). An additional mixture of 42 pesticides were recovered from oranges, red wine, red grapes, raisins and wheat flour, using liquid chromatography–tandem mass spectrometry (LC–MS/MS) for determination. The pesticides chosen for this study included many of the most frequently detected ones and/or those that are most often found to violate the maximum residue limit (MRL) in food samples, some compounds that have only recently been introduced, as well as a few other miscellaneous compounds. The method employed involved initial extraction in a water/acetonitrile system, an extraction/partitioning step after the addition of salt, and a cleanup step utilizing dispersive solid-phase extraction (D-SPE); this combination ensured that it was a rapid, simple and cost-effective procedure. The spiking levels for the recovery experiments were 0.005, 0.01, 0.02 and 0.2 mg kg−1 for GC–MS/MS analyses, and 0.01 and 0.1 mg kg−1 for LC–MS/MS analyses. Adequate pesticide quantification and identity confirmation were attained, even at the lowest concentration levels, considering the high signal-to-noise ratios, the very good accuracies and precisions, as well as the good matches between the observed ion ratios. Mean recoveries mostly ranged between 70 and 110% (98% on average), and relative standard deviations (RSD) were generally below 10% (4.3% on average). The use of analyte protectants during GC analysis was demonstrated to provide a good alternative to the use of matrix-matched standards to minimize matrix-effect-related errors. Based on these results, the methodology has been proven to be highly efficient and robust and thus suitable for monitoring the MRL compliance of a wide range of commodity/pesticide combinations.