Effects of temperature and purity of magnesium sulfate during extraction of pesticide residues using the QuEChERS method.

Despite its many documented advantages, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation approach has problems with a few unstable pesticides, partly due to the exothermic reaction generated by the use of anhydrous magnesium sulfate (anh. MgSO4) during extraction. These pesticides also tend to be difficult to analyze by GC/MS. The aim of this study was to evaluate the effect of temperature during the extraction process in a revised version of AOAC Official Method 2007.01 using anh. MgSO4 > or = 99% (fine powder) or > or = 97% (granular) purity, and the use of an ice bath for particular unstable pesticides of interest (chlorothalonil, captan, captafol, folpet, and the degradation products cis-1,2,3,6-tetrahydrophthalimide and phthalimide). Recoveries of 38 representative pesticides were measured in limes and broccoli at different extraction conditions by LC/MS/MS and low-pressure GC/MS/MS. Results showed that the difference in temperature when using > or = 99% versus > or = 97% purity anh. MgSO4 was 6-9 degrees C, which did not lead to significant differences in recoveries. The use of an ice bath aided recovery for some of the analytes in broccoli, but no significant differences were observed for limes, which already provided greater stability of the base-sensitive analytes due to acidity of the matrix.