A simple and efficient method for imidazolinone herbicides determination in soil by ultra-high performance liquid chromatography-tandem mass spectrometry.

ABSTRACT

The use of pesticides in agriculture has generated numerous consequences to the environment, requiring analysis of the persistent residues in soil, water and air. The variability of soil properties interferes in the extraction of pesticide residues with robustness and accuracy. The group of imidazolinones herbicides, widely used for weed control, becomes an additional task in multiresidue extraction procedures because of their low pKa values. In order to determine these compounds in soil samples, different methods have been proposed, however they can be very laborious and require more time and well trained analysts. Thus, this study aimed to develop a simple and efficient method for determination of imidazolinones (imazamox, imazapic, imazapyr, imazaquin and imazethapyr) residues in soil, using an extraction with aqueous ammonium acetate solution (0.5 M) and clean-up with dispersive solid phase extraction employing PSA, followed by UHPLC-MS/MS analysis. Satisfactory values of accuracy (70-93%) and RSD (≤17%) were achieved, as well as lower limit of quantification (5.0 µg kg(-1)). Considering the matrix and compounds complexity, the developed and validated method proved to be an excellent tool for rapid analysis (20 min), with reliability for application in real samples with wide pH range. In the analysis of 22 real samples, the method allowed the quantification of imazapic (5.84 and 12.1 µg kg(-1)), imazapyr (5.3 µg kg(-1)) and imazethapyr (24.0 and 37.7 µg kg(-1)) in three samples.