Multiresidue determination and confirmation of imidazolinone herbicides in soil by high-performance liquid chromatography/electrospray ionization mass spectrometry

Abstract

A new multiresidue method was developed to determine 6 imidazolinone herbicides in 5 different soil types, using high-performance liquid chromatography/electrospray ionization mass spectrometry (HPLC/ESMS). Good recoveries and sensitivity were obtained for the compounds investigated at the 2.0 ppb limit of quantitation. A 50 g portion of soil was extracted with 0.5N NaOH. A portion of the extract was acidified to precipitate humic acids, and the supernatant was loaded onto a preconditioned tC-18 solid-phase extraction (SPE) cartridge and eluted with ethyl acetate. Further cleanup was achieved by using a tandem strong-anion-exchange SPE/strong-cation-exchange (SCX) SPE. Analytes were eluted from the SCX SPE with saturated KCI in methanol. After cleanup, the sample was desalted with an RP-102 SPE cartridge. Quantitation was achieved by monitoring the [M + H]+ ions for each compound, with a time-scheduled selective-ion-monitoring program (positive mode). The extraction and cleanup procedure produced a purified extract for MS confirmation using 3 ions with "in-source" collision-induced dissociation.