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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-ex- change 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.

journal of aoac international

Multiresidue Determination and Confirmation of Imidazolinone Herbicides in Soil by High-Performance Liquid Chromatography/Electrospray Ionization Mass Spectrometry