High-performance liquid chromatographic determination of benzoylurea insecticides residues in grapes and wine using liquid and solid-phase extraction

A method for the determination of the benzoylurea insecticides diflubenzuron, triflumuron, teflubenzuron, lufenuron and flufenoxuron in grapes and wine by HPLC has been developed and validated. Grape samples (50 g) were homogenized and extracted with ethyl acetate-sodium sulfate and further cleaned-up by solid-phase extraction on silica sorbent. Wine samples (10 ml) diluted with water (1:3) were solid-phase extracted on an octadecyl sorbent using methanol as the eluent. The pesticides were separated on a reversed-phase octadecyl narrow-bore column by gradient elution and the residues were determined with a UV diode array detector. The calibration plots were linear over the range 0.05-5 micrograms/ml. Recoveries of benzoylurea pesticides from spiked grapes (0.02-2.0 mg/kg) and wine (0.01-0.2 mg/l) were 85.8-101.6% and 69.1-104.8%, respectively, and the limits of quantification for these insecticides were < 0.01 mg/kg for grapes and < 0.01 mg/l for wine. The method was applied to the determination of flufenoxuron and teflubenzuron residues in grapes from treated fields and in produced wine.