Determination of the pesticide diflubenzuron in mushrooms by high-performance liquid chromatography-atmospheric pressure chemical ionisation mass spectrometry.

A method using high-performance liquid chromatography-atmospheric pressure chemical ionisation mass spectrometry (HPLC-APCI-MS) has been developed and validated for the determination of the insecticide diflubenzuron [1-(4-chlorophenyl)-3-(2,6-difluorobenzoyl)urea] in mushrooms. Samples were homogenised with acetone, extracted into dichloromethane-cyclohexane and further cleaned-up by size-exclusion chromatography (SEC). HPLC was performed on an ODS column with methanol-water at 1 ml/min. The limit of detection was 0.02 ng/microl (equivalent to 0.017 mg/kg in the crop). The calibration was linear over the range 0.025-1.0 ng/microl. Recovery of diflubenzuron from spiked mushrooms (0.06-0.58 mg/kg) was 85.5% with a relative standard deviation of 14.5% (n = 56).