title: Determination of the pesticide diflubenzuron in mushrooms by high-performance liquid chromatography-atmospheric pressure chemical ionisation mass spectrometry.
abstract: 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).
authors.affiliation: Ministry of Agriculture, Fisheries and Food, CSL Food Science Laboratory, Colney, Norwich, UK.
authors.forename: K A
authors.initials: KA
authors.lastname: Barnes
authors.forename: J R
authors.initials: JR
authors.lastname: Startin
authors.forename: S A
authors.initials: SA
authors.lastname: Thorpe
authors.forename: S L
authors.initials: SL
authors.lastname: Reynolds
authors.forename: R J
authors.initials: RJ
authors.lastname: Fussell
mesh_terms: D001274:Atmospheric Pressure; D001487:Basidiomycota / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004132:Diflubenzuron / Q000032:analysis*; D007477:Ions; D013058:Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis*; D011786:Quality Control; D012680:Sensitivity and Specificity
chemical_list: D007477:Ions; D010573:Pesticide Residues; D004132:Diflubenzuron