title: Determination of residues of pirimicarb and its desmethyl and desmethylformamido metabolites in fruits and vegetables by liquid chromatography-electrospray/mass spectrometry.
abstract: A method was developed for the simultaneous determination of residues of pirimicarb (I) and its desmethylformamido (II) and desmethyl (III) metabolites in plums, peas, green beans, broad beans, carrots, and swedes. The compounds were extracted with ethyl acetate and determined, without cleanup, by reversed-phase liquid chromatography and electrospray mass spectrometry (MS). MS and MS/MS were used concurrently to monitor the protonated molecules and their common collision-induced dissociation product. The limit of detection (signal-to-noise ratio of >3) was 1 ng/mL, corresponding to crop concentrations of <0.0015 mg/kg. All 3 compounds were determined in plums, broad beans, and green beans by MS without interference. Interferences which affected the determination of desmethylformamido-pirimicarb in peas, and to a lesser extent in carrots and swedes, were eliminated by MS/ MS. Recoveries for all 3 compounds, at 0.05 mg/kg for plums and 0.005 mg/kg for other commodities, were in the range 83-124%. No interconversion of I, II and III, occurred during extraction, and the compounds were stable in extracts for > or = 7 days under appropriate conditions.
authors.affiliation: Central Science Laboratory, Sand Hutton, York, UK.
authors.forename: J R
authors.initials: JR
authors.lastname: Startin
authors.forename: M D
authors.initials: MD
authors.lastname: Sykes
authors.forename: J C
authors.initials: JC
authors.lastname: Taylor
authors.forename: S J
authors.initials: SJ
authors.lastname: Hird
authors.forename: K
authors.initials: K
authors.lastname: Jackson
authors.forename: R J
authors.initials: RJ
authors.lastname: Fussell
authors.forename: A R
authors.initials: AR
authors.lastname: Hill
mesh_terms: D002219:Carbamates / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D005638:Fruit / Q000737:chemistry*; D007306:Insecticides / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D008956:Models, Chemical; D011743:Pyrimidines; D014675:Vegetables / Q000737:chemistry*
chemical_list: D002219:Carbamates; D007306:Insecticides; D011743:Pyrimidines; C011994:pirimicarb