title: Single-laboratory validation and uncertainty analysis of 82 pesticides determined in pomegranate, apple, and orange by ethyl acetate extraction and liquid chromatography/tandem mass spectrometry.
abstract: Single-laboratory validation results are reported for the multiresidue determination of 82 pesticides at < or = 10 ng/g levels in pomegranate, apple, and orange. Samples were extracted with ethyl acetate, and the extracts were cleaned up by dispersive solid-phase extraction with primary secondary amine sorbent. The concentrations of the pesticides were estimated within 18 min of chromatographic run time by liquid chromatography/mass spectrometry with multiple-reaction monitoring. The method was reproducible (HorRat of < 0.5 at 10 ng/g) with measurement uncertainties of < 15% for all the compounds at 10 nglg in all 3 matrixes. The limits of quantitation ranged from 2.5 to 5.0 ng/g with recoveries of 70-120% for most pesticides. Matrix-induced signal suppressions were significantly higher in orange compared with those in pomegranate and apple. The method offers a less expensive and safer alternative to the existing multiresidue analysis methods for fruits and vegetables.
authors.affiliation: National Research Centre for Grapes, PO Manjri Farm, Pune-412 307, India. kbgrape@yahoo.com
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.forename: Dasharath P
authors.initials: DP
authors.lastname: Oulkar
authors.forename: Shubhangi B
authors.initials: SB
authors.lastname: Patil
authors.forename: Sangram H
authors.initials: SH
authors.lastname: Patil
authors.forename: Soma
authors.initials: S
authors.lastname: Dasgupta
authors.forename: Rahul
authors.initials: R
authors.lastname: Savant
authors.forename: Pandurang G
authors.initials: PG
authors.lastname: Adsule
mesh_terms: D000085:Acetates; D002498:Centrifugation; D002853:Chromatography, Liquid; D032084:Citrus sinensis / Q000737:chemistry*; D005506:Food Contamination / Q000032:analysis; D029561:Lythraceae / Q000737:chemistry*; D027845:Malus / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D012015:Reference Standards; D015203:Reproducibility of Results; D012997:Solvents; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry
chemical_list: D000085:Acetates; D010573:Pesticide Residues; D010575:Pesticides; D012997:Solvents; C007650:ethyl acetate