title: Coupled-column liquid chromatography method with photochemically induced derivatization for the direct determination of benzoylureas in vegetables.
abstract: The coupled-column (LC-LC) system, consisting of a first column packed with internal surface reversed phase (ISRP) (50 x 4.6mm ID) and a Chrompack C18 (100 x 4.6 mm ID) as second column, allowed the simultaneous determination of five benzoylurea insecticides in dichloromethane (CH2Cl2) extracts of vegetable samples without any clean-up step. This system was combined with a photochemically induced fluorescence (PIF) post-column derivatization in order to provide strongly fluorescent photoproducts from the non-fluorescent benzoylureas. Limits of detection ranged from 0.21 to 0.98 microg L(-1) of pesticide (equivalent to 0.14-0.65 microg kg(-1) in vegetable samples) and limits of determination ranged from 4.0 to 10.0 microg L(-1) (equivalent to 2.7-6.7 microg kg(-1)). Linearity of the method was established between 2 and 1800 microg L(-1), depending upon the compound. Validation of the total method was performed by randomly analyzing recoveries of four vegetable samples (aubergine, cucumber, green bean, and tomato) spiked at two levels of concentration (10.0 and 33.3 microg kg(-1)). The combination of the LC-LC system with PIF detection provides a sensitive, selective, and rapid method for the determination of pesticides in vegetable samples at levels lower than the maximum residue levels (MRLs) established for these compounds by Spanish legislation.
authors.affiliation: Department of Analytical Chemistry, University of Almería, La Cañada de San Urbano, 04120 Almería, Spain. mdgil@ual.es
authors.forename: Maria Dolores Gil
authors.initials: MD
authors.lastname: García
authors.forename: Dolores Barranco
authors.initials: DB
authors.lastname: Martínez
authors.forename: María Martínez
authors.initials: MM
authors.lastname: Galera
authors.forename: Piedad Parrilla
authors.initials: PP
authors.lastname: Vázquez
mesh_terms: D000818:Animals; D001549:Benzamides / Q000032:analysis*; D002138:Calibration; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D007306:Insecticides / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis; D010671:Phenylurea Compounds / Q000032:analysis*; D010777:Photochemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014675:Vegetables / Q000737:chemistry*
chemical_list: D001549:Benzamides; D007306:Insecticides; D010573:Pesticide Residues; D010671:Phenylurea Compounds