PMID- 15537073 OWN - NLM STAT- MEDLINE DCOM- 20050329 LR - 20191210 IS - 1615-9306 (Print) IS - 1615-9306 (Linking) VI - 27 IP - 14 DP - 2004 Oct TI - Coupled-column liquid chromatography method with photochemically induced derivatization for the direct determination of benzoylureas in vegetables. PG - 1173-80 AB - 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. FAU - Garcia, Maria Dolores Gil AU - Garcia MD AD - Department of Analytical Chemistry, University of Almeria, La Canada de San Urbano, 04120 Almeria, Spain. mdgil@ual.es FAU - Martinez, Dolores Barranco AU - Martinez DB FAU - Galera, Maria Martinez AU - Galera MM FAU - Vazquez, Piedad Parrilla AU - Vazquez PP LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - Germany TA - J Sep Sci JT - Journal of separation science JID - 101088554 RN - 0 (Benzamides) RN - 0 (Insecticides) RN - 0 (Pesticide Residues) RN - 0 (Phenylurea Compounds) SB - IM MH - Animals MH - Benzamides/*analysis MH - Calibration MH - Chromatography, Liquid/instrumentation/*methods MH - Insecticides/*chemistry MH - Pesticide Residues/analysis MH - Phenylurea Compounds/*analysis MH - Photochemistry MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Vegetables/*chemistry EDAT- 2004/11/13 09:00 MHDA- 2005/03/30 09:00 CRDT- 2004/11/13 09:00 PHST- 2004/11/13 09:00 [pubmed] PHST- 2005/03/30 09:00 [medline] PHST- 2004/11/13 09:00 [entrez] AID - 10.1002/jssc.200301661 [doi] PST - ppublish SO - J Sep Sci. 2004 Oct;27(14):1173-80. doi: 10.1002/jssc.200301661.