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Coupled‐column liquid chromatography method with photochemically induced derivatization for the direct determination of benzoylureas in vegetables
Author(s) -
Gil García María Dolores,
Barranco Martínez Dolores,
Martínez Galera María,
Parrilla Vázquez Piedad
Publication year - 2004
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301661
Subject(s) - chromatography , derivatization , chemistry , detection limit , dichloromethane , residue (chemistry) , pesticide residue , pesticide , high performance liquid chromatography , organic chemistry , solvent , agronomy , biology
The coupled‐column (LC‐LC) system, consisting of a first column packed with internal surface reversed phase (ISRP) (50×4.6 mm ID) and a Chrompack C 18 (100×4.6 mm ID) as second column, allowed the simultaneous determination of five benzoylurea insecticides in dichloromethane (CH 2 Cl 2 ) 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 μg L –1 of pesticide (equivalent to 0.14–0.65 μg kg –1 in vegetable samples) and limits of determination ranged from 4.0 to 10.0 μg L –1 (equivalent to 2.7–6.7 μg kg –1 ). Linearity of the method was established between 2 and 1800 μg 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 μg 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.