Solid-phase microextraction for the determination of benzoylureas in orange juice using liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection

• Published in: Journal of separation science Vol. 31; no. 1; pp. 56 - 63
• Main Authors: Parrilla Vázquez, Piedad, Mughari, Ahmed R, Martínez Galera, María
• Format: Journal Article
• Language: English
• Published: Weinheim Wiley-VCH Verlag 2008; WILEY-VCH Verlag; WILEY‐VCH Verlag; Wiley
• Subjects: Benzoylureas; Biological and medical sciences; Food industries; Fruit and vegetable industries; Fundamental and applied biological sciences. Psychology; LC separation; Non alcoholic beverage industries and mineral waters; Orange; Photochemically induced fluorescencence; Solid phase microextraction; LC separation; Chemical analysis; Insecticide; HPLC chromatography; Photochemical reaction; Derivatization; Orange; Postcolumn; Chemical enrichment; Chitin synthesis inhibitor; Sample preparation; Ureas; Beverage; Quantitative analysis; Benzoylureas; Trace analysis; Validation; Fluorescence detector; Fruit; Pesticides; Contamination; Solid phase microextraction; Photochemically induced fluorescencence; Orange juice; Residue
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.200700289

A solid-phase microextraction (SPME) method has been developed for the determination of six benzoylureas (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, lufenuron, and flufenoxuron) in natural orange juice based on the direct immersion mode of a 60 μm polydimethylsiloxane/divinylbenzene fiber. An orange juice was obtained from blended, homogenized, and diluted ecological natural orange juice samples. An aliquot of 3 mL of a spiked sample was extracted under optimum SPME conditions. The determination of benzoylureas was carried out using HPLC combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection. The limits of quantification obtained in matrix were within the range of 0.02 to 0.04 mg/kg and these limits are lower than the maximum residue levels established in Spanish regulations for all pesticides in this study. Recoveries in juice samples ranged between 85 and 110% and relative standard deviations between 1.8 and 7.4%.