Analysis of phenylurea and propanil herbicides by solid-phase microextraction and liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection

• Published in: Analytica chimica acta Vol. 593; no. 2; pp. 157 - 163
• Main Authors: Mughari, Ahmed R., Vázquez, P. Parrilla, Galera, M. Martínez
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 19.06.2007; Elsevier
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Exact sciences and technology; Groundwater; Liquid chromatography separation; Other chromatographic methods; Phenylurea herbicides; Photochemically induced fluorescence; Solid-phase microextraction; Spectrometric and optical methods; Solid-phase microextraction; Liquid chromatography separation; Phenylurea herbicides; Photochemically induced fluorescence; Groundwater; Water; Fluorescence detector; Pesticides; Microanalysis; HPLC chromatography; Derivatization; Herbicide; Fluorescence spectrometry; Solid phase microextraction; Sample preparation; Phenylureas; Detection limit; Standard deviation; Ground water
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2007.04.061

This study examines the application of solid-phase microextraction coupled with high performance liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection (SPME–HPLC–PIF–FD) for the determination of four phenylurea herbicides (monolinuron, diuron, linuron and neburon) and propanil in groundwater. Direct immersion (DI) SPME was applied using a 60 μm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber for the extraction of the pesticides from groundwater samples. An AQUASIL C 18 column (150 mm × 4.6 mm i.d., 5 μm) was used for separation and determination in HPLC. The method was evaluated with respect to the limits of detection (LODs) and the limits of quantification (LOQs) according to IUPAC. The limits of detection varied between 0.019 μg L −1 and 0.034 μg L −1. Limits of quantification ranged between 0.051 μg L −1 and 0.088 μg L −1. These values meet the recommended limits for individual pesticides in groundwater (0.1 μg L −1) established by the EU. Recoveries ranged between 86% and 105% and relative standard deviation values between 2% and 8%.